Bismuth-based electrodes for determination of Pb (II) and Cd (II) using anodic stripping voltammetry.
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More than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\\n\\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\\n\\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\\n\\nAdditionally, each book published by IntechOpen contains original content and research findings.
\\n\\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\\n\\n\\n\\n
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'
Simba Information has released its Open Access Book Publishing 2020 - 2024 report and has again identified IntechOpen as the world’s largest Open Access book publisher by title count.
\n\nSimba Information is a leading provider for market intelligence and forecasts in the media and publishing industry. The report, published every year, provides an overview and financial outlook for the global professional e-book publishing market.
\n\nIntechOpen, De Gruyter, and Frontiers are the largest OA book publishers by title count, with IntechOpen coming in at first place with 5,101 OA books published, a good 1,782 titles ahead of the nearest competitor.
\n\nSince the first Open Access Book Publishing report published in 2016, IntechOpen has held the top stop each year.
\n\n\n\nMore than half of the publishers listed alongside IntechOpen (18 out of 30) are Social Science and Humanities publishers. IntechOpen is an exception to this as a leader in not only Open Access content but Open Access content across all scientific disciplines, including Physical Sciences, Engineering and Technology, Health Sciences, Life Science, and Social Sciences and Humanities.
\n\nOur breakdown of titles published demonstrates this with 47% PET, 31% HS, 18% LS, and 4% SSH books published.
\n\n“Even though ItechOpen has shown the potential of sci-tech books using an OA approach,” other publishers “have shown little interest in OA books.”
\n\nAdditionally, each book published by IntechOpen contains original content and research findings.
\n\nWe are honored to be among such prestigious publishers and we hope to continue to spearhead that growth in our quest to promote Open Access as a true pioneer in OA book publishing.
\n\n\n\n
\n'}],latestNews:[{slug:"intechopen-signs-new-contract-with-cepiec-china-for-distribution-of-open-access-books-20210319",title:"IntechOpen Signs New Contract with CEPIEC, China for Distribution of Open Access Books"},{slug:"150-million-downloads-and-counting-20210316",title:"150 Million Downloads and Counting"},{slug:"intechopen-secures-indefinite-content-preservation-with-clockss-20210309",title:"IntechOpen Secures Indefinite Content Preservation with CLOCKSS"},{slug:"intechopen-expands-to-all-global-amazon-channels-with-full-catalog-of-books-20210308",title:"IntechOpen Expands to All Global Amazon Channels with Full Catalog of Books"},{slug:"stanford-university-identifies-top-2-scientists-over-1-000-are-intechopen-authors-and-editors-20210122",title:"Stanford University Identifies Top 2% Scientists, Over 1,000 are IntechOpen Authors and Editors"},{slug:"intechopen-authors-included-in-the-highly-cited-researchers-list-for-2020-20210121",title:"IntechOpen Authors Included in the Highly Cited Researchers List for 2020"},{slug:"intechopen-maintains-position-as-the-world-s-largest-oa-book-publisher-20201218",title:"IntechOpen Maintains Position as the World’s Largest OA Book Publisher"},{slug:"all-intechopen-books-available-on-perlego-20201215",title:"All IntechOpen Books Available on Perlego"}]},book:{item:{type:"book",id:"7023",leadTitle:null,fullTitle:"Ticks and Tick-Borne Pathogens",title:"Ticks and Tick-Borne Pathogens",subtitle:null,reviewType:"peer-reviewed",abstract:"It is vital to understand ticks and tick-borne pathogens as well as their impact on humans. 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\r\n\tThe book, Chitin and Chitosan - Physicochemical Properties and Industrial Applications, provides an overview of the extraction, modification, characterization, and application of chitin and chitosan derivatives from crustacean by-products and their physicochemical properties. It presents and explains important studies and develops new and innovative methods of biological and physicochemical analysis in the fields of organic and mineral environmental pollution, corrosion inhibitors, drug delivery systems, superabsorbent materials, nanotechnology, textiles, biotechnology, and biomedical sciences.
\r\n\r\n\tOur book will distinguish itself from competing volumes by discussing the synthesis, purification, analysis, and properties of chitin-chitosan polymers as a renewable source of natural biodegradable polysaccharides and also by presenting various practical and potential new applications of these materials. It is highly recommended for industrial personnel involved in bioprocesses, biochemistry, microbiology, bioengineering, food engineering, medical and pharmaceutical industries as well as for readers interested in environmental protection and who wish to specialize in chitin and chitosan derivative technologies.
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Member of the Quebec Order of Chemists and holder of more than ten registered patents.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"224783",title:"Prof.",name:"Mohammed",middleName:null,surname:"Berrada",slug:"mohammed-berrada",fullName:"Mohammed Berrada",profilePictureURL:"https://mts.intechopen.com/storage/users/224783/images/system/224783.jpg",biography:"Professor Berrada joined the Hassan II University of Casablanca in 1994 and assumed many responsibilities which led him to head the Casablanca Innovation and Technology Platform. He has set up in his Laboratory of Biomolecules and Organic Synthesis, a research program in the fields of thermostable and photosensitive materials, intelligent polymers, hydrogels, and nanoparticles for drug delivery systems, biodegradable superabsorbents, and corrosion inhibitors. Professor Berrada received a Ph.D. in Polymer Science from the Macromolecular Sciences Division of Pierre and Marie Curie University in 1992, and another Ph.D. in Organic Chemistry from Ben M\\'Sik Faculty of Sciences in 1998. He completed postdoctoral training at the Engineering Department of Tokyo University of Agriculture and Technology in Japan in 1994. From 2006 to 2009, Professor Berrada was Director of Research and Development Department at Intersand Inc., where he patented the innovative OdourLock litter technology which was a breakthrough and a huge success for the company. He joined Lysac Technologies in January 2003 and took on the task of creating and leading the Department of Polymer Chemistry. Prof. Berrada has also been involved in many University-Industry transfer technology projects. In 1998, he joined the Department of Radiation Oncology at McGill University. In 2000, he joined Biosyntech Inc. a Canadian pharmaceutical industry and was Director of the Therapeutic Delivery Department. 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Cosmetic and pharmaceutical uses of bismuth compounds can be dated back over two centuries ago. Bismuth materials including metal bismuth as well as its compounds have been long regarded as green materials due to their eco-friendliness. Owing to their biocompatibility, extensive research of bismuth has been conducted in diverse fields. For example, the layered structure of bismuth oxychloride (BiOCl) enabling it to give pearl-like coloring was used in cosmetics. Electrodes decorated with bismuth-based materials such as Bi(NO3)3 and Bi2O3 have been used for the electrochemical stripping analysis of heavy metals as an alternative method to replace toxic mercury-based ones [1, 2, 3]. In particular, owing to its large surface area, extraordinary electronic transport properties and high electrocatalytic activities, BiOCl has been extensively studied especially for industrial purpose such as photocatalytic/electrochemical materials [4, 5]. Notably, it was reported that bismuth subsalicylate (BSS), the active ingredient of an antacid drug with the trademark of Pepto-Bismol that was approved for sale over a century in North America, is hydrolyzed into BiOCl in the stomach [6, 7, 8, 9], suggesting its organism safety for clinical practice. Meanwhile, because of their therapeutic efficacy to deal with gastrointestinal disorders and microbial infections, bismuth-based conjugates such as colloidal bismuth subcitrate have been explored in the pharmaceutical industry.
Despite the extraordinary photo/electro-chemical properties, the layer structure of bismuth-related material typified by BiOCl may limit its practical applications. Therefore, in an effort to obtain BiOCl-based material of defined morphology, mesoporous silica materials including Korea Advanced Institute of Science and Technology-6 (KIT-6) have been tested as structural support to produce BiOCl-KIT-6 composites. As shown in Figure 1A, scanning electron microscopic image (SEM) of BiOCl has revealed its layer assembly, which was composed of microspheres with a diameter of about 3 μm. By comparison, BiOCl-KIT-6 composites exhibited a relatively large form distributing in a size range of tens of micrometers (Figure 1B) with a raspberry-like display of bunched balls. It was found that both BiOCl and BiOCl-KIT-6 composites were composed of nanoplates of several nanometers in thickness, aligning radically and tightly to form hierarchical microspheres. X-ray diffraction (XRD) analysis was performed to study the crystallographic structure of the BiOCl-KIT-6 composites. As shown in Figure 2, the well-crystallized phase of BiOCl-KIT-6 composite agreed well with that of the tetragonal BiOCl (JCPDS Card No.06-0249). The peaks located at 24.0°, 34.8°, and 36.5° correspond to (002), (012), and (003) crystalline planes of the BiOCl structure, respectively, representing the characteristics of lamellar structures. The crystallite size (average size of the coherent scattering region) for the BiOCl component was found to be 17.8 nm, calculated according to the Scherrer formula [10].
SEM images of (A) BiOCl (Adapted from Ref. [
XRD pattern of BiOCl-KIT-6 composite (adapted from Ref. [
The method to achieve bismuth-based electrode mainly included in situ plating and ex situ plating. The in situ plating involves the addition of Bi3+ into the sample solution. The bismuth film was formed on the surface of the electrode through the deposition during analyzing process. This method is limited as the assay pH of the sample solution has to be kept acidic. The ex situ plating includes plating the bismuth film on the electrode prior to the analysis of the sample solution. As such, preforming bismuth film on the electrode surface is not influenced by the assay conditions, ex situ method is relatively versatile for the real analysis though additional cautions and preparations are needed compared with in situ one. It is worth mentioning that bismuth-based electrode prepared by ex situ method can be reused. After the measurement, the bismuth-based electrode can be reactivated by holding the electrode at an adequate potential, which is more negative than the oxidation potential of bismuth while more positive than the oxidation stripping potential of analyzed metal ions. Therefore, after the reactivation, the bismuth-based electrode can be regenerated without any possible interference of deposited metals.
The application of bismuth-based electrode for heavy metal detection dated back to 2000 when Wang and coauthors tried to plate thin bismuth films on the carbon electrode as an alternative to mercury-based electrode [1]. The main advantage of bismuth-based material modified electrode is its nontoxicity to the environment as well as the biosafety for the operational personnel. Meanwhile, the bismuth-based sensors provide detection sensitivity and accuracy comparable to that of mercury-based ones [11], which are attractive for practical applications. Recently, bismuth-based sensors, exhibiting improved separation ability of intermetallic compounds, compared with mercury-based ones, have been used to evaluate heavy metals such as Cd2+ and Pb2+. These toxic heavy metals originating from severe environmental conditions including mining area, smelting works, and sewage plant [12] are harmful for the public health.
Nowadays, electrochemical methods owing to their portability, ultrasensitivity, readiness, and low cost have become useful and efficient for the trace determination of heavy metals [13, 14, 15, 16, 17]. Among them, anodic stripping voltammetry (ASV), which involves an effective preconcentration step to form metals on the electrode surface by reducing metal ions in the assay solution, followed by a sensitive stripping analysis where metals were reoxidized contributing to a remarkable signal-to-noise ratio, has been intensively employed in this aspect during the past decade (Figure 3). The amplified stripping signal resulting from bismuth-based electrodes reflects the ability of bismuth to form “fused” multicomponent alloys with targeted heavy metals [18]. Bismuth-based sensors thus hold potentials for the assays of heavy metal with applications ranging from continuous remote sensing to disposable chips. Since the bismuth-based electrode was applied for the determination of heavy metals in 2000 [1], many reports related to various bismuth-based material modified electrodes have been devoted to this area. In 2008, Xu and coworkers used a Nafion-coated bismuth electrode to achieve the simultaneous determination of three heavy metals including Pb2+, Cd2+, and Zn2+ in vegetables using differential pulse anodic stripping voltammetry [19]. In 2014, Sosa and coworkers analyzed Cd2+ and Pb2+ in groundwater based on sputtered bismuth screen-printed electrode [20]. In 2015, Cerovac and coworkers used the bismuth-oxychloride particle-multiwalled carbon nanotube composite-modified glassy carbon electrode to detect trace-level lead and cadmium in sediment pore water [21]. And it is also readily possible to evaluate the heavy metal amounts of human blood sample. For example, Song and coworkers determined Cd2+ in blood samples based on BiOCl-KIT-6 modified glassy carbon electrode [11]. During the past decade, many studies have introduced a number of trace heavy metal detection methods based on bismuth-based electrode. Some typical bismuth-based sensors as well as the resulting analytical performance are summarized in Table 1.
A schematic diagram of measurement of heavy metal ions using anodic stripping voltammetry.
Sensor | Method | Deposit. potent. (v) | Deposit. time (s) | Linear range (μg/L) | LOD(μg/L) | Ref. | ||
---|---|---|---|---|---|---|---|---|
Pb | Cd | Pb | Cd | |||||
Bi-CNT SPE | SWASV | −1.4 | 300 | 2–100 | 2–100 | 1.3 | 0.7 | [27] |
NCBFE | DPASV | −1.4 | 180 | 4–36 | 4–36 | 0.17 | 0.17 | [19] |
Bi/GCE | SWASV | −1.2 | 600 | 5–60 | 5–60 | 0.8 | 0.4 | [28] |
BispSPE | DPASV | −1.3 | 360 | 0.5–20 | 0.3–12 | 0.16 | 0.10 | [20] |
BiOCl/MWCNT-GCE | SWASV | −1.2 | 120 | 5–50 | 5–50 | 0.57 | 1.2 | [21] |
BiOCl-KIT-6/GCE | SWASV | −1.3 | 120 | 0.2–300 | 0.2–300 | 0.05 | 0.06 | [12] |
Bismuth-based electrodes for determination of Pb (II) and Cd (II) using anodic stripping voltammetry.
Bi-CNT SPE, bismuth-modified carbon nanotube modified screen-printed electrode; NCBFE, Nafion-coated bismuth film electrode; Bi/GCE: bismuth nanoparticles modified GCE; BispSPE, sputtered bismuth screen-printed electrode; MWCNT, multiwalled carbon nanotube; SWASV, square wave anodic stripping voltammetry; DPASV, differential pulse anodic stripping voltammetry.
Nevertheless, in comparison with mercury-based electrode, bismuth-based one often works well in a relatively narrow potential window, particularly being in a more negative anodic range due to the fact that bismuth is more easily oxidized than mercury. Meanwhile, the cathodic limit of bismuth-based electrode posed by hydrogen reduction is close to that of mercury-based one. Therefore, the accessible potential window of bismuth-based electrode is narrower than that made of mercury. Additionally, it was found that the potential window of bismuth-based electrode was strongly affected by the pH values of the sample solution. The relationship of operational potential windows of bismuth-based electrode and assay pH is shown in Table 2 [22]. Moreover, it was observed that the constructed BiOCl-KIT-6/GCE possessed a wide potential window ranging from −1.22 to −0.25 V versus SCE by recording the CV spectra of electrode in 0.1 M acetate buffer (pH 4.5) (Figure 4). The wide potential window of BiOCl-KIT-6/GCE may permit the simultaneous determination of Zn2+ (stripped at −1.15 V), Pb2+ (stripped at −0.58 V) and Cd2+ (stripped at −0.83 V). It should be noted that the stripping analysis of heavy metals is limited if oxidation potentials of analyzed metals are close to or more positive than that of bismuth such as Cu, Sn, and Sb.
Medium | pH | Anodic limit (V) | Cathodic limit (V) | Potential window (V) |
---|---|---|---|---|
0.1 M HClO4 | 1.00 | −0.05 | −1.05 | 1.10 |
0.2 M HAc-NaAc | 4.24 | −0.25 | −1.25 | 1.00 |
0.1 M NaOH | 12.17 | −0.55 | −1.55 | 1.00 |
Operational potential of bismuth-based materials plated on carbon-paste electrodes at different pH (Data taken from Ref. [22]).
Cyclic voltammetry (CV) analysis of BiOCl-KIT-6/GCE in acetate buffer solution (0.1 M, pH 4.5) (adapted from Ref. [
In the aspect of heavy metal measurement, many earlier studies have focused on the design of bismuth-based sensors as well as the detection principle. However, their applications to environmental, food, and clinical samples have just started. For example, by the use of anodic stripping voltammetry, cadmium and lead at trace levels in environmental samples [23, 24], food products [25, 26] and biological fluids [11] have been determined. Using square-wave anodic stripping voltammetry (SWASV), the constructed BiOCl-KIT-6/GCE applied to the determination of cadmium-spiked human blood samples resulted in a calibration curve of Cd2+ with 2 linear ranges from 0.5 to 10 and from 10 to 300 μg/L (Figure 5), respectively, and a detection limit of 65 ng/L. As shown in Figure 6, a good agreement between the detection methods of SWASV and inductively coupled plasma mass spectrometry (ICP-MS) was observed [11]. Moreover, the BiOCl-KIT-6/GCE could be repeatedly used for at least 30 continuous times in one day and at least 10 continuous days with a marginal reduction of stripping peak current of 6.8 and 3.6%, respectively.
(A) Square-wave anodic stripping voltammetric (SWASV) responses of peak current on the concentration of Cd2+ using BiOCl-KIT-6/GCE in acetate buffer solution (pH 4.5) at the deposition potential of −1.3 V and deposition time of 120 s. (B) Calibration curves of Cd2+ over a concentration range of 0.5–300 μg/L (adapted from Ref. [
The determination results of blood cadmium concentration by anodic stripping voltammetry (ASV) using BiOCl-KIT-6/GCE in comparison with ICP-MS assay (adapted from Ref. [
Despite considerable progress achieved during the past decade, most of the earlier studies have mainly explored various bismuth-based materials towards the sensor fabrication. Therefore, practical concerns still remain to be addressed to fulfill the demands of environmental protection and so on. Further works to utilize the constructed sensor under harsh operational conditions and to simply the assay procedures are still needed in the future.
Bismuth is a heavy metal element located close to lead and tin elements in the periodic table of elements, and thus shares similar physicochemical properties with these elements. But different from lead and tin, bismuth is usually regarded as nontoxic and biologically safe. Therefore, bismuth as well as its derivate has been extensively explored in biomedical applications. For example, bismuth salts are valuable for synthesis of various bismuth-based complexes as the active ingredients for pharmaceutical uses. The first report on bismuth-containing medicine in 1786 revealed its efficacy in the treatment of dyspepsia. And since then, there is a growing number of bismuth complexes which were explored to deal with gastrointestinal disorders and microbial infections including syphilis, diarrhea, gastritis, and colitis, which point out desirable therapeutic effects yet low toxicity after the intake of drug molecules.
In the laboratory, the antimicrobial activities of bismuth-based materials can be evaluated by recording the growth curve of model bacteria such as Gram-positive
Growth curves of
In the presence and absence of BiOCl-KIT-6 suspension (200 μg/mL),
Bismuth complex | Name of pharmaceuticals |
---|---|
Bismuth potassium citrate | Livzon Dele, Bielomatik |
Bismuth subcitrate | De-nol, Tripotassium dicitratobismuthate |
Bismuth citrate | Ranitidine |
Colloidal bismuth pectin | Colloidal bismuth pectin capsules |
Bismuth aluminate | Debitai, Compound bismuth aluminate tablets |
Bismuth-containing drugs for the treatment of gastrointestinal diseases.
Over the years, to produce a number of bismuth complexes for biomedical uses, the synthesis methods have also historically evolved, which mainly include hydrothermal, solvothermal, and microwave synthesis. Hydrothermal synthesis is a method to synthesize single crystals from high temperature aqueous solutions at high vapor pressures. Chen et al. synthesized bismuth-amino acid coordination polymers (BACPs) with different sizes by heating the aqueous reacting solution of Bi(NO3)3·5H2O and asparagine at different temperatures [30]. The prepared BACPs synthesized in a facile green hydrothermal method exhibited unique biological activities and potential applications in biomedicine. He et al. prepared low-toxicity bismuth asparagine coordination polymer spheres (BACP-2) with sphere-like microstructures of an average 800 nm in diameter through a hydrothermal reaction at 80°C overnight [31]. Solvothermal synthesis is usually carried out in organic media to produce chemicals of refined crystallinity and morphology through a combination of sol-gel and hydrothermal routes. Andrews and coworkers have developed two new bis-carboxylate Bi(III) complexes including PhBi(
(A) Structure of (Bi(H2L)(NO3)2)NO3 with atomic numbering scheme. (B) Polyhedra showing distorted geometry around the bismuth atom. H2L, 2,6-diacetylpyridine bis(4
Several bismuth derivates have revealed antibacterial and antifungal activities. For example, (Bi(H2L)(NO3)2)NO3 shows higher antibacterial properties with the minimum inhibitory concentration (MIC) of 10.66 μM against Gram-positive bacteria
It should be noted that although bismuth complexes have been widely applied for medical practice against
Because of the nontoxicity of bismuth (III) salts, there is growing interest to explore various bismuth (III) salts for diverse applications including stripping analysis of heavy metals as well as antimicrobial agents. The bismuth-based sensors for the heavy metals are extensively studied in an effort to replace the mercury-based methods. The precise control of morphology and surface properties of bismuth-based materials on the modified electrode will greatly determine the sensitivity and accuracy of the constructed sensors. On the other hand, bismuth-based compounds as the inorganic pharmaceutical molecules may offer advantages over organic ones for biomedical use. As the dosage is the major cause of neurotoxicity of bismuth compounds, it is of importance to monitor the in vivo efficacy of bismuth-based pharmaceuticals. Along this direction, some cargo molecules of ordered structure such as metal-organic frameworks (MOFs) for the controlled release of bismuth hold potentials to improve the curative effect.
The work was supported by National Natural Science Foundation of China (U1703118), a project funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD), Jiangsu Shuangchuang Program, Open Funds of the State Key Laboratory for Chemo/Biosensing and Chemometrics (2016015) and the National Laboratory of Biomacromolecules (2017kf05) and Jiangsu Specially-Appointed Professor project, China.
In this section, first of all the history and the literature data of the rapid tooling will be mentioned. Then, the AM using methods of rapid tooling will be explained in detail. Finally, examples to be taken into consideration when making the tool will be given basic flow chart of the processes can be seen in Figure 1.
Data transfer between the computer-aided design (CAD) and the RP system [
AM techniques for tool production (known in literature rapid tooling [RT]) provide efficiency in terms of time and cost, while RT is often the best known manufacturing method for complicated structures in low numbers [2]. AM techniques for manufacturing, prototyping, and tool production methods can also allow producers to manufacture high-quality elements in a short period [3, 4]. In today’s world, with the technology advancing rapidly, companies are looking for ways to manufacture varied and complicated items with high quality while reducing the cost and time needed [5].
AM techniques for tool production defines a method resulting from mixing AM techniques for prototyping with standard tooling disciplines to produce a die rapidly or components of a functional model from CAD information at a reduced cost and in less time than conventional machining methods.
There are two main categories. One category includes indirect methods using AM techniques for prototyping master designs to manufacture a mold, while the other category is a direct strategy, where the rapid prototyping machine constructs the real inserts of the core and cavity mold.
Due to its market potential, many businesses prefer AM techniques for tool produce and growth. Each method comes with a number of strengths that are contracted by limitations. Yet these advances cause a flurry of requests from businesses in the Americas, Europe, Asia, and other advanced markets due to their potential effect. Meanwhile, in both of these methods, numerous facilities are working hard to determine whether the time is correct to phase further information can be seen in Table 1.
To achieve various lead times, expenses, and process capabilities, there occurred several pattern-based methods in manufacturing a mold. To compose a pattern, the precision of RP processes gets considered with each part structure and the precision of the RP process preferred:
Vacuum casting.
Kirksite tooling.
Electroforming.
RTV silicone rubber molds.
Wax injection molding.
RIM.
Spin casting.
Plaster molds.
Rapid solidification process.
Sprayed steel.
Cast resin tooling.
Investment casting has been used for thousands of years as a manufacturing method and is particularly suited to finely detailed metal parts being formed and high melting point metals being used.
Founded in 1947, Vaupell uses SLA patterns for casting to quickly deliver 3D-printed patterns for casting to customers in aerospace industry. Here, AM (SLA) is used to manufacture a sacrificial model. Using this sacrificial model, investment casting is carried out as it would traditionally be the model with a ceramic coating, scorching the model, filling the remaining ceramic shell with molten metal, and removing the ceramic case after the metal has been solidified and cooled [6].
As a first step in the 3D Keltool process, cavity mold inserts and a core get designed in CAD to get followed by manufacture of the core and cavity patterns with stereolithography or some other processes. Once these core and cavity patterns meet the requirements of the surface, silicone rubber cast gets applied on them to form molds in which a mixture of a metal powder and binder get poured and packed.
The instruments used in this process illustrate very qualified surface finish and definition. In general, lead time results in shorter time period than the conventional tooling. The main limitation is the size restriction. The size of a mold insert could be 100 × 150 × 215 mm (4 × 5.9 × 8.5 inches) at most. If the x and/or y dimension gets smaller, the z-direction has the possibility to extend to 145 mm (5.75 inches). To manufacture larger items, some tool makers have two or more cheek-to-cheek inserts in a die base [6].
Metal spray molds had been used effectively in low-pressure procedures including RIM, vacuum forming, and rotational molding. Currently, the improvements in spray metals and spraying methods give rise to its use in injection molding.
The order of steps is like the one applied to manufacture epoxy molds, with the exception that the pattern is sprayed first with metal and then supported by epoxy resin filled with metal. The process of spraying with, for example, an electrical compressed air gun gets applied until the required shell thickness is met (0.5 mm + − mm is reported). In this technique, the material consisting of pattern must have increased strength and durability to withstand the thermal impact inherent: in this regard, the use of ABS FDM masters, polycarbonate SLS masters, and machinable wax gave positive results some of the indirect methods which uses AM, and their advantages and disadvantages are shown in Table 2. In addition to them, a reflective coating could be protective. Also, SLA models were tried process of the spray metal tooling depicted in Figure 2 [6].
Methods of rapid tooling.
Advantages and disadvantages of indirect methods, which use AM.
Spray metal tooling [
All the past AM techniques mentioned include indirect production of a master model producing the tool. The time required to manufacture and complete its pattern is one of the major issues with the manufacturing tool. Moreover, such replication methods can still cause increase in inaccuracies. As a result, although the most of direct tooling techniques have constraints, corporations ask directly produced tooling.
Applying additive “layer manufacturing” methods, further properties may get included in the item, which cannot be acquired with conventional tooling techniques. Conformal heating (or cooling) channels provide the system with the ability to heat or cool the exact points needed, and it is the most critical property of it. It is shown that conformal channels could result with the reduction in cycle times of injection molding by up to 40% [6].
Rather than making a master stereolithography pattern around which a material is cast, it also is possible to build the cavity directly on the stereolithography machine. This method has been described as Direct AIM by 3D Systems (Valencia, CA). (AIM stands for ACES Injection Molding. ACES stands for “accurate clear epoxy solid,” which is a stereolithography construction style.) Even though they are not as strong or difficult as standard tools, various thermoplastics can get injected into those cavities so that elements to get used could get manufactured. Even though only less abrasive and lower melting polymers can get molded, studies are going on in order to increase its applicability [6].
Just as a cavity can be produced directly by stereolithography, the laser sintering method can also be used to construct tool cavities directly. Digital core and cavity geometry models are developed and sent to a Sinterstation manufacturing device in RapidSteel powder with DTM’s RapidSteel (also known as RapidTool, earlier similar methods are known as Indirect Metal Selective Laser Sintering). This material comprises of mild stainless-steel particles that are covered with a thin layer of a material for a polymer binder. The Sinterstation generates green components that fire in a furnace afterwards. The furnace removes the polymer binder and by capillary action infiltrates bronze into the inserts of the mold. This method generates a completely thick tool consisting of approximately 60% steel and 40% bronze. Then the inserts are completed, drilled for ejector pins, and fitted to the base of the mold.
The technique generates a durable mold that can be used as well as die-casting apps for injection mold tooling. Hundreds of aluminum, zinc, and magnesium components were casted using RapidSteel molds. The technique enables complicated geometries, and molds from RapidSteel can resist injection molding circumstances. RapidSteel, however, needs finishing and polishing that can take time scheme of the SLS process can be seen in Figure 3 [6].
DTM SLS Sinterstation 2500 plus [
The DTM (Austin, Texas) copper polyamide tooling method is consisted of selective laser sintering of a matrix of copper and polyamide powder to manufacture a tool. All sintering process happens among the polyamide powder particles. This technique provides improvements in toughness of items unlike some of the other smooth tooling techniques and heat transfer. The copper is not only appropriate for these properties but also can offer some advantages to users like operating a device with pressure and temperature settings which are closer to the environment of the process. The main inconvenience of it is the material’s low resistance [7].
Arcam provides technology to manufacture completely solid metal elements with electron beam melting (EBM). Parts layer by layer are made by the EBM technology using strong electron beam (4 kW power), which melts metal powder. The use of EBM method performed in a vacuum provides users with stress relaxed components with better mechanical, chemical, and material properties the casting and forming.
The method depends on the use of high-level energy thanks to its ability to provide high fusion ability and high productivity. The EBM method is mainly developed in order to process refractory as well as resistant materials (tantalum, niobium, molybdenum, tungsten, vanadium, hafnium, zirconium, titanium) and alloys thereof. It is defined primarily by not only high-speed manufacturing but also complicated geometries of elements with comparable mechanical characteristics to heat-treated products [7].
Direct metal laser sintering (DMLS) from EOS consists of metal powders processed directly in a laser sintering machine. The machine manufactures not only tool inserts but also metal parts. Two materials are available for DMSL method and this method depicted in Figure 4:
Bronze-based materials are preferable for injection molding of up to 1000 elements in various products.
Steel-based material which is advantageous for injection molded components of up to 100,000 plastics [7].
DMLS 3D printing process [
Laminated tooling is another applicable option to construct cavities on an AM used prototyping machine. By using a CAD model, sheet layers of metal are sliced, which uses comparable principles to the laminated object manufacturing (LOM) method to multiply slices. Either water-jet or laser cutting techniques are usually applied to obtain the profiles. Manufacturing the molding tool requires CAD model to take the form of the necessary cavity. A mass of laminates can be accomplished to replicate by cutting all the cavity slices into sheet metal. To eliminate complicated post-process cutter path planning, a pseudo-solid cavity in hardened tool steel is manufactured by using either clamping or diffusion bonding related picture can be seen in Figure 5 [6].
Laminated tooling process [
The Optomec (Albuquerque, New Mexico) laser-engineered net shaping (LENS) system—initially created at the Sandia National Laboratories—is used to build elements into a laser, primarily laser cladding using a metal powder feed. Through a highly intense laser beam into a molten metal pool, a metal powder is injected in this method. The manufacturing method takes place for oxygen-free operation in a low-pressure argon chamber. A movement scheme drives a platform through x and y planes (two-dimensional) as the laser beam traces the cross section of the fabricated portion which can be seen in Figure 6 [7].
Laser-engineered net shaping (LENS) process [
Albrecht Röders GmbH & Co. KG (Soltau, Germany) has marketed a method called controlled metal buildup (CMB). At the Fraunhofer Institute for Production Technology (IPT) (Aachen, Germany), the fundamental technology was initially created. Three systems were purchased by the business last year.
Components having 100% density are resulted by using this method covering lased cladding and friction. The material is deposited by CMB from a steel wire, and a 1–2 kW HDL laser welds the steel to the workpiece surface. Before every fresh layer is deposited, a cutter with a high speed is used to flat each layer [6].
The ProMetal AM used tool production system of Extrude Hone—named RTS-300—is 3DP method for the manufacture of metal components and tooling. Steel parts up to size of 12 ‘12 ‘10 inches (300 ‘300 ‘250 mm) can be achieved by the machine. ProMetal applications covers vacuum forming, lost foam patterns, injection molding, blow molding, and powder metal part manufacturing [6].
Thin SL shells in shell tooling are applied to manufacture inserts reinforced by materials with high thermal conductivity like aluminum-filled epoxy. Therefore, higher mold strengths are attainable in contrast to those achieved by the direct AIM tooling technique, which builds a strong resin mold. Due to aluminum’s increased conductivity, which offers faster cooling of mold, the cycle time gets shorter. To improve wear resistance, metal plate can be used to cover the outer surface brief advantages/disadvantages chart of direct methods is depicted in Table 3 [12].
Advantages and disadvantages of direct methods which use AM.
In all industries, customized and tailored design is gaining importance, and therefore small series production has increased in the last decade. The increasing number of variant types and also the decreasing number of the same parts affect the manufacturing processes deeply. For instance, metal forming is known to be economical for large series production. One of the main factors affecting the cost of the metal forming process is tool costs. Conventional methods and materials to produce forming tools result in certain disadvantages: Not only the production process takes too much time, but also the whole process is expensive.
Therefore, rapid tooling methodologies are gaining importance also for metal forming technologies in recent years. Rapid tooling methods offer indispensable advantages in time, though the cost of the tool must be optimized according to the number of parts to be produced, material couple to be chosen, and the production methodology.
To optimize the part quality, the method, and the cost prediction, a methodology to predict the most appropriate rapid tooling method as well as the prediction of the tool life becomes indispensable.
As the abrasive wear on the metal forming tools increases, it is getting more and more important to predict the tool wear and the life of the tool, when the tool is in design stage. By this way the most appropriate tool materials, design, and maintenance periods can be planned.
First a methodology to ensure that the chosen rapid tooling technique and material are appropriate to produce the part must be introduced. This includes the dimensional accuracy, mechanical properties, the surface quality of the rapid tooling process, the related production process parameters like deformation of the tool, temperature distribution, and a determination of tribologically matching material couple and surface properties important factors can also be seen in Figure 7.
The main factors affecting the choice of the rapid tooling material and production method.
Then the number of parts, which can be produced with this rapidly produced tool, must be predicted. In order to predict the operation time of a tool, the following approach is offered.
A metal forming process is economically advantageous, if and only if the tool costs can be controlled and predicted. Forecasts of the number of parts to be produced with the tools are of highest advantage. Therefore, in the PhD thesis, a method to predict tool wear is established and validated and verified an approach is depicted in Figure 8 [13].
Approach to predict the wear on forming tools.
This approach is tested with a simple cup deep-drawing geometry. The die is made of rapid tooling, whereas the punch and blankholder are produced by conventional methods out of tool steel as given in Figure 9. For that reason, the punch and blankholder are modeled as rigid body, whereas the die is modeled with 3D deformable elements.
(a) Schematic presentation of deep drawing of a cup geometry. (b) a quarter model of a simplified circular deep drawing geometry [
In order to enable testing, a follow-on tool is designed, and an optical and tactile measurement methodology is determined. The die made out of rapid tooling is measured at determined intervals, and the wear propagation over time is measured. Four different locations are measured, and the experiments are conducted up to five times. The details of the repeatability and reliability of the data and measurement methodology can be found in [13].
The contact pressure distribution is obtained by finite element methodology as depicted in Figure 10. As the die material is made out of rapid tooling, these materials are generally very susceptible to abrasive wear.
Comparison of wear behavior of different rapidly produced tools (PA220 (PA-SLS), ZAMAK (SLA + casting), LaserFormA6 (SLS RapidSteel) vs. tool steel (conventional method) [
The key technology for predicting the development of wear in metal forming tools is numerical simulation. In forming applications, a wear is commonly described using models based on contact mechanics, the most important one being the Archard wear equation. Here the parameters affecting the wear are contact pressure, sliding distance, hardness, and a tribological constant.
With the offered methodology, the wear depth at each location at each punch stroke can be predicted. Figure 11 depicts as an example a predicted vs. measured die radius wear rate after 10,000 punch strokes.
Contact pressure obtained by finite element simulation [
The Figure 12 shows the wear rate of different dies produced by AM technologies, measured at different time intervals. As expected all rapidly produced tools have higher wear, i.e., shorter operation times. LaserFormA6 a kind of stainless steel powder produced by SLS RapidSteel has the best wear resistance as expected, among others. Polyamide die has remarkably high wear rate which indicates that these are not appropriate for any series more than 100 parts. ZAMAK (zinc, aluminum, copper alloy) produced by casting into a SLA mold turns out to have a moderate wear resistance. All these trends obtained in these experiments are in accordance with the Archard theory, where the wear of the tool is indirectly proportional to the hardness of the die materials. Still, when investigated in detail their wear behavior, their elastic deformation, and tribological behavior affect the wear distribution over time, i.e., number of parts, sliding distance, or wear work.
Measured wear depth in the profile (gray) compared to the simulation results of the same location (black) [
This implies that according to the geometry and the number of the parts needed, this method can also be considered an alternative for sheet metal forming tool.
Customized and tailored design is gaining significance in all areas in the recent decades. The growing amount of variants and the declining amount of the same components also have a profound impact on the production procedures. Additive manufacturing is gaining importance due to many advantages, and in tool design it is used mostly due to its lead time advantage. Even if AM in tool production offers indispensable advantages in time, the cost of the tool must be optimized according to the number of parts to be produced, the couple of materials to be selected, and the method of production.
A methodology for predicting the most suitable AM technique for tooling, as well as predicting the life of the tool, becomes indispensable in order to optimize the part quality, process, and price prediction. First, it must be guaranteed that the selected fast tooling method and material are suitable for producing the tool. This involves dimensional precision, mechanical characteristics, surface quality of the selected AM method, associated process parameters such as tool deformation and temperature distribution, and determination of corresponding material pair and surface characteristics tribologically.
In this chapter a metal forming tool in a simplified round die geometry is chosen as an example to predict the wear of a AM-produced tool, and the results show that the AM-produced tool has a shorter operation life, showing a wider range of lifetime depending on the AM technique and the tool material which are used.
From these results it can be concluded that in the chosen AM method, the material must be optimized according to the geometry of the part to be produced, number of parts to be produced, process parameters, tribological requirements, and the time and cost constraints.
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\\n\\nInterested? Contact Ana Pantar (book.idea@intechopen.com) for more information.
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\n\nOur reputation – Everything we publish goes through a two-stage peer review process. We’re proud to count Nobel laureates among our esteemed authors. We meet European Commission standards for funding, and the research we’ve published has been funded by the Bill and Melinda Gates Foundation and the Wellcome Trust, among others. IntechOpen is a member of all relevant trade associations (including the STM Association and the Association of Learned and Professional Society Publishers) and has a selection of books indexed in Web of Science's Book Citation Index.
\n\nOur expertise – We’ve published more than 4,500 books by more than 118,000 authors and editors.
\n\nOur reach – Our books have more than 130 million downloads and more than 146,150 Web of Science citations. We increase citations via indexing in all the major databases, including the Book Citation Index at Web of Science and Google Scholar.
\n\nOur services – The support we offer our authors and editors is second to none. Each book in our program receives the following:
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\n\nInterested? Contact Ana Pantar (book.idea@intechopen.com) for more information.
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