",isbn:"978-1-83968-760-0",printIsbn:"978-1-83968-759-4",pdfIsbn:"978-1-83968-761-7",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"cc49d6034d85f8f2e2890c6acc3cc629",bookSignature:"Dr. Abhijit Biswas",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10285.jpg",keywords:"Mott Insulators, Semi Metals, Polycrystals, Single Crystals, Electronic Properties, Magnetic Properties, PLD, MBE, Topological Insulators, Topological Hall Effect, Devices Applications, Catalysis",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"September 9th 2020",dateEndSecondStepPublish:"October 7th 2020",dateEndThirdStepPublish:"December 6th 2020",dateEndFourthStepPublish:"February 24th 2021",dateEndFifthStepPublish:"April 25th 2021",remainingDaysToSecondStep:"5 months",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:"A pioneering researcher in the field of tailoring metal oxide crystal surfaces and growth as well as engineering of thin films for various emergent phenomena and energy applications. Dr. Biswas received his Ph.D. from POSTECH, South Korea.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"194151",title:"Dr.",name:"Abhijit",middleName:null,surname:"Biswas",slug:"abhijit-biswas",fullName:"Abhijit Biswas",profilePictureURL:"https://mts.intechopen.com/storage/users/194151/images/system/194151.png",biography:"Dr. Abhijit Biswas is a research associate at the Indian Institute of Science Education and Research (IISER) Pune, in India. His research goal is to design and synthesize highest quality epitaxial heterostructures and superlattices, to play with their internal degrees of freedom to exploit the structure–property relationships, in order to find the next-generation multi-functional materials, in view of applications and of fundamental interest. His current research interest ranges from growth of novel perovskite oxides to non-oxides epitaxial films, down to its ultra-thin limit, to observe unforeseeable phenomena. He is also engaged in the growth of high quality epitaxial layered carbides and two-dimensional non-oxide thin films, to exploit the strain, dimension, and quantum confinement effect. His recent work also includes the metal-insulator transitions and magneto-transport phenomena in strong spin-orbit coupled epitaxial perovskite oxide thin films by reducing dimensionality as well as strain engineering. He is also extremely interested in the various energy related environment friendly future technological applications of thin films. In his early research career, he had also extensively worked on the tailoring of metal oxide crystal surfaces to obtain the atomic flatness with single terminating layer. Currently, he is also serving as a reviewer of several reputed peer-review journals.\nDr. Biswas received his B.Sc. in Physics from Kalyani University, followed by M.Sc in Physics (specialization in experimental condensed matter physics) from Indian Institute of Technology (IIT), Bombay. His Ph.D., also in experimental condensed matter physics, was awarded by POSTECH, South Korea for his work on the transport phenomena in perovskite oxide thin films. Before moving back to India as a national post-doctoral fellow, he was a post-doc at POSTECH working in the field of growth and characterizations of strong spin-orbit coupled metal oxide thin films.",institutionString:"Indian Institute of Science Education and Research Pune",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"2",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"Indian Institute of Science Education and Research Pune",institutionURL:null,country:{name:"India"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"20",title:"Physics",slug:"physics"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"205697",firstName:"Kristina",lastName:"Kardum Cvitan",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/205697/images/5186_n.jpg",email:"kristina.k@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copyediting and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. 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\n
1. Introduction
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The holographic recording materials are traditionally used to record holograms, and they have been mainly studied and characterized for holographic applications [1, 2, 3]. Along with the evolution of photonics, communications and optical processing of information, the relevance, and capabilities of these materials to store any kind of phase or amplitude diffraction pattern, with good results also for low spatial frequencies, are surfacing [4, 5, 6]. At this point, the complete characterization of these materials for low spatial frequencies is decisive to design a material with the optimum characteristics for each specific application [7, 8].
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The holographic recording materials change their properties when they are exposed to the light, and there are many examples of them, for example, the photographic emulsions [9], photochromic materials [10], dichromated gelatin [11], photorefractive materials [12], or photopolymers [13].
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The last ones, photopolymers, are a very promising option, for example, for the development of holographic memories due to its high resolution and fidelity. The use of this recording material has spectacularly been increased because of its versatility at the time of changing their composition or design [14]. Moreover, they present high reliability, repeatability, and flexibility together with their tunable thickness, self-processing capabilities, and low cost. It is undeniable how those features set the photopolymers as one of the best holographic storage media and a good option for applications inside the diffractive optics and optical processing fields.
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In these fields, one of the main drawbacks to be faced is the conservation of the element recorded into the photopolymer. In this sense, along this chapter, we will study the effects and improvements added by a coverplating together with an index-matching system. This system not only improves the lifetime of the material but also affects to the molecules diffusion inside the material.
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2. Overview of the materials and DOE recording process
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2.1. The recording materials
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A photopolymer is a formulation based in an organic polymer sensitive to the light of certain wavelength. The basic formula is made of a sensitizer dye, an initiator to generate free radicals and one or more polymerizable monomers. These components are disposed in a matrix composed of a polymer such as poly(vinyl alcohol) (PVA), sodium polyacrylate, or vinyl chloride (PVC).
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The basic way to record a DOE into a photopolymer, a phase media, is by refractive index modulation between the polymerized and nonpolymerized areas, which correspond to illuminated and nonilluminated areas, respectively [15].
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A great variety of these materials can be developed based on a given monomer, a support matrix, a dye, and the rest of the components of the solution. These components and their concentration will affect the final properties of the photopolymer, as well as its applications. The main factor is the binder, because it will determine the range of monomer, dye, and initiator to be used in the final compound.
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In this chapter, all the results presented are based on three different materials: one of the most studied photopolymers, based on PVA and acrylamide (AA) as main monomers, which has demonstrated its high linearity and fidelity working in low- and high-spatial frequencies [4, 5]. Despite these good characteristics, the main drawback of this material is its high toxicity, mainly given by AA, which is known to be carcinogenic since many years. Also, it is known that the low environmental compatibility in terms of the low biodegradability of the devices is made of this material [16]. In this sense, our research group has developed a biocompatible photopolymer, called Biophotopol [17], which use sodium acrylate (NaAO) as a main monomer and has demonstrated to have a great dynamic range and high sensitivity together with its high biocompatibility and the main properties of the photopolymers such as the self-processing capabilities and low cost.
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The third material used, polymer dispersed liquid crystal (PDLC), demonstrates how the versatility of the photopolymers can be improved by the inclusion of new components, like nanoparticles or dispersed liquid crystal (LC) molecules, in their formula [18, 19]. In this case, thanks to the addition of LC molecules, it is possible to fabricate polymers that change their optical properties by means of an external stimulus, in this case an electrical field. A hologram can be recorded into the material and then modulate its DE on real time thanks to the electrical field applied. The formulations of the different materials are shown in Table 1.
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Material: PVA/AA-based photopolymer
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TEA (ml): 2.0
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PVA (ml) (8%, w/v): 25
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AA (g): 0.84
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BMA (g): 0.2
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YE (0.8%, w/v) (ml): 0.6
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Material: Biophotopol
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PVA (8%, w/v): 15
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NaAO (M): 0.34
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TEA (M): 0.15
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PRF (M): 1.00 × 10−3
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Material: PDLC (wt%)
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\n
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DPHPA: 48.8
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BL036: 29.2
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YEt: 0.1
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NPG: 1.5
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NVP: 16.4
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OA: 4.4
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\n\n
Table 1.
Formulation of different photopolymers used.
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2.2. The photopolymerization reaction
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The photopolymerization reaction (Figure 1) starts when the photopolymers are illuminated by light of certain wavelength, and the monomer starts to polymerize, causing a shrinkage on the illuminated areas, increasing the refractive index and decreasing the monomer concentration of these areas. This chemical compound gradient of the monomer, dye and radical generator causes a diffusion of the different components from the areas where the concentration is high, “dark areas” to the areas where the concentration has decreased, the “illuminated areas.” This diffusion causes a decreasing of volume in the dark areas, and therefore, the volume of the illuminated areas is increased by incoming molecules, counteracting the shrinkage due to the polymerization process.
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Figure 1.
Representation of the formation of the hologram in a photopolymer.
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The simplest DOE that can be recorded into a photopolymer is the sinusoidal profile, which can be obtained by the interference of two plane beams, controlling the period of the grating by changing the angle between the two beams. To record more complex DOE, it is necessary to control the shape of the incident beam to generate the desired profile. Nowadays, the advances on the spatial light modulators (SLMs) based on liquid crystal on silicon (LCoS) displays, thanks to the microelectronics technology, are allowing the production of commercial devices with resolutions higher than 4094 × 2464 (4 K) in the same size that of a conventional LCD screen. The use of this device in the optic setups allows the recording of an enormous variety of different complex DOEs with an active control of the function displayed by the LCD screen through a computer.
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These complex profiles may suffer a smoothing of the profile due to different factors such as the cutoff frequency of the optical system, the cross talk between pixels, the finite size of the polymer chains, the diffusion of the monomer or the nonlinearity of the recording process. This deviation from the ideal profile depends on the R parameter, which indicates the relative importance of the photopolymerization with respect to the monomer diffusion:
where D is the monomer diffusivity, FR is the polymerization rate, and Kg is the grating number, related with the grating period Λ by means of Kg = 2π/Λ. At the time of modeling the behavior of these materials, there are many other parameters involved in the phase image formation process to consider, starting by the intensity and the fringes visibility, V. The importance of these parameters is analyzed by the relationship between polymerization rate and incident intensity.
The kR(t) factor is the polymerization parameter, which indicates the speed of the photochemical reaction that takes place in the material and depends on the concentration and type of the substances involved and their media, I(x,z,t) is the recording intensities’ distribution, exponentially attenuated with depth due to the dye absorption (Beer’s law [20]), α indicates this absorption (it decreases when the dye is consumed), V is the fringes visibility (typically 1), and γ represents the relationship between the polymerization rate and the recording intensity. This parameter usually takes values between 0.5 and 1, corresponding the value 0.5 to more liquid polymerizable systems and 1 to more solid systems.
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To model the three-dimensional behavior of the monomer and polymer volume fractions, m and p, respectively, the following general equations can be used, where φ(m) and φ(p) are the monomer and polymer concentrations, respectively:
where Dm is the monomer diffusion inside the material, which decreases with time. To solve these differential equations, there are different methods. In the recording model used through this chapter, we have used the finite-difference method (FDM) to obtain a numerical solution.
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Once we have measured the monomer and polymer concentrations, the refractive index of the photopolymeric layer can be calculated as a function of the volume fraction variations of each component using the Lorentz-Lorenz equation [21]:
where φ(m0) is the average initial value for the monomer volume fraction, np is the polymer refractive index, nm is the monomer refractive index, and nb is the support matrix refractive index. These two last parameters can be measured using a refractometer, and the value of np can be obtained through zero-spatial frequency measurement technique [22].
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The linearity in the material response can be studied in very low spatial frequencies to avoid the influence of the monomer diffusion in the diffractive image formation; the R parameter, described in Eq. (1), takes values higher than the ones obtained in holographic regime due to the high value of the spatial period.
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The diffraction efficiency (DE) of the different diffracted orders in Fraunhofer domain is given by the Bessel functions [23]. Figure 2 shows the behavior of the main four diffracted orders as a function of the phase shift. The comparison of this figure and the DE results obtained for certain material gives an approach of the linearity in the response of the material.
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Figure 2.
Diffraction efficiency of the main four orders of a sinusoidal grating as a function of the phase depth.
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2.3. Influence of the index matching
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As we mentioned in Section 1, one of the main drawbacks of the photopolymers is their conservation. In this sense, the inclusion of an index-matching system and coverplating not only improves the lifetime and conservation of the materials, but also allow us to measure the internal monomer diffusion [24]. This index-matching system allows us to clarify how the fast changes are measured in uncovered layers. Therefore, some authors observed in PVA/AA materials some fast changes on the surface [4]. They fitted this monomer diffusion around 10−7 cm2/s. Some years late, Close et al. [25], using a coverplating and index-matching agent to avoid the surface changes, measured the monomer diffusion inside the material around 10−10 cm2/s. They also obtained the diffusion of other substances such as acetone inside the material, which lead us to make a distinction between the “apparent” diffusion of the surface, the first one, and the “real” diffusion, the internal monomer diffusion, the second one.
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The thickness variations of the material play an important role in the DOEs formation at very low spatial frequency recording [5]. In DOEs recorded in materials without index matching, the transmitted beam has the information of the thickness and refractive index modulation mixed. By using the index-matching system (Figure 3), it is possible to study separately the changes produced by the refractive index variation. To achieve the index matching, we must choose a liquid with a refractive index very close to the mean of the polymer refractive index and not soluble with the photopolymer. When the shrinkage due to the polymerization takes place, this liquid will fill up the holes generated in the surface of the material, minimizing the diffractive effects due to the relief structure.
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Figure 3.
Diagram of a DOE recording using index-matching system. The so-called “apparent” diffusion is due to the recovering surface changes and the “real” diffusion is due to the internal monomer motion.
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The value measured for uncovered layers due to this “apparent” diffusion is around 10−7 cm2/s, which is not a suitable value to record complex DOEs with sharp profiles, due to the fast mass transfer, which produces a smoothening of these sharp profiles. For index-matched samples; this value is around 10−11 cm2/s, suitable for complex structures recording. Thanks to the reduction of the mass transfer produced by the sealant, it is possible to record sharp profiles with insignificant smoothening of the profile.
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2.3.1. Characterization of the different materials
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To analyze the effects of this index-matching system, we use the setup shown in Figure 4; in this setup, we can distinguish two beams, the recording beam, provided by a solid-state Verdi laser (Nd-YVO4) with a wavelength of 532 nm (green light), at which the material exhibits maximum absorption, and the analyzing beam, provided by a He-Ne laser at a wavelength of 644 nm, at which the material is not sensitive.
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Figure 4.
Experimental setup used to record and analyze in real time the DOEs formation on the photopolymers. Di, diaphragm; Li, lens; BS, beam splitter; SFi, spatial filter; LP, linear polarizer; and RF, red filter.
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The DOE to be recorded is provided by an LCoS SLM, placed along the recording arm of our setup and sandwiched between two polarizers (P), oriented to produce amplitude-mostly modulation. To obtain a linear response for each level of gray and good contrast, this device was characterized using the model proposed in [26]. Then, a 4F system images the intensity distribution generated by the SLM onto the recording material. The intensity of the recording beam is 0.25 mW/cm2.
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The analyzing arm, which allows us to study on real time the grating formation onto the photopolymer, was designed to collimate the light incident on the recording material, and a diaphragm (D1) was used to limit the aperture of the collimated beam. A nonpolarizing beam splitter (BS) split the beam in two within the same path. A red filter (RF) was placed behind the recording material to ensure that only the analyzing beam is incident on the CCD camera placed at the end of the setup. To separate the different diffraction orders, we placed a lens behind the material, obtaining the Fraunhofer diffraction pattern on the camera.
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In Figure 5, the experimental DE of the four main orders for a sinusoidal grating with spatial period of 168 μm is shown. The sample has a thickness of 85 μm. We made two experiments, one without the coverplating and index-matching system (Figure 5a) and a second one using the index-matching system and coverplating (Figure 5b). It is noticeable how for longer exposure times, greater than 300 s, the phase modulation of both cases looks similar. In samples without index-matching, the recorded phase grating can be understood as the superposition of two phase gratings: a refractive index grating and a relief grating. It can be assumed that the effects of the last one are weaker for long exposure times. At these times, the fast diffusion through the surface in the uncovered sample has mitigated the effects of the relief grating. On the other hand, this relief grating causes that, in the case of the nonindex-matched sample, the maximum DE is achieved after 180 s, three times later that in the index-matched case. This is produced by the decrease in the phase modulation caused by the shrinkage, which is canceled at longer exposure times, as has already been said. In the experiments carried out for gratings with different spatial periods, we have observed that the behavior is similar. This is important for the recording of complex elements with different spatial frequencies mixed in their shapes such as diffractive lenses.
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Figure 5.
Experimental DE during recording of a grating with spatial period of 168 μm and thickness of 85 μm without index-matching system (a) and with index-matching system (b).
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For the holographic regime, the diffusion times are very short and they do not exceed 0.1 s, which greatly hinders its measurement. Thus, to measure the species diffusion in frequencies around 1000 lines/mm, it is necessary to use indirect methods. At very low spatial frequencies, we can measure many diffracted orders to obtain information about the phase profile and its evolution after recording due to the diffusion. An interesting experiment is to measure the evolution of the DOE stored after recording. These variations are called in-dark evolution. In Figure 6, it can be appreciated the in-dark evolution of a nonindex-matched sample and an index-matched sample, exposing the sample during 50 s and shutting off the recording laser, analyzing the post exposure evolution of the DOE. For the nonindex-matched samples, the variation of the DEs is very fast in comparison with the index-matched ones. In the last case, it is noticeable how the two first orders remain practically constant after recording. The fitted values of the monomer diffusion in each case can be observed in Figure 7. We noted that the phase depth, ∆φ, becomes time independent after a time range, which goes from several minutes to a few days after exposure. Taking this into account, it is possible to follow the procedure of [27] to obtain the “apparent” diffusion of this kind of materials, which depends on two variables: Λ, the grating period and τ, the characteristic time of monomer variation.
Experimental DE during 50 s recording of a sinusoidal grating of 168 μm in an 85 μm thickness index-matched and nonindex-matched samples and the in-dark evolution.
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Figure 7.
Fitting of the experimental values after 50 s of recording time a nonindex-matched sample (a) and index-matched sample (b).
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τ can be calculated by fitting the phase depth of the grating variation with time [6]. To obtain this value, we can use Fick’s Law equation to describe species concentration after exposure and the fitting of the temporal variation for ∆φ:
where the species modulation generated inside the photopolymer is represented by ∆φ(i)(x), φf(i) is the average value of the residual species concentration, and ∆φ(avg) is the average for all molecules. This corresponds to the point at which monomer diffusion eventually stops due to a uniform monomer distribution. The molar volume of the monomer is represented by Vm and tends asymptotically (in practice in some minutes) to the value:
The only assumption is that ∆φ is proportional to ∆(avg), which is reasonable for small polymer concentrations.
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In Figure 6, it can be seen how the slope of the linear fitting for the nonindex-matched sample is almost two magnitude orders higher than the index-matched one. The diffusion measured for the last one is 3.5 × 10−10 cm2/s, within the expected values for these materials. On the other hand, the “apparent” diffusion measured for the nonindex-matched sample is 1.6 × 10−8 cm2/s. The differences between using or not the index-matching system are clear together with this separation between “apparent” and “real” diffusion. Using this index-matching system, it is possible to get a phase depth of 2π for PVA/AA samples of 105 μm without using any crosslinker. To get this, 2π phase depth modulation is very important as is needed by many applications related to the complex DOEs recording, such as blazed gratings or diffractive lenses [29, 30].
\n
One of the methods to increase the phase depth is the inclusion of a crosslinker monomer. The role of this component is to increase the chain length and compaction by linking the polyacrylamide chains between them. Therefore, the polymerization rate, shrinkage, and refractive index are increased [30]. With the use of a crosslinker, it is possible to get the 2π phase depth in samples around 85 μm. In Figure 8, the effects of using N,N′-methylene-bis-acrylamide (BMA) as a crosslinker agent in the PVA/AA photopolymer formulation is shown. Comparing this figure with Figure 2, it is noticeable that the phase depth of 1.4·2π is reached after 200 s of exposure time in a sample of 95 μm thickness, a value substantially lower than the 105 μm needed for materials formulated without this crosslinker. Therefore, including agents such as BMA can drastically improve the material properties at very low spatial frequency recording.
\n
Figure 8.
Experimental DE for the recording of a sinusoidal grating of 168 μm during 200 s of exposure time in an AA/PVA material with 95 μm thickness without the index-matching and coverplating system.
\n
The same analysis had been done for the Biophotopol green photopolymer, studying the effects of the index-matching system. Due to the similarities between this material and the PVA/AA-based one, Biophotopol also presents important relief structures formed during recording, avoiding the separate study of the refractive index distribution generated by polymerization. We have also studied the use of different crosslinker agents such as the already-mentioned BMA or the N,N′-(1,2-dihydroxyethylene) bisacrylamide (DHEBA), a highly environmental compatible crosslinker, which is also able to dissolve the NaAO, increasing the utility life of the samples up to 10 times, preventing the monomer crystallization [31]. Figure 9 shows the experimental diffraction efficiency of a Biophotopol + DHEBA sample. In general, the results obtained are very similar to the ones obtained for the other photopolymers. In this case, the maximum phase depth obtained was around 1.4 π for a 90 μm sample. Therefore, assuming a linear behavior with thickness, a sample of around 128 μm will be required to achieve a phase depth of 2π. Regarding the monomer diffusion, the values obtained were around 10−10 cm2/s, a bit slower compared to PVA/AA material.
\n
Figure 9.
Experimental DE for the recording of a sinusoidal grating of 168 μm during 400 s of exposure time in an Biophotopol + DHEBA material with 90 μm thickness.
\n
At this point, it is also interesting to show the capabilities of the PDLC material to work with low spatial frequencies and develop tunable DOEs by means of an electrical field. The use of this material is very common for holographic regime, where it presents a high value of refractive index modulation providing DEs very close to 100% for optical thicknesses around 10 μm. The main drawback of this material is its high scattering. Regarding this factor, it is important to remark that this family of materials is always enclosed between indium tin oxide (ITO) glasses that make impossible to use the index-matching technique used in the other two materials. Thus, in this case, it is impossible to distinguish between “real” and “apparent” diffusion. The results obtained for the recording of a 168 μm period sinusoidal grating into a 30 μm thickness layer are shown in Figure 10. It can be seen how the phase depth of 2π can be achieved, but despite this, the fast values of diffusion, around 10−8 cm2/s, together with the impossibility to distinguish the internal monomer diffusion from the “apparent” one make its selection difficult as a candidate to record low-frequency DOEs.
\n
Figure 10.
Experimental DE for the recording of a sinusoidal grating of 168 μm during 600 s of exposure time in a PDLC material with 30 μm thickness.
\n
\n
\n
\n
2.4. Simulation of the behavior of the materials
\n
A model able to simulate the behavior of the material is a powerful tool to obtain the desired material or illumination parameters to fabricate a particular DOE. We have already introduced our recording model in Section 2.2. Based on the solving of the differential equations that represents the behavior of the monomer and polymer volume fractions, it is possible to predict with fidelity how the different materials will behave during the DOEs recording. This model also includes the effects of the holes produced in the surface during polymerization process and analyzes both the hole and monomer diffusion separately [32].
\n
Holes generation and its diffusion role in the model can be taken into account adding the following equations to the previously introduced, in Section 2.2:
where φ(h) represents the holes volume fraction and Kh is the holes rate generation, proportional to FR, and Dh is the diffusion constant for holes. We assume that the holes are concentrated close to the surface, and their motion is along x direction, with the grating vector parallel to x-axis.
\n
To check the capability of the recording model to simulate both the recording process on the material and the role of the sealant in this process, we recorded sinusoidal gratings in a PVA/AA material. The results obtained were compared with the simulation results, introducing in the model the parameters of the analyzed material. In Figure 11 both the experimental results are shown that are compared with the simulation results of the DE of the main four orders of a sinusoidal grating with a period of 168 μm recorded into a PVA/AA material of 80 μm without (a) and with index matching (b). In both cases, the good agreement can be appreciated between the model and the experimental results. The results obtained are in line with the results shown previously, and the index-matched sample takes less time to reach the maximum DE due to the mitigation of the effects produced by the thickness variations.
\n
Figure 11.
Comparison between experimental and simulated results of the main four orders of DE as a function of time for the recording of a sinusoidal grating of 168 μm in a PVA/AA material with 80 μm thickness, without index matching (a) and with it (b).
\n
The model is also capable to faithfully reproduce the postexposure evolution of the material in both index-matched and nonindex-matched samples. In Figure 12, it can be seen, apart from the good agreement between experimental and simulation results, how for the nonindex-matched sample (a) the DE continues changing after shutting of the recording beam due to the hole diffusion through the surface. These effects are not present in the index-matched sample (b), in which the DE evolution stops with the shutdown of the laser.
\n
Figure 12.
Comparison between experimental and simulated results of the postexposure evolution of the main four orders of DE as a function of time for the recording of a sinusoidal grating of 168 μm in a PVA/AA material with 80 μm thickness, without index matching (a) and with it (b).
\n
\n
\n
\n
3. Recording of complex DOEs
\n
\n
3.1. Recording of blazed gratings
\n
The lower monomer diffusion shown by the materials with index-matching system together with their capabilities of reaching 2π phase depth makes us able to explore the recording of more complex DOEs. One of these complex profiles is the blazed grating, a sharp profile with abrupt changes, which has many applications in communications and theoretically can reach DEs of 100% [28].
\n
Taking into account the previous results of monomer diffusion, we attempt to store this kind of DOE in PVA/AA and Biophotopol materials. The value of D0 tested for PDLC materials avoids the generation of sharp profiles on them. The recording model used is the one described in Section 2.2. In this case, the light intensity distribution during the recording process can be written as follows:
where fs is the period of the grating and I0 is the maximum recording intensity.
\n
The experimental setup has been described previously in Section 2.3.1. We placed the CCD camera in the material plane, and the image at this place and the intensity distribution of this image are shown in Figure 13. This figure shows a smoothening of the abrupt edges of the profile due to the low-pass filtering that the experimental setup introduces, especially due to the diaphragm (D3) placed to eliminate the pixilation of the LCoS screen of the SLM. To improve the accuracy of the recording model, we introduced this recording intensity on it so that the model takes into account the low-pass filtering introduced by the experimental setup.
\n
Figure 13.
Image of a 672-μm blazed grating provided by the LCoS captured by the CCD at the material plane (a) and intensity profile across a vertical line of this image (b).
\n
To analyze the response of the different materials and the capability of our model to predict the behavior of these materials, we perform different period gratings recording. First, we simulated the recording of this kind of DOE using our model to have an idea of the index-matching influence in both materials for different periods. Once we had a theoretical idea of the influence of index matching and period, we compared the simulations with the experimental results. Figure 14 shows the simulated and the experimental DEs of a blazed grating of 672 μm recorded in a PVA/AA photopolymer 90 μm thick and a 336 μm one recorded in a Biophotopol photopolymer of 90 μm. It can be seen how the DE of the first order reaches a maximum of almost 70% after an exposure time of 150 s in the PVA/AA photopolymer and almost 55% in the Biophotopol one. Considering the low-pass filtering introduced by the setup, these are good results because we achieved near the maximum value of DE achievable taking into account this low-pass filtering. It is also noticeable that there is a good agreement between the simulation and the experimental results. The lower value of DE obtained for Biophotopol is due to the lower values of kr and np of this family of photopolymers and can be increased using thicker samples or higher concentrations of crosslinker in the final solution. For shorter period gratings recorded in the same kind of material, it is also appreciable a reduction of the maximum DE reached. This is due to the higher influence of the low-pass filtering at shorter spatial periods together with a higher diffusion.
\n
Figure 14.
Comparison of the simulated and experimental DE of a 672 μm blazed grating recorded in a PVA/AA material (a) and a 336 μm blazed grating recorded in Biophotopol (b), both during an exposure time of 300 s.
\n
In both cases and in the rest of the analysis carried out, the results present similarity independent of the spatial frequency of the grating, showing the low influence of the monomer diffusion at these spatial frequencies.
\n
The recording model allows us to probe the capability of the materials to reach the 100% of DE without considering the low-pass filtering introduced by the experimental setup. This simulation is shown in Figure 15, where it can be seen how a DE of 100% could be reached for PVA/AA-based material and a DE of 97% for the Biophotopol one. The low-pass filtering introduced by the experimental setup means a reduction of over 20% of DE for both materials. This value is achieved at less exposure time than in the experiments by both materials due to the ideal recording intensity. It is also noticeable how in this ideal simulation, the PVA/AA-based material takes less time to reach the maximum DE than the Biophotopol due to the differences in np and kr.
\n
Figure 15.
Simulation results of the DE as a function of time for PVA/AA and Biophotopol materials without taking into account the low-pass filtering introduced by the experimental setup.
\n
\n
\n
3.2. Diffractive lenses
\n
The capabilities of the materials working with a complex profile such as blazed gratings have been proved obtaining near the maximum DE achievable taking into account the low-pass filtering introduced by the setup. Also, the recording model has demonstrated its fidelity reproducing the recording of this element in the different materials, with different spatial periods and considering the index-matching system and low-pass filtering.
\n
Going further, another example of complex DOE to evaluate the model and materials capabilities is diffractive lenses. This DOE includes different spatial periods in its shape, being critical to avoid the smoothening of the profile and to achieve similar behavior for the different spatial periods.
\n
The study of the recording of this kind of DOE has been made only for PVA/AA materials and Biophotopol for the same reasons of the blazed gratings. It is also important to remark that it is necessary to adapt the recording model to make it able to reproduce the cylindrical and spherical lenses formation in these materials. The two-spatial dimension equation shown in Section 2.2 can be applied to reproduce the cylindrical lenses behavior; nevertheless, it is necessary to add a new dimension, the “y” variable dimension, to simulate the case of a spherical lens recording [30]. Eqs. (3) and (4) remain as follows:
The recording intensity distribution is generated by the LCoS SLM in the amplitude regime, which, as in the previously shown experiments, is projected on the material to generate the corresponding phase element. This intensity distribution is defined in Eq. (16), where the phase depends on the quadratic value of the distance between the point and the lens centrum. This equation then is wrapped to 2π and normalized to the maximum value of intensity, I0.
In this equation, f is the focal length and λ represents the light wavelength. The intensity distribution of a 50 cm focal length lens generated using the SLM is shown in Figure 16.
\n
Figure 16.
Horizontal cut of the theoretical intensity distribution of a 50 cm focal lens to be projected onto the photopolymer by the SLM.
\n
The experimental setup used to record diffractive lenses is also the one already shown in Figure 4, with the particularity that in this case, L5 is not present as the lens recorded into the photopolymer is responsible for the focusing of the 633 nm wavelength beam. We imaged the point spread function (PSF) generated by this lens onto the CCD camera, controlling the magnification of the setup by means of the 4F system. The camera is also placed in the material plane to evaluate the intensity pattern imaged on the material. The image taken at this plane and the intensity profile across a horizontal line passing through the center of the lens are shown in Figure 17. We can see the characteristic ring structure with a decreasing spatial period as we move away from the center of the diffractive lens. Also, in the intensity profile image, it is noticeable the improvement of the profile with respect to ones presented using a transmissive LCD as SLM with a pixel size of 44 μm [33].
\n
Figure 17.
Image provided by the LCoS SLM at the material plane captured by the CCD camera (a) and intensity profile across a horizontal line passing through the center of the lens (b).
\n
Using the recording model, it is possible to predict the refractive index distribution generated by the incident beam modulated by the SLM. Once we had obtained this refractive index distribution, we can apply the Fresnel propagation [34] to calculate the intensity distribution as a function of time. Thus, we can analyze the focalization of the lens and the optimum recording time to obtain a good focalization. In Figure 18, the results of the recording simulation can be seen for the recording of a 50 cm diffractive spherical lens in a PVA/AA material with index matching compared to the experimental results, specifically the intensity at the focal point as a function of time. At this point, it is important to add that the simulated behavior exhibited by cylindrical and spherical lenses in the photopolymers used and different focal lenses is similar. Thus, the results shown correspond to the spherical one. In the figure, the good agreement is noticeable between the simulation and the experimental results, together with the good focalization power of the lenses. The model is also capable to predict the optimum recording time for the lenses in the different materials, as it will be shown in the following figures, and the decrease in the focal intensity. This occurs when the exposure time is longer than the optimum and the phase modulation overcomes 2π, as we chemically design the materials to obtain phase depth saturation slightly higher than 2π for the physical thickness used.
\n
Figure 18.
Intensity at the focal point as a function of time for a spherical lens f = 50 cm in a PVA/AA material of 95 μm.
\n
Thanks to the small pixel size of the LCoS screen of the SLM, it is possible to attempt to store shorter focal lenses, for example, 13 cm, to study the influence of the focal on the lenses recording. Figure 19 shows the comparison between the simulation and the experimental measurements of the intensity at the focal point as a function of time for two different focal lenses recorded in Biophotopol material. In this case, there is also a good agreement between the simulation and the experimental results. Both focal lenses present similar behavior than the one exhibited by the lens recorded in PVA/AA material. The lens with shorter focal takes less time to focalize, maybe due to the higher influence of the monomer diffusion.
\n
Figure 19.
Comparison of the experimental results and the simulation of the intensity at the focal point for two different focal lengths (13 and 60 cm) of diffractive lenses recorded in Biophotopol material of 140 μm thickness.
\n
\n
3.2.1. Influence of the material parameters
\n
At the beginning of the chapter, the importance of different parameters in the recording process was remarked. One of the most important aspects of having a recording model that takes into account many of these parameters is that we can study separately the influence of each one of them in the final DOE recorded. In this section, we will discuss the influence of one of these parameters, the internal monomer diffusion (D0), as a sample of the model’s capability. The influence of other parameters, such as the relationship between intensity and polymerization (γ) and the influence of the depth attenuation (α), can be consulted in Ref. [29]. We have studied the variation of each one of these parameters keeping the rest constant. This gives us the idea of which parameters are more important for the lens formation.
\n
To check the influence of D0, we have simulated different lenses with a range of monomer diffusivities from 3 × 10−8 to 3 × 10−11 cm2/s and studied how the diffusion affects in the focal plane. Figure 20 shows the intensity at the focal point for different internal monomer diffusivities. In this case, the intensity at the focal point for the two smallest values does not show any important difference. On the other hand, for both highest values of diffusivity, we appreciate a clear variation as it was expected. The increase in the monomer diffusivity has influence for these spatial frequencies for values higher than 3 × 10−10 cm2/s. Below this value, the influence is low in the lens formation. Therefore, we assumed that for the PDLC material presented in a previous section, the results will not be as good as for the PVA/AA and Biophotopol materials.
\n
Figure 20.
Intensity at the focal point as a function of time for different internal monomer diffusivities.
\n
\n
\n
\n
\n
4. Conclusions
\n
In this chapter, we have presented a method to record low-frequency diffractive optical elements into photopolymers. This process is influenced by many parameters that we have introduced in a three-dimensional diffusion model to predict the phase image formation. Using this model together with different experimental measurements, we have developed an analysis of the requirements needed to achieve a phase modulation range of 2π in different families of materials. The results show the effectiveness and versatility of the recording model used. Thanks to this model, it is possible to predict the experimental behavior of the recording of any kind of DOE in the different photopolymers. The effectiveness of the model was validated by the experimental work carried out and based in the inclusion of an LCoS SLM. This device allows us to store any kind of DOE selected dynamically and analyze the influence of the different material properties during the recording.
\n
Together with that, we have shown the effects of using the index-matching system, which apart from improving the conservation and lifetime of the recorded DOE, let us differentiate between the diffusion in the surface of the photopolymer and the internal diffusion. The lower values of diffusion obtained in the index-matched materials can be exploited to record sharp DOEs without significant smoothening of the refractive index profile.
\n
\n
Acknowledgments
\n
We want to acknowledge the financial support from the Spanish Ministerio de Trabajo y Competitividad under projects FIS2014-56100-C2-1-P and FIS2015-66570-P and by the Generalitat Valenciana of Spain under project PROMETEOII/2015/015.
\n
\n',keywords:"photopolymer, holography, diffractive optical elements, recording materials",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/57574.pdf",chapterXML:"https://mts.intechopen.com/source/xml/57574.xml",downloadPdfUrl:"/chapter/pdf-download/57574",previewPdfUrl:"/chapter/pdf-preview/57574",totalDownloads:840,totalViews:226,totalCrossrefCites:0,totalDimensionsCites:0,hasAltmetrics:1,dateSubmitted:"May 30th 2017",dateReviewed:"October 6th 2017",datePrePublished:"December 20th 2017",datePublished:"January 17th 2018",dateFinished:null,readingETA:"0",abstract:"The technologies based on holographic and photonic techniques related to the optical storage and optical processing of information are rapidly evolving. One of the key points of this evolution are the new recording materials able to perform under the most specific situations and applications. In this sense, the importance of the photopolymers is growing spectacularly. This is mainly due to their versatility in terms of composition and design together with other interesting properties such as self-processing capabilities. In this chapter, we introduce the diffractive optical elements (DOE) generation in these materials and some of the most important parameters involved in this process. The deep knowledge of the material is essential to model its behavior during and after the recording process and we present different techniques to characterize the recording materials. We also present a 3D theoretical diffusion model able to reproduce and predict the experimental behavior of the recording process of any kind of DOE onto the photopolymers. The theoretical results will be supported by experimental analysis using a hybrid optical-digital setup, which includes a liquid crystal on silicon display. Besides this analysis, we study a method to improve the conservation and characteristics of these materials, an index-matching system.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/57574",risUrl:"/chapter/ris/57574",book:{slug:"recent-research-in-polymerization"},signatures:"Roberto Fernández Fernández, Víctor Navarro Fuster, Francisco J.\nMartínez Guardiola, Sergi Gallego Rico, Andrés Márquez Ruiz,\nCristian Neipp López, Inmaculada Pascual Villalobos and Augusto\nBeléndez Vázquez",authors:[{id:"46619",title:"Prof.",name:"Andrés",middleName:null,surname:"Márquez",fullName:"Andrés Márquez",slug:"andres-marquez",email:"andres.marquez@ua.es",position:null,institution:null},{id:"191593",title:"Dr.",name:"Francisco Javier",middleName:null,surname:"Martínez",fullName:"Francisco Javier Martínez",slug:"francisco-javier-martinez",email:"fj.martinez@ua.es",position:null,institution:{name:"University of Alicante",institutionURL:null,country:{name:"Spain"}}},{id:"192588",title:"Prof.",name:"Sergi",middleName:null,surname:"Gallego",fullName:"Sergi Gallego",slug:"sergi-gallego",email:"sergi.gallego@ua.es",position:null,institution:null},{id:"192589",title:"Dr.",name:"Roberto",middleName:null,surname:"Fernández",fullName:"Roberto Fernández",slug:"roberto-fernandez",email:"roberto.fernandez@ua.es",position:null,institution:null},{id:"192592",title:"Prof.",name:"Inmaculada",middleName:null,surname:"Pascual",fullName:"Inmaculada Pascual",slug:"inmaculada-pascual",email:"pascual@ua.es",position:null,institution:null},{id:"192593",title:"Prof.",name:"Augusto",middleName:null,surname:"Beléndez",fullName:"Augusto Beléndez",slug:"augusto-belendez",email:"a.belendez@ua.es",position:null,institution:null},{id:"222305",title:"Prof.",name:"Cristian",middleName:null,surname:"Neipp López",fullName:"Cristian Neipp López",slug:"cristian-neipp-lopez",email:"cristian@dfists.ua.es",position:null,institution:null},{id:"222306",title:"Dr.",name:"Victor",middleName:null,surname:"Navarro Fuster",fullName:"Victor Navarro Fuster",slug:"victor-navarro-fuster",email:"victor.navarro@ua.es",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Overview of the materials and DOE recording process",level:"1"},{id:"sec_2_2",title:"2.1. The recording materials",level:"2"},{id:"sec_3_2",title:"2.2. The photopolymerization reaction",level:"2"},{id:"sec_4_2",title:"2.3. Influence of the index matching",level:"2"},{id:"sec_4_3",title:"2.3.1. Characterization of the different materials",level:"3"},{id:"sec_6_2",title:"2.4. Simulation of the behavior of the materials",level:"2"},{id:"sec_8",title:"3. Recording of complex DOEs",level:"1"},{id:"sec_8_2",title:"3.1. Recording of blazed gratings",level:"2"},{id:"sec_9_2",title:"3.2. Diffractive lenses",level:"2"},{id:"sec_9_3",title:"3.2.1. Influence of the material parameters",level:"3"},{id:"sec_12",title:"4. Conclusions",level:"1"},{id:"sec_13",title:"Acknowledgments",level:"1"}],chapterReferences:[{id:"B1",body:'Weiser MS, Bruder FK, Fäcke T, Hönel D, Jurbergs D, Rölle T. 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Polymer holography in acrylamide-based recording material. In: Rosen J, editor. Holography, Research and Technologies. InTech; 2011. DOI: 10.5772/14564\n'},{id:"B16",body:'Hashimoto K, Aldridge WN. Biochemical studies on acrylamide, a neurotoxic agent. Biochemical Pharmacology. 1970;19(9):2591-2604. DOI: 10.1016/0006-2952(70)90009-2\n'},{id:"B17",body:'Ortuño M, Fernández E, Gallego S, Beléndez A, Pascual I. New photopolymer holographic recording material with sustainable design. Optics Express. 2007;15(19):12425-12435. DOI: 10.1364/OE.15.012425\n'},{id:"B18",body:'Hata E, Mitsube K, Momose K, Tomita Y. Holographic nanoparticle-polymer composites based on step-growth thiol-ene photopolymerization. Optical Materials Express. 2011;1(2):207-222. DOI: 10.1364/OME.1.000207\n'},{id:"B19",body:'Suzuki N, Tomita Y. Silica-nanoparticle-dispersed methacrylate photopolymers with net diffraction efficiency near 100%. Applied Optics. 2004;43(10):2125-2129. DOI: 10.1364/AO.43.002125\n'},{id:"B20",body:'Gallego S, Ortuño M, Neipp C, Márquez A, Kelly JV, Sheridan JT, Beléndez A, Pascual I. 3D behaviour of photopolymers as holographic recording material. In: Proc. SPIE 6252, Holography 2005: International Conference on Holography, Optical Recording, and Processing of Information; 9 June 2006; Varna, Bulgaria, SPIE; 2006. p. 62520B. DOI: 10.1117/12.676525\n'},{id:"B21",body:'Aubrecht I, Miler M, Koudela I. Recording of holographic diffraction gratings in photopolymers: Theoretical modelling and real-time monitoring of grating growth. Journal of Modern Optics. 1998;45(7):1465-1477. DOI: 10.1080/09500349808230641\n'},{id:"B22",body:'Gallego S, Márquez A, Méndez D, Neipp C, Ortuño M, Álvarez M, Fernández E, Beléndez A. Real-time interferometric characterization of a polyvinyl alcohol based photopolymer at the zero spatial frequency limit. Applied Optics. 2007;46(30):7506-7512. DOI: 10.1364/AO.46.007506\n'},{id:"B23",body:'Hariharan P. Optical Holography: Principles, Techniques and Applications. 2nd ed. Cambridge: Cambridge University Press; 1996. DOI: 10.1017/CBO9781139174039\n'},{id:"B24",body:'Fernández R, Gallego S, Márquez A, Francés J, Martínez FJ, Beléndez A. Influence of index matching on AA/PVA photopolymers for low spatial frequency recording. Applied Optics. 2015;54(11):3132. DOI: 10.1364/AO.54.003132\n'},{id:"B25",body:'Close CE, Gleeson MR, Mooney DA, Sheridan JT. Monomer diffusion rates in photopolymer material. Part II. High-frequency gratings and bulk diffusion. Journal of the Optical Society of America B. 2011;28(4):842-850. DOI: 10.1364/JOSAB.28.000842\n'},{id:"B26",body:'Martínez FJ, Márquez A, Gallego S, Ortuño M, Francés J, Pascual I, Beléndez A. Predictive capability of average Stokes polarimetry for simulation of phase multilevel elements onto LCoS devices. Applied Optics. 2015;54(6):1379-1386. DOI: 10.1364/AO.54.001379\n'},{id:"B27",body:'Gallego S, Márquez A, Marini S, Fernández E, Ortuño M, Pascual I. In dark analysis of PVA/AA materials at very low spatial frequencies: Phase modulation evolution and diffusion estimation. Optics Express. 2009;17(20):18279-18291. DOI: 10.1364/OE.17.018279\n'},{id:"B28",body:'Fernández R, Gallego S, Márquez A, Francés J, Navarro-Fuster V, Beléndez A. Blazed gratings recorded in absorbent photopolymers. Materials. 2016;9(3):195. DOI: 10.3390/ma9030195\n'},{id:"B29",body:'Fernández R, Gallego S, Márquez A, Francés J, Navarro-Fuster V, Pascual I. Diffractive lenses recorded in absorbent photopolymers. Optics Express. 2016;24(2):1559-1572. DOI: 10.1364/OE.24.001559\n'},{id:"B30",body:'Andrzejewska E. Photopolymerization kinetics of multi-functional monomers. Progress in Polymer Science. 2001;26(4):605-665. DOI: 10.1016/S0079-6700(01)00004-1\n'},{id:"B31",body:'Fernández R, Gallego S, Francés J, Pascual I, Beléndez A. Characterization and comparison of different photopolymers for low spatial frequency recording. Optical Materials. 2015;44(1):18-24. DOI: 10.1016/j.optmat.2015.02.025\n'},{id:"B32",body:'Gallego S, Fernández R, Márquez A, Ortuño M, Neipp C, Gleeson MR, Sheridan JT, Beléndez A. Two diffusion photopolymer for sharp diffractive optical elements recording. Optics Letters. 2015;40(14):3221-3224. DOI: 10.1364/OL.40.003221\n'},{id:"B33",body:'Marquez A, Gallego S, Ortuño M, Fernandez E, Alvarez ML, Belendez A, Pascual I. Generation of diffractive optical elements onto a photopolymer using a liquid crystal display. In: SPIE Proceedings 7717, Optical Modelling and Design, 77170D; 14 May 2010; Brussels, Belgium. SPIE; 2010. DOI: 10.1117/12.854786\n'},{id:"B34",body:'Goodman JW. Introduction to Fourier Optics. 2nd ed. New York: McGraw-Hill; 1987. 528 p\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Roberto Fernández Fernández",address:"roberto.fernandez@ua.es",affiliation:'
University Institute of Physics Applied to Sciences and Technologies, University of Alicante, Alicante, Spain
University Institute of Physics Applied to Sciences and Technologies, University of Alicante, Alicante, Spain
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\n
1. Introduction
\n
Magnetic materials that are paramagnetic, ferrimagnetic, and ferromagnetic have received much attention because of their unique properties especially ready to modify and nontoxic [1, 2]. Magnetite (Fe3O4), one of many magnetic materials, is widely investigated for possible magnetic resonance imaging, sensor, and adsorbent. Magnetic nanoparticles typically consist of a magnetic core, a coating, and, in some cases, surface active modifiers.
\n
The magnetite nanoparticles have a high surface area that yields numerous active sites. However, preparation of Fe3O4 nanoparticles is problematic since it can agglomerate, which leads to the decrease in the active sites. Coating with organic or inorganic surfactants is one way to avoid the particle agglomeration. The organic surfactants act as capping agents, but at times, they can give bigger particle size. Inorganic capping agent such as silica (SiO2) has exceptional physical and chemical properties. SiO2 is chemically stable in acidic solution and tuneable for modification. Coating of Fe3O4 nanoparticles with SiO2 will also avoid the agglomeration and protect them from dissolution in acidic solution. SiO2 will cover the surface of each Fe3O4 nanoparticle to form Fe3O4/SiO2 nanoparticle core-shell system [3].
\n
Morel et al. have coated Fe3O4 particles with SiO2 to form core-shell having nanometer scale with an average diameter of 49 nm [4]. The success of Fe3O4/SiO2 core-shell nanoparticle formation depends on the size of magnetite. However, stirring with the magnetic bar during the preparation causes condensation and agglomeration of the particles. The nonmagnetic mechanical stirring method was chosen for the preparation of Fe3O4 nanoparticle [5].
\n
Many researchers used thiol group as an adsorbent for [AuCl4]− ion with a better performance [2, 3, 6, 7, 8, 9]. We have reported on the synthesis of the Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group. The Fe3O4/SiO2 nanoparticle core-shell preparation was performed by applying nonmagnetic stirring method. For improving adsorption capacity, modification with thiol group has been conducted. The thiol groups are of the soft bases.
\n
On the other hand, the [AuCl4]− ions are classified as weak acid species, thus provided specific interaction with each other based on Pearson’s hard-soft acid-based concepts [10]. The adsorption kinetics, adsorption capacity, and interaction model for the adsorption of [AuCl4]− ion in solution by Fe3O4/SiO2 nanoparticle core-shell adsorbent are reported. A recent review of the matter can be found elsewhere [11].
\n
Figure 1 shows the schematic architecture of the magnetite-silica-functional groups. The core is magnetite to function as the important part for separation. The shell is silica, which can protect the magnetite from dissolution especially when it contacts with an acidic environment. Modification of the silica surface can be realized by silanization to give functional groups having an important function to react with the metal cations. The functional group must have a strong bond with the surface via complex formation.
\n
Figure 1.
Step-by-step of Fe3O4@SiO2 core-shell preparation and functionalization [3].
\n
Recovery of the magnetic material is key in the process following the adsorption. The spent adsorbent can be separated using a magnetic field. Figure 2 shows how the used magnetic is separated by the external magnetic field. The magnetic adsorbent that has a high content of rare metals can be subject to dissolution and further separation. It is important to state that in the industrial purpose the powerful electromagnet system can be applied to do the job. In the purification, there are many possible green purification processes of metallurgy, starting from electrochemical separation to blast furnace.
\n
Figure 2.
Image of simplified recovery technique of spent magnetic material after adsorption of precious metals [3].
\n
\n
\n
2. Preparation of Fe3O4
\n
Magnetite is commonly prepared by co-precipitation of Fe(II) and Fe(III) salts with suitable bases. Sodium hydroxide and ammonia are both commonly used in the preparation of magnetite. There are many bases that can be used to help control the size and the shape of the particles. Magnetite nanoparticles can be prepared in the presence of carboxylate such as laurate, palmitate, linoleate, and so on. The addition of surfactant helps reduce the particle size and control the shape. The required shape is usually spherical with a diameter of the nanoscale.
\n
For co-precipitation methods, the size, shape, and composition of the resulting nanoparticles very much depend upon the following [12]:
The type of precursors’ salts used, for example, chloride, sulfate, perchlorate, or nitrate
The Fe2+/Fe3+ ratio
The mixing orders
The mixing rates
The reaction temperature
The pH value
The ionic strength of the media
\n
The remaining issue is that magnetite nanoparticles are easily oxidized to maghemite, so this method is often used to obtain nanoparticles of magnetite and maghemite with the small size of 4–20 nm. Grüttner et al. have listed the size, coating, heating behavior, and magnetic properties of some iron oxide nanoparticles produced by this method [13]. Nanoparticles are produced by this method range in size from 4 to 45 nm. For fixed-synthesis conditions, the quality of the magnetite nanoparticles is very reproducible. Although co-precipitation is unquestionably the easiest process and highly scalable, it is not without issues. Controlling the shape is not easy, and the nanoparticles can be more varied in size than that produced in some other methods [12].
\n
Precursors for the Fe(II) include ferrous sulfate, ferrous nitrate, and ferrous chloride. Some use ferrous acetate and ferrous oxalate. The most used precursor is ferrous sulfate. For the Fe(III), we can use ferric chloride, ferric nitrate, and so on. Ferric nitrate is used a lot. Ferric acetate and ferric oxalate are also commonly used as Fe(III) precursors.
\n
The Fe(II) to Fe(III) molar ratio must be controlled strictly at 1:2. Therefore, the concentration of the starting material must be fixed. The oxidation of the Fe(II) ion must be contained by controlling the atmosphere by the use of inert atmosphere. During the co-precipitation, the nitrogen gas must be kept flowing to reduce possible oxidation process. Other noble gases could be used, which give a better magnetite product.
\n
There are various ways to prepare Fe3O4 nanoparticles, such as hydrothermal synthesis [14], co-precipitation [15], microwave irradiation [16], oxidation of Fe(OH)2 by H2O2 [17], and microemulsion [18]. The Fe3O4 nanoparticles synthesized by a hydrothermal method in the presence of sodium sulfate have a particle size of 160 nm [14]. Among various ways to prepare Fe3O4, hydrothermal is one of the simple methods because it gives unique characters. The shape and size of nanoparticles have a good homogeneity and high degree of crystallinity [19].
\n
The widespread method to produce Fe3O4 is by co-precipitation of Fe2+/Fe3+ solution mixture with a molar ratio of 1:2 in alkaline solution [15, 20]. The reaction for Fe3O4 formation by co-precipitation method is shown in chemical Eq. (1). Although this method is well known for synthesis Fe3O4, the molar ratio of reactant, pH, and temperature still need attention to get the proper size and morphology [15]:
Microwave irradiation might be a promising method in processing materials due to its thermal and nonthermal effects. Microwave synthesis has the advantages of short reaction time, small particle size, and narrow size distribution. Aging under microwave irradiation in short period yields Fe3O4 nanoparticles with complete crystalline structure than those aged for 7 days at room temperature [16]. Yu et al. used H2O2 as an oxidizing agent to construct nano-sized superparamagnetic Fe3O4 powders with the size of 8–10 nm. The Fe(OH)2 precipitates were partially oxidized to generate ultrafine Fe3O4 nanoparticles in the presence of surfactants [17]. Work on the control of the size of magnetite-silica via sol–gel method has also been reported [21].
\n
Some researchers use capping agent to control crystal growth during Fe3O4 nanoparticle formation. Co-precipitation technique was used to prepare magnetite nanoparticles with diameter around 35 nm using 0.90 M NaOH solution as the precipitating agent and trisodium citrate as a capping agent. The precursors are ferric and ferrous chloride salts with predetermined Fe3+/Fe2+ molar ratio. The diameter of silica-coated magnetite nanoparticles synthesized by Stöber method was about 50 nm. Due to an electrostatic interaction between the Fe3+/Fe2+ ions of the Fe3O4 NPs and trisodium citrate surfactant, a stable magnetic fluid containing dispersed Fe3O4 NPs was produced [22]. A green and facile method for synthesis of magnetite nanoparticles was proposed [23]. Nano-sized polyhedral particles were synthesized by heating an aqueous solution of Fe2+, Fe3+, and urea at 85°C. The use of PVA in the synthesis system gives spherical magnetite nanoparticles with loose structure, unaggregated. The size of the microspheres can be tuned by changing the concentration of PVA. Upon addition of acetic acid to the system with PVA, microspheres with looser structure were produced. The size of the microspheres can further be tuned by changing the concentration of acetic acid. The co-precipitation of Fe2+ and Fe3+ in aqueous solutions under ultrasound irradiation results in smaller Fe3O4 NPs with a narrow size distribution (4–8 nm) than that produced without ultrasound irradiation [4]. Diethylene glycol (DEG) is also possibly used to control the particle size as reported earlier. This surfactant takes an important role in the preparation of magnetite/zinc oxide hybrid material [24].
\n
\n
\n
3. Coating of Fe3O4 with SiO2
\n
The next step is coating magnetite with silica (SiO2). It is usually performed via silanization reaction. The functional group that is ready to bond to iron oxide is methoxy silane (CH3-O-Si-) or ethoxy silane (CH3-CH2-O-Si-). After the reaction, it forms a covalent bond of Fe-O-Si leaving the end group remains free. The leaving group is methane and ethane. The reaction is better to be done in an organic solvent. The silane group may have a spacer of long ethylene chain (-CH2−). The ending of the silane may be carboxylic, an amine group, hydroxyl, and so on. The surface of the silica has different accesses to the organic functional groups [25].
\n
For example, modification by the use of 3-mercaptopropyltrimethoxysilane (3-MPTS) [3] reaction is depicted as a chemical reaction (2). For further surface modification, we can use other silanization compounds [3]:
Iron oxide is not stable in acidic condition. After coating with silica, the magnetite core is usually stable in the acidic solution. It will come readily with a proton to give its corresponding ion either Fe2+ or Fe3+. Dissolution of the magnetite will make the core-shell system unstable and break the bond between Fe-O-Si. To make sure that the magnetite is not dissolved in the acidic solution, we can test it by the use of an acid such as hydrochloric acid or nitric acid. The concentration of total iron as Fe2+ or Fe3+ can be an indicator if the magnetite is still strong. If high concentration of Fe3+ is found in the solution, we can say that the magnetite structure is collapsed and even broken down.
\n
The visual indication can be seen from the color of the dispersion of Fe3O4@SiO2 core-shell. The solution of Fe3+ in the solution is pale yellow. If the dispersion color is pale yellow, it can be concluded that magnetite does dissolve. The color is getting dark when the more magnetite dissolved in the dispersion. A combination of atomic absorption spectrometry and visual observation helps us make sure the magnetite core is still strongly intact.
\n
Fe3O4/SiO2 core-shell nanoparticles were obtained by dispersing Fe3O4 into the mixture solution of 80 mL of ethanol, 20 mL of deionized water, and 1.0 mL of concentrated aqueous ammonia solution (28 wt.%). After this, the mixture solution was homogenized by ultrasonication for 30 min to form a uniform dispersion. Subsequently, a certain amount of tetraethoxysilane (TEOS) was added dropwise into the solution with vigorous stirring. After stirring at room temperature for 6 h, the product was separated with a magnet bar, washed with deionized water for three times, and dried in vacuum at 50°C for 12 h. A series of SiO2@Fe3O4 particles were prepared with 1–9% SiO2 content [26].
\n
The silica coating used on a core particle has several advantages. The essential advantages of the silica coating compared with another inorganic (metal or metal oxide) or organic coating are as follows: It reduces the bulk conductivity and increases the suspension stability of the core particles. Also, silica is the most chemically inert material available; it can block the core surface without interfering in the redox reaction at the core surface [27]. There are two methods for coating Fe3O4 with silica, by acidic hydrolysis of silicate in aqueous solutions and the modified Stöber process [4, 28].
\n
The Stöber method consists of the alkaline hydrolysis of tetraethyl orthosilicate (TEOS) in ethanol/water mixture in the presence of Fe3O4 NPs [28]. The Stöber process is applied to the classic sol–gel process [29]. The Stöber synthesis has the advantage of being easy to scale up for commercial applications and the possibility to effortlessly transfer the nanoparticles into aqueous solutions [30]. Some methods that lead to the synthesis of Fe3O4/SiO2 are shown in Table 1.
\n
\n
\n
\n
\n
\n\n
\n
Core
\n
Shell
\n
\n\n\n
\n
Method
\n
Precursors
\n
Method
\n
Basic reagent
\n
\n
\n
Wet chemical reaction
\n
FeCl3, N2H4
\n
Sol–gel
\n
TEOS
\n
\n
\n
Wet chemical reaction
\n
FeCl3, FeSO4
\n
Hydrolysis
\n
Na2SiO3
\n
\n
\n
Wet chemical reaction
\n
FeCl3, FeSO4
\n
Hydrolysis
\n
Commercial SiO2
\n
\n
\n
A chemical reaction in microemulsion
\n
FeCl3, FeSO4
\n
Sol–gel reaction in microemulsion
\n
TEOS
\n
\n\n
Table 1.
Methods for synthesis of Fe3O4 coated with SiO2.
\n
About the modification and application of magnetic materials, a coating of Fe3O4 by the use of various materials has been reported elsewhere. TiO2@Fe3O4, TiO2@Fe3O4@chitosan, and methyl pyrazolone-functionalized TiO2@Fe3O4@chitosan were prepared for photocatalytic degradation of dyes [32]. They found that the core is important for separation and the shell is an active catalyst. The degradation of dye using these catalysts can reach up to 98–99%.
\n
Thioctic acid-modified silica-coated magnetite nanoparticles, RS-SR-NH-SiO2@Fe3O4, have been prepared, and its ability for the recovery of Au(III) in aqueous solutions was evaluated [31]. The Au(III) adsorption capacity of the produced adsorbent is about 25 mg/g. The possible interaction is shown in Figure 3. Another study shows the success of recovery of gold from copper anode slime by means of magnetite nanoparticles [33]. The surface of magnetite was also modified with oleic acid, methyl methacrylate, and ethylenediamine (EDA-MMA-OA@ Fe3O4) giving the adsorption of indium of about 54 mg/g [34].
\n
Figure 3.
Possible interaction between RS-SR-NH-SiO2@Fe3O4 and au(III) ions [31].
\n
An interesting example of functionalization of Fe3O4 is by the use of dithiocarbamate, and it is applied as a magnetic nano-adsorbent for recovery of precious metal nanoparticles by contacting the nano-adsorbent with Au, Ag, Pd, or Pt hydrosols [35]. The magnetic particles are very efficient for Au due to strong affinity of sulfur-containing groups at the magnetite surfaces with this metal. Since Au colloids are used in laboratory and industrial contexts, the material could have an impact on the development of nanotechnology to recover precious metals like Au [35] and Ag. Another trial is modification using chitosan and EDTA. It shows more selective for the quasi-precious metal of Cu than Cd and Pb [36].
\n
\n
\n
4. Surface functionalization of Fe3O4@SiO2−X
\n
In reaction (1), we can see the steps of surface modification of Fe3O4@SiO2 core-shell to form Fe3O4@SiO2−X, where X is a functional group. The layer of SiO2 was usually coated on the surface of Fe3O4 using the Stöber method. The prepared Fe3O4 nanoparticles were used as cores and dispersed in ethanol, and it was added to a three-neck round-bottom flask in ethanol and deionized water. The solution of the concentrated ammonia solution was added. After 15 min, TEOS was added dropwise in 10 min. The mixture was allowed for mechanical stirring for 8 h to perform the silica coating. The produced Fe3O4@SiO2 was separated and washed with deionized water and ethanol [37].
\n
Direct modification by the use of organic compound is also studied, without first modification by silica. Magnetic nanoparticles modified with third-generation dendrimers followed by ethylenediaminetetraacetic acid (EDTA) were prepared and tested for their performance for recovery of precious metals that are Pd(IV), Au(III), Pd(II), and Ag(I) in the aqueous system [38]. It is interesting that high valence Pd(IV) and Au(III) exhibit relatively better adsorption efficiency than that of Pd(II) and Ag(I) with lower valence. It suggests that the adsorption of precious metals by this type of materials modified with EDTA is a function of valence. When the competing ion such as Zn(II) presents, the adsorption efficiency of the adsorbent for all four precious metals, which are Pd(IV), Au(III), Pd(II), and Ag(I), reduces much.
\n
Magnetite nanoparticles could be directly modified with an organic compound of oleic acid. Iron oxide surface possibly bonds to carboxylic end of lauric acid [21]. However, this method of functionalization might not produce an acid-resistive magnetic adsorbent. The bond between lauric acid and magnetite could be easily damaged when the acidic solution is used. Therefore, the magnetite modified with lauric acid may find application in biological systems since both lauric acid and magnetite are biocompatible.
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Silane compound such as (3-aminopropyl)trimethoxysilane (APTMS) could be used to coat magnetite nanoparticles. The product can be described as Fe3O4@SiO2-CH3-NH2. Further surface modification by alginate gives Fe3O4@SiO2-CH3-NH2-AA. The alginate forms the outer shell of the magnetite by electrostatic interaction with amine [39]. Figure 1 shows a step-by-step extension of magnetite coating and functionalization. Silica coating will allow further functionalization via silanization, extension (additional of the spacer), and functional group attachment. The functional groups should be free to bond the metal ion either by an ionic or covalent coordination bond. Directed functional groups allow selective reaction with certain cation.
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\n
\n
5. Characterization
\n
Characterization of the magnetite can be done by at least five methods, which are vibrating sample magnetometer, powder X-ray diffraction, electron microscopy, elemental analysis, and infrared (IR) spectroscopy. The vibrating sample magnetometer (VSM) can reveal the magnetic properties of the magnetic materials. The microscopic images can be obtained commonly by the use of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM). Nanomaterials are best to characterize by TEM and AFM. The IR spectroscopy is useful to detect the functional groups present on the magnetite surface. The IR spectroscopy is one of the methods to make sure that functionalization of the surface is successful.
\n
For elemental analysis, a nondestructive energy dispersive X-ray spectrometry (EDS) can be used to estimate the chemical composition. The SEM is usually equipped with EDS system. The EDS results may lack precision and accuracy; however, it can detect the chemical composition in situ. The destructive methods such as atomic absorption spectrometry, UV–Vis spectrometry, and so forth may be used in place of EDS method. The destructive methods are usually not of choices for this type of materials.
\n
One major analytical method in the magnetite characterization is powder X‐ray diffraction. Figure 4 shows the XRD patterns of Fe3O4 and Fe3O4/SiO2 solid nanoparticle core-shell. The Fe3O4 diffraction patterns have five main peaks at 2θ values of 30.1°, 35.5°, 43.3°, 57.1°, and 62.5°. The Fe3O4 has a cubic system as confirmed by JCPDS Card No. 88–0315. The magnetite phase can be detected with certainty by XRD. However, when it is coated with silica, the intensity of the XRD peaks will be much diminished since silica is an amorphous solid. Further decrease in the XRD is expected after organic modification on top of the silica layer.
\n
Figure 4.
XRD patterns of Fe3O4 (top) and Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group (bottom) [3].
\n
The FT-IR could also be useful for more characterization of magnetic materials. It can offer details of the bond between the core, the shells, and the surface modifiers. Here is the example, the FT-IR spectra of Fe3O4 and Fe3O4/SiO2 nanoparticle core-shell are presented in Figure 5. Both spectra have a broad peak at 586 cm−1. The peak is attributed to the Fe-O stretching mode of magnetite. The peak at 3400 cm−1 is due to the O-H stretching mode. The sharp peak at 1100 cm−1 can be attributed to the Si-O-Si stretching mode. The Si-O bending vibration mode of the silanol group is seen at 964 cm−1. It indicates that the silica has coated well the outer surface of Fe3O4 particles [3]. The surface modification of Fe3O4/SiO2 nanoparticles by thiol groups can give a better interaction with [AuCl4]− ions in the solution. The FT-IR spectra of the Fe3O4/SiO2 nanoparticle core-shell after modification with thiol group are shown in Figure 5. The peak at 686 cm−1 is attributed to the C-S bending vibration mode. The peak at near 2570–2590 cm−1 is attributed to the stretching vibration mode of S-H. The S-H stretching vibration mode is not usually detected [2]. The band at around 2850–2900 cm−1 is due to the stretching vibration of C-H of methylene. This result suggests that the surface modification of Fe3O4/SiO2 nanoparticle core-shell is successful.
\n
Figure 5.
FT-IR spectra of resulted Fe3O4 (a), Fe3O4/SiO2 nanoparticle core-shell (b), and Fe3O4/SiO2 nanoparticle core-shell modified with a thiol group (c) [3].
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The covering of Fe3O4 nanoparticle core-shell by using silica does not only protect the magnetite core from dissolution in acid but also control the agglomeration of Fe3O4 particles. Silica acts as a capping agent for each Fe3O4 nanoparticle to form Fe3O4/SiO2 core-shell. Figure 6 shows the TEM images of Fe3O4/SiO2 nanoparticle core-shell. The Fe3O4/SiO2 nanoparticle core-shell has a size of approximately 10–20 nm. The size of Fe3O4/SiO2 core-shell can be observed. These results prove that the synthesis of Fe3O4/SiO2 nanoparticle core-shell is successful.
\n
Figure 6.
TEM image of Fe3O4/SiO2 nanoparticle core-shell [3].
\n
In situ analysis of adsorbent is preferable to understand the chemical composition of the product without a change in its nature. Figure 7 shows the EDX spectra of modified Fe3O4/SiO2 solid nanoparticle core-shell. The sulfur content is 1.32% (w/w). It suggests that thiol group is present on the surface of Fe3O4/SiO2 nanoparticle core-shell material. It confirms the FT-IR spectra. The modification of Fe3O4/SiO2 solid nanoparticle core-shell by 3-MPTS will give free thiol groups on the nanoparticles’ surface. The thiols are expected to form covalent coordination bond with the target ion.
\n
Figure 7.
EDX spectra of Fe3O4/SiO2 nanoparticles modified with thiol group [3].
\n
The EDX may also give details of atomic mapping across the sample, especially that of the functional group. For example, sulfur atom in the thiol group is mapped by the EDX method nicely. Functional groups such as amine, thiol, sulfonate, and phosphate may be better detected by EDX rather than destructive methods such as UV–Vis spectrophotometry.
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\n
\n
6. Adsorbent performance
\n
Table 2 shows a comparison of adsorbent performance for adsorption of precious metals especially gold and palladium [3, 38]. The first two rows show the adsorption performance of magnetic material modified with thiol and dendrimers. It shows that functionalization of the magnetite is very important to increase the adsorption capacity. Thiol group on the surface of magnetite produces high affinity toward Au(III). As we know, thiol can strongly react with gold to form a covalent bond. However, the adsorption capacity of magnetite is still far below that of adsorbent produced by the use of lignin as a precursor.
Comparison of adsorption capacities (qmax) of some adsorbents for selected precious metals from aqueous solution. Data presented here are based on the Langmuir isotherm.
\n
An adsorbent of magnetic nanoparticles modified by thiourea for effective and selective adsorption of precious metals like gold(III), palladium(II), and platinum(IV) in aqueous acid solution has also been reported. It needs contact time of less than 30 min to reach maximum capacity. Its maximum adsorption capacity of precious metals as determined by Langmuir model was 43.34, 118.46, and 111.58 mg/g for Pt(IV), Au(III), and Pd(II), respectively, at pH 2 and 25°C [40]. The adsorption is selective for Au(III) even in the presence of high concentrations of interfering ion Cu(II). The recycling was achieved by the use of a solution containing 0.7 M thiourea and 2% HCl. The result of the adsorption–desorption test shows that the adsorbent is reusable for the recovery of precious metals.
\n
In general, the adsorption capacity of the magnetite-based adsorbent can reach up to 118.46 mg/g, which is very promising. It may still be less than that of lignin derivatives. For chitosan-modified magnetite, it even can reach the capacity for gold(III) of 707 mg/g [41]. The core‐shell‐modifier based adsorbent may not have such a high adsorption capacity. The modification step was done through the reaction between chitosan and polymeric Schiff’s base of thiourea/glutaraldehyde in the presence of magnetite.
\n
After adsorption test, desorption of the adsorbed cation must also be examined. Complete desorption of the adsorbed cation indicates a better adsorbent performance. In most cases, the acids can desorb adsorbed ion from the surface. The desorption process may use strong acids such as HCl, H2SO4, and HNO3. The cation is believed to form complex coordination bonds with the surface, and leaching them is difficult.
\n
On the other hand, application of concentrated acid solution may damage the structure of adsorbent. Therefore, mildly acidic solutions are usually employed to release the cation from the adsorbent’s surface. People use a complexing agent to release the adsorbed metal cations. Thiourea and EDTA are of important environmentally friendly complexing agents.
\n
Thiourea solution in 1 M HCl was employed to liberate [AuCl4]− ions that had been adsorbed by the material [3]. Thiourea has a better affinity than that of thiol and amine groups. It can form a complex ion with [AuCl4]− ion to dissolve back into the solution. According to the HSAB theory, both thiol and [AuCl4]− ion are among the weak bases. A strong coordination bond forms between thiourea and [AuCl4]− ion.
\n
Figure 8 depicts the curve of desorption of [AuCl4]− ion by thiourea in 1 M HCl solution at various concentrations following adsorption by the magnetite modified with a thiol group. Dilute thiourea solution can only desorb 43 mg/g [AuCl4]− ion of initially adsorbed 68 mg/g or 60% of the total [AuCl4]− ions bond to the surface. Figure 9 displays schematic adsorption of [AuCl4]− ion by magnetite modified with a thiol group and desorption. The desorption is done by applying thiourea in HCl solution. The concentration of the thiourea is low. The thiol group may form a covalent coordination bond with [AuCl4]− ion on the adsorbent surface.
\n
Figure 8.
Profile of [AuCl4]− ion desorption by HCl/thiourea at various concentration [3].
\n
Figure 9.
Adsorption and desorption of AuCl4− ions by magnetite nanoparticles modified with a thiol group [3].
\n
\n
\n
7. Summary
\n
Modified magnetic adsorbents have been synthesized and used in the recovery of precious metals from aqueous solutions. Among the magnetic materials, magnetite is studied widely. Surface modification of nanoscale magnetite core is crucial to have a better adsorption capacity, stability, and turnover. The key issues of the magnetic adsorbent include size and shape of the core, choice of surface modification, adsorption capacity, stability, and recyclability. The size of the magnetite core is also better if it is in the nanoscale rather than in micron scale. It will improve the contact between pursued ions and adsorbent surface. The surface modification must have a good affinity toward certain precious metal cations. Many researchers attempt to combine adsorption capability and magnetic properties of the magnetite-based adsorbent for certain metal recovery from the solution. Selective adsorbents are also of interest for separation of precious metals from a complex system such as industrial waste. Adsorption selectivity is highly considered for complex matrices. Magnetite core has low stability in strongly acidic aqueous media. Coating with silica has two advantages, for protection against the acidic environment and a binding site for further functionalization. A suitable modification of the magnetic particles by coating or functionalization using inorganic components or organic molecules is usually needed.
\n
The synthesis of magnetite as the core material has been established. The use of salts of Fe(II) and Fe(III) with careful stoichiometric calculation is a must. The pH of the magnetic formation should also be controlled, either by the use of sodium hydroxide or ammonia solution. In many cases, ammonia can give better homogeneous particles. It may be better to add a stabilizing agent for reducing aggregation of the magnetite nanoparticle and improve the stability of the colloid. Coating of magnetite with silica has also been well understood. TEOS and TMOS are the main choices for the outer shell of the magnetite, although sodium silicate may work. Silica is a preferable coating since it is resistant to acid and base, which will protect the magnetite core.
\n
The final surface modification is functionalization of the silica with ligands that will strongly bind the cations. The end of the modification chain must have a special interaction with the cations, especially through coordination bonds. The functional groups could be an amine, carboxylate, thiol, sulfonate, amide, hydroxyl, and so on. Based on reagent availability, the functional groups determine the selectivity toward certain precious metal cations.
\n
The release of the adsorbed metal cations after being concentrated in the adsorbent can be realized using acids and strong complexing agents. The acids are usually not desirable since they can cause the magnetite core to dissolve. Dissolution will damage the structure of the magnetite, which may not be possible to reuse. Complexing agents such as thiourea and EDTA can give a better option to minimize the damage to the magnetite-based adsorbents.
\n
Purification of the recovered metals may be done through well-known processes. Electrochemical process is the best choice of metallurgy. Other methods by the use of chemical reduction could also be selected. In the large scale, we can consider blast furnace combined with a redox reaction. One important point to consider, the use of environmentally friendly reprocessing of the metals must always be prioritized.
\n
\n
\n
8. Future recommendation and direction
\n
The conventional metal reprocessing uses chemicals that are not environmentally friendly. The magnetite-based adsorbents offer technology that can reduce the application of toxic chemicals. The adsorbents give the possibility to reduce, reuse, and recycle for a few times. The magnetic core of the adsorbent is also readily synthesized with environmentally benign precursors. The coating with silica protects against acid and base media during application and recycle. The silica coating can also facilitate the attachment of the functional groups, which is critical in the modification step.
\n
The current advanced electronic devices utilize the precious metals in their important components. The waste of electronic devices grows rapidly along with an increase in smartphone and PC use. Computer parts like processors, memories, motherboards, hard drives, and CD/DVD drives contain gold and other precious metals such as silver, palladium, and so on. The conventional gold recovery process uses cyanide ions for complex ion formation and electrolysis. The current technology attempts to recover gold and other precious metals from computers’ and smartphones’ components by utilizing magnetite nanoparticles. The new magnetic materials are effective yet environmentally friendly to recover precious metals. The magnetic adsorbents could also be the future of reclaiming precious metals from the waste of the other industries.
\n
In the magnetic adsorbent development, the magnetite core could be possibly substituted with other oxides of transition metals such as manganese, cobalt, or nickel if they maintain strong magnetic characters. However, silica is the main choice for easy coating of the magnetic core, which also helps protect the magnetic core from dissolution in the acidic and basic media. The presence of the ligands on the surface of the magnetite-silica core-shell is critical for adsorption process. The environmentally safe polymers and simple molecules may be used to facilitate coordination bond with the target cations. The desorption process must be done using suitable solutions. The solution for desorption should leave the adsorbent in good shape for further reuse and turnover. The present technology available for purification of the recovered metals may apply electrochemical, chemical, and thermal processes.
\n
\n
Symbols and abbreviations
AFM
atomic force microscopy
APTMS
aminopropyl trimethoxysilane
DEG
diethylene glycol
EDTA
ethylenediamine tetraacetate
EDA-MMA-OA
ethylenediamine, methyl methacrylate, and oleic acid
EDX
energy dispersive X-ray spectroscopy
JCPDS
Joint Committee on Powder X-ray Diffraction Standards
MPTS
mercaptopropyltrimethoxysilane
NPs
nanoparticles
PVA
polyvinyl alcohol
qe
maximum capacity of adsorbent (mg/g)
SEM
scanning electron microscopy
TEOS
tetraethyl orthosilicate
TEM
transmission electron microscopy
VSM
vibrating sample magnetometer
\n',keywords:"magnetic nanoparticle, recovery, silica, precious metal, adsorption, desorption",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/62594.pdf",chapterXML:"https://mts.intechopen.com/source/xml/62594.xml",downloadPdfUrl:"/chapter/pdf-download/62594",previewPdfUrl:"/chapter/pdf-preview/62594",totalDownloads:1059,totalViews:413,totalCrossrefCites:2,dateSubmitted:"March 12th 2018",dateReviewed:"June 18th 2018",datePrePublished:"November 5th 2018",datePublished:"November 14th 2018",dateFinished:null,readingETA:"0",abstract:"Magnetic nanoparticles such as magnetite have been studied intensively for their unique properties that are susceptible to a magnetic field, ready to coat with silica and able to modify with a variety of functional groups. The magnetite-silica core-shell system offers flexibility for extensive modification. The magnetic core is also important in the separation by the use of a magnetic field. The shell, meanwhile, is needed for protection of the magnetic core and further modification. Functional groups at the surface shell are critical in the reaction with target precious metal ions during application. In this contribution, we will have a comprehensive look at the preparation, characterization, and use of the magnetite core-shell modified with functional groups as a magnetic adsorbent. After adsorption, the materials together with the ions can be recovered by the use of magnet before further separation and purification.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/62594",risUrl:"/chapter/ris/62594",signatures:"Roto Roto",book:{id:"7471",title:"Advanced Surface Engineering Research",subtitle:null,fullTitle:"Advanced Surface Engineering Research",slug:"advanced-surface-engineering-research",publishedDate:"November 14th 2018",bookSignature:"Mohammad Asaduzzaman Chowdhury",coverURL:"https://cdn.intechopen.com/books/images_new/7471.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"185329",title:"Prof.",name:"Mohammad Asaduzzaman",middleName:null,surname:"Chowdhury",slug:"mohammad-asaduzzaman-chowdhury",fullName:"Mohammad Asaduzzaman Chowdhury"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:null,sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Preparation of Fe3O4",level:"1"},{id:"sec_3",title:"3. Coating of Fe3O4 with SiO2",level:"1"},{id:"sec_4",title:"4. Surface functionalization of Fe3O4@SiO2−X",level:"1"},{id:"sec_5",title:"5. Characterization",level:"1"},{id:"sec_6",title:"6. Adsorbent performance",level:"1"},{id:"sec_7",title:"7. Summary",level:"1"},{id:"sec_8",title:"8. Future recommendation and direction",level:"1"},{id:"sec_11",title:"Symbols and abbreviations",level:"1"}],chapterReferences:[{id:"B1",body:'Haw CY et al. Hydrothermal synthesis of magnetite nanoparticles as MRI contrast agents. Ceramics International. May 2010;36(4):1417-1422\n'},{id:"B2",body:'Zhang S et al. Thiol modified Fe3O4@SiO2 as a robust, high effective, and recycling magnetic sorbent for mercury removal. Chemical Engineering Journal. Jun. 2013;226:30-38\n'},{id:"B3",body:'Roto R, Yusran Y, Kuncaka A. Magnetic adsorbent of Fe3O4@SiO2core-shell nanoparticles modified with thiol group for chloroauric ion adsorption. Applied Surface Science. 2016;377:30-36\n'},{id:"B4",body:'Morel A et al. Sonochemical approach to the synthesis of Fe3O4@SiO2 Core−Shell nanoparticles with tunable properties. ACS Nano. 2008;2(5):847-856\n'},{id:"B5",body:'El-kharrag R, Amin A, Greish YE. Low temperature synthesis of monolithic mesoporous magnetite nanoparticles. Ceramics International. Jan. 2012;38(1):627-634\n'},{id:"B6",body:'Lin J, Lai Q, Liu Y, Chen S, Le X, Zhou X. Laccase–Methacryloyl functionalized magnetic particles: Highly immobilized, reusable, and efficacious for methyl red decolourization. International Journal of Biological Macromolecules. 2017;102:144-152\n'},{id:"B7",body:'Peng L et al. Modifying Fe3O4 nanoparticles with humic acid for removal of Rhodamine B in water. Journal of Hazardous Materials. 2012;209-210:193-198\n'},{id:"B8",body:'Nigam S, Barick KC, Bahadur D. Development of citrate-stabilized Fe3O4 nanoparticles: Conjugation and release of doxorubicin for therapeutic applications. Journal of Magnetism and Magnetic Materials. 2011;323(2):237-243\n'},{id:"B9",body:'Zhang JM, Zhai SR, Zhai B, Da An Q, Tian G. Crucial factors affecting the physicochemical properties of sol-gel produced Fe3O4@SiO2-NH2 core-shell nanomaterials. Journal of Sol-Gel Science and Technology. 2012;64(2):347-357\n'},{id:"B10",body:'Hakami O, Zhang Y, Banks CJ. Thiol-functionalised mesoporous silica-coated magnetite nanoparticles for high efficiency removal and recovery of hg from water. Water Research. 2012;46(12):3913-3922\n'},{id:"B11",body:'Aghaei E, Alorro R, Encila A, Yoo K. Magnetic adsorbents for the recovery of precious metals from leach solutions and wastewater. Metals (Basel). 2017;7(12):529\n'},{id:"B12",body:'Narayan R editor. Nanobiomaterials: Nanostructured Materials for Biomedical Applications, Magnetic Nanoparticle Synthesis. Amsterdam: Elsevier Ltd; 2017. Chapter 8. p. 197‐229\n'},{id:"B13",body:'Grüttner C, Müller K, Teller J, Westphal F. Synthesis and functionalisation of magnetic nanoparticles for hyperthermia applications. International Journal of Hyperthermia. 2013;29(8):777-789\n'},{id:"B14",body:'Ni S et al. Hydrothermal synthesis of Fe3O4 nanoparticles and its application in lithium ion battery. Materials Letters. 2009;63(30):2701-2703\n'},{id:"B15",body:'Valenzuela R et al. Influence of stirring velocity on the synthesis of magnetite nanoparticles (Fe3O4) by the co-precipitation method. Journal of Alloys and Compounds. Nov. 2009;488(1):227-231\n'},{id:"B16",body:'Mahmoud ME, Amira MF, Zaghloul AA, Ibrahim GAA. Microwave-enforced sorption of heavy metals from aqueous solutions on the surface of magnetic iron oxide-functionalized-3-aminopropyltriethoxysilane. Chemical Engineering Journal. 2016;293:200-206\n'},{id:"B17",body:'Yu LQ, Zheng LJ, Yang JX. Study of preparation and properties on magnetization and stability for ferromagnetic fluids. 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Low-dimensional systems and nanostructures. 2010;42(6):1824-1829\n'},{id:"B23",body:'Yang C, Yan H. A green and facile approach for synthesis of magnetite nanoparticles with tunable sizes and morphologies. Materials Letters. 2012;73:129-132\n'},{id:"B24",body:'Feng X, Guo H, Patel K, Zhou H, Lou X. High performance, recoverable Fe3O4 ZnO nanoparticles for enhanced photocatalytic degradation of phenol. Chemical Engineering Journal. 2014;244:327-334\n'},{id:"B25",body:'Habila MA, Alothman ZA, El-Toni AM, Labis JP, Soylak M. Synthesis and application of Fe3O4@SiO2@TiO2 for photocatalytic decomposition of organic matrix simultaneously with magnetic solid phase extraction of heavy metals prior to ICP-MS analysis. Talanta. 2016;154:539-547\n'},{id:"B26",body:'Liu H, Jia Z, Ji S, Zheng Y, Li M, Yang H. Synthesis of TiO2/SiO2@Fe3O4 magnetic microspheres and their properties of photocatalytic degradation dyestuff. Catalysis Today. 2011;175(1):293-298\n'},{id:"B27",body:'Ghosh Chaudhuri R, Paria S. Core/shell nanoparticles: Classes, properties, synthesis mechanisms, characterization, and applications. Chemical Reviews. 2012;112(4):2373-2433\n'},{id:"B28",body:'Stober W, Fink A. Controlled growth of Monodispersed silica spheres in the Micron size range. Journal of Colloid and Interface Science. 1968;26:62-69\n'},{id:"B29",body:'Liu J et al. Extension of the stöber method to the preparation of monodisperse resorcinol-formaldehyde resin polymer and carbon spheres. Angewandte Chemie, International Edition. 2011;50(26):5947-5951\n'},{id:"B30",body:'Gholami T, Salavati-niasari M, Bazarganipour M. Superlattices and microstructures synthesis and characterization of spherical silica nanoparticles by modified Stöber process assisted by organic ligand. Superlattices and Microstructures. 2013;61:33-41\n'},{id:"B31",body:'Abd Razak NF, Shamsuddin M, Lee SL. Adsorption kinetics and thermodynamics studies of gold(III) ions using thioctic acid functionalized silica coated magnetite nanoparticles. Chemical Engineering Research and Design. 2018;130:18-28\n'},{id:"B32",body:'Abdelwahab NA, Morsy EMH. Synthesis and characterization of methyl pyrazolone functionalized magnetic chitosan composite for visible light photocatalytic degradation of methylene blue. International Journal of Biological Macromolecules. 2018;108:1035-1044\n'},{id:"B33",body:'Ranjbar R, Naderi M, Omidvar H, Amoabediny G. Gold recovery from copper anode slime by means of magnetite nanoparticles (MNPs). Hydrometallurgy. 2014;143:54-59\n'},{id:"B34",body:'Chiou CS, Chuang KJ, Chen HW, Chen YC. Magnetite modified with amine polymer to adsorb indium ions. Powder Technology. 2015;279:247-253\n'},{id:"B35",body:'Lopes JL, Marques KL, Girão AV, Pereira E, Trindade T. Functionalized magnetite particles for adsorption of colloidal noble metal nanoparticles. Journal of Colloid and Interface Science. 2016;475:96-103\n'},{id:"B36",body:'Ren Y, Abbood HA, He F, Peng H, Huang K. Magnetic EDTA-modified chitosan/SiO2/Fe3O4 adsorbent: Preparation, characterization, and application in heavy metal adsorption. Chemical Engineering Journal. 2013;226:300-311\n'},{id:"B37",body:'Habila MA, Alothman ZA, El-Toni AM, Labis JP, Soylak M. Synthesis and application of Fe3O4@SiO2@TiO2 for photocatalytic decomposition of organic matrix simultaneously with magnetic solid phase extraction of heavy metals prior to ICP-MS analysis. Talanta. 2016;154:539-547\n'},{id:"B38",body:'Yen CH, Lien HL, Chung JS, Der Yeh H. Adsorption of precious metals in water by dendrimer modified magnetic nanoparticles. Journal of Hazardous Materials. 2017;322:215-222\n'},{id:"B39",body:'Yang L et al. Modification and characterization of Fe3O4 nanoparticles for use in adsorption of alkaloids. Molecules. 2018;23:562\n'},{id:"B40",body:'Lin TL, Lien HL. Effective and selective recovery of precious metals by thiourea modified magnetic nanoparticles. International Journal of Molecular Sciences. 2013;14(5):9834-9847\n'},{id:"B41",body:'Donia AM, Atia AA, Elwakeel KZ. Recovery of gold(III) and silver(I) on a chemically modified chitosan with magnetic properties. Hydrometallurgy. 2007;87(3-4):197-206\n'},{id:"B42",body:'Chang YC, Chen DH. Recovery of gold(III) ions by a chitosan coated magnetic nano-adsorbent. Gold Bulletin. 2006;39(3):98-102\n'},{id:"B43",body:'Parajuli D, Kawakita H, Inoue K, Funaoka M. Recovery of gold(III), palladium(II), and platinum(IV) by aminated lignin derivatives. Industrial and Engineering Chemistry Research. 2006;45(19):6405-6412\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Roto Roto",address:"roto05@ugm.ac.id",affiliation:'
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Yogyakarta, Indonesia
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Open Access publishing helps remove barriers and allows everyone to access valuable information, but article and book processing charges also exclude talented authors and editors who can’t afford to pay. The goal of our Women in Science program is to charge zero APCs, so none of our authors or editors have to pay for publication.
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