Main parameters of the DCMS and HiPIMS discharges described in this work and characterized by resonant optical absorption spectroscopy.
\\n\\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\\n\\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\\n"}]',published:!0,mainMedia:null},components:[{type:"htmlEditorComponent",content:'IntechOpen is proud to announce that 179 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\nThroughout the years, the list has named a total of 252 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\nReleased this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\nWe wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
\n'}],latestNews:[{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"},{slug:"oiv-awards-recognizes-intechopen-s-editors-20201127",title:"OIV Awards Recognizes IntechOpen's Editors"},{slug:"intechopen-joins-crossref-s-initiative-for-open-abstracts-i4oa-to-boost-the-discovery-of-research-20201005",title:"IntechOpen joins Crossref's Initiative for Open Abstracts (I4OA) to Boost the Discovery of Research"},{slug:"intechopen-hits-milestone-5-000-open-access-books-published-20200908",title:"IntechOpen hits milestone: 5,000 Open Access books published!"},{slug:"intechopen-books-hosted-on-the-mathworks-book-program-20200819",title:"IntechOpen Books Hosted on the MathWorks Book Program"}]},book:{item:{type:"book",id:"3528",leadTitle:null,fullTitle:"Cardiac Surgery - A Commitment to Science, Technology and Creativity",title:"Cardiac Surgery",subtitle:"A Commitment to Science, Technology and Creativity",reviewType:"peer-reviewed",abstract:"In this book it is shown how this specialty has evolved over the past 20 years, with significant advances in diagnosis and palliative and definitive techniques for correction of cardiovascular diseases. 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Chun",coverURL:"https://cdn.intechopen.com/books/images_new/3476.jpg",editedByType:"Edited by",editors:[{id:"164636",title:"Prof.",name:"Jang Ho",surname:"Chun",slug:"jang-ho-chun",fullName:"Jang Ho Chun"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"49672",title:"Diagnostics of Magnetron Sputtering Discharges by Resonant Absorption Spectroscopy",doi:"10.5772/61840",slug:"diagnostics-of-magnetron-sputtering-discharges-by-resonant-absorption-spectroscopy",body:'Among the families of plasma-related methods involved in thin films growth, those belonging to physical vapor deposition (PVD) are among the most commonly utilized. The PVD-related techniques cover wide range of the deposition methods, including evaporation, vacuum arc deposition, laser ablation, and sputtering. These methods are different from another class referred to as chemical vapor deposition (CVD) in the sense that the source of material is solid or liquid as opposed to a gaseous one in the case of CVD [1]. Thermal evaporation has been the most used PVD process for many years because of the easy handling and relatively high deposition rate comparing to the first known sputtering process, namely, the diode sputtering [2]. The latter process has been known since its first description in 1852 by W. R. Grove, who had performed sputtering using a massive inductive coil [3]. In diode sputtering, ions of the sputter gas, commonly argon, hit a negatively biased cathode (also known as target) with energy up to several hundred electron volts (eV). This energy is high enough to induce ejection of the superficial atoms, which is followed by their condensation on the chamber surfaces, including a potential substrate [4]. In diode sputtering, however, due to the relatively high process pressure needed to ensure the discharge stability (nearly 0.1 Torr), the mean free path of the ejected atoms is in the mm range, which is much lower than the typical substrate-target distance (cm range) resulting in relatively poor quality of the deposited coating.
The limitations of diode sputtering have been overcome in 196× with the works of E. Kay and W. Gill [5,6], who have proposed to utilize magnetic field to create efficient electron trapping above the cathode (target) in order to accelerate the ionization and sputtering itself. The electron trapping region is created due to the fact that the electrons propagate mainly along the magnetic field lines as a result of well-known gyration effect (with gyration radius being in the µm range). The implementation of magnetic field for sputtering, naturally producing the name “magnetron,” has been shortly followed by the introduction of planar magnetron sources in 1974 [2,7], for which the presence of permanent magnets beneath the cathode was a distinctive feature, as schematically illustrated in Figure 1. As a result of the electron trapping, these innovations led to essential increase in the ionization degree of the sputter (bulk) gas in the cathode vicinity. As a result, the pressure necessary to maintain the discharge current in this case could be reduced by about one order of magnitude, i.e., down to the mTorr range [5]. Another critical point related to efficiency of magnetron sputtering is the topology of magnetic field. Indeed, the arrangement of magnets beneath the cathode affects significantly the degree of electron confinement above the target. In the so-called balanced magnetron sources, the dense plasma region above the target is roughly comparable to its radius (assuming a planar circular target) [8]. If the substrate is located outside this region, the bombardment of growing film by the plasma ions is essentially reduced (the resulting ion current is <1 mA/cm2), limiting the benefit of the sputtering process. This effect is different in the so-called unbalanced sources, where the topology of the magnetic field near cathode is different, letting some magnetic field lines reach the substrate. In this case, plasma is not confined completely, and the ion current densities of about 2–10 mA/cm2 can be reached, which is typically one order of magnitude higher than in the case of balanced magnetrons [9].
Side view of a typical magnetron source, including planar circular magnetron target, permanent magnets, and cooling system. The magnetic field lines are shown schematically.
In addition to magnetic field configuration, the voltage waveform and its repetition rate also play significant role in magnetron sputtering. The development of the plasma sources utilizing this effect has been mainly driven by the efficient deposition of the insulating compounds using reactive sputtering (see below). Thus, in addition to the well-known direct current magnetron sputtering (DCMS) devices, the radio frequency (RF) magnetron sources mainly working at 13.56 MHz have been introduced. Following the same trend, in the early 1990s, the idea of using pulsed-DCMS (also known as P-DCMS, or pulsed-DC) has been proposed (see, e.g., [10,11]). In most cases, the pulsed-DC power supplies operate successively alternating the negative (sputtering phase) and positive (charge dissipation phase) voltage cycles. The power supply in this case might be unipolar or bipolar, depending on polarity of the utilized pulses. Nowadays, most of magnetron sputtering processes for the synthesis of insulating compound coatings use pulsed magnetron sputtering approach [9].
Further development of the pulsed magnetron sputtering technology has triggered the new family of magnetron sputtering processes, so-called ionized physical vapor deposition (IPVD) techniques [12]. In a typical IPVD discharge, significant fraction of the sputtered atoms is ionized, reaching up to 100% in certain cases. The main idea behind the IPVD techniques is to generate denser plasmas than those appear in conventional magnetron sputtering in order to ionize the sputtered atoms more efficiently (up to the level of number densities ~1013–1014 cm–3 vs. 108–1011 cm–3 in the DCMS case). Among the different approaches targeted to increase the ionization degree, such as using an inductive coil [13], or hollow cathodes [14], the high-power impulse magnetron sputtering technique, or HiPIMS (also known as high-power pulsed magnetron sputtering—HPPMS), is the most notorious IPVD example. HiPIMS discharge uses the pulse duration ranged from few µs to few hundreds µs, while the pulse repetition frequency typically varies from ~10 Hz to ~10 kHz. Under these conditions, the peak current density may reach values of up to several A/cm–2 compared to a few mA/cm–2 in DCMS, but only during a short time, typically 1–2% of the repetition period [15]. As a result, a dense plasma is generated during the plasma on time enabling not only efficient target sputtering but also high ionization degree of metallic vapor [16], at the same time keeping the average applied power comparable to that of DCMS [15–17]. The schematic comparison of the DCMS, P-DCMS, and HiPIMS techniques in terms of the applied power is shown in Figure 2. Note that the level of time-averaged power applied to the sputtered cathode in each case is roughly the same, which is first of all due to the fact that the permanent magnets beneath the target should not be overheated and reach the Curie temperature (which is as low as about 580 K for widely used neodymium-based magnets). The actual applied power level is typically equal to several hundred Watt and often defined by the magnetron source cooling system (i.e., water temperature) used beneath the target. The interest to the pulsed magnetron discharges and, namely, the HiPIMS discharges from both scientific and application points of view has been continuously increasing since the introduction these techniques [18,19]. The main advantages of the HiPIMS technique, along with the achievements in characterization of these discharges, are described in the numerous works [15,17,20–23].
Comparison between the DCMS (a), P-DCMS (b), and HiPIMS (c) magnetron sputtering techniques in terms of the temporal distribution of the applied power. Typical range of the relevant discharge parameters and the values along both horizontal and vertical axes are given for reference only. The quantities f, tON, DR, and Ppeak stand for repetition frequency, plasma on time, duty ratio, and peak power, respectively.
Why is the knowledge of the absolute density in plasma and particularly in magnetron sputtering discharges important? There are few main reasons making this parameter critical. First, particle fluxes in the discharge can be estimated knowing the density and velocity of each sort of the sputtered species, which is critical for any film growth process. Second, the discharge physics and chemistry can be significantly clarified having the absolute concentration of the relevant species in the discharge estimated properly. Third, the absolute concentration of the discharge species or their fluxes can be used as input information for further kinetic/chemical modeling of the discharge processes. Among the known plasma characterization approaches, resonant optical absorption spectroscopy (ROAS), also known as atomic absorption spectroscopy (AAS) [24,25], represents one of the straightforward ways for the determination of the absolute density of atomic and/or molecular species in gaseous discharges. Utilizing this technique, the density of the absorbers can be determined using an external (reference) light source by measuring the attenuation in its intensity after passing a volume with the absorbing species (see, e.g., Mitchell and Zemansky [24], p. 92). Along with the laser-based plasma diagnostic techniques, such as laser-induced fluorescence (LIF), ROAS technique has been playing a significant role in studying the plasma discharges during the last decades, involving both coherent (such as diode lasers) [26–28], and noncoherent (e.g., hollow cathode lamps—HCL) [29–31] radiation sources. The range of applications of this technique has been continuously increasing due particularly to the improvements of the tunable diode laser systems, namely, their stability, power level, tuning range, etc. [27,32].
In the domain of magnetron sputtering discharges, the determination of number density of the discharge particles by ROAS has been undertaken in the variety of systems, including time-resolved [33] and space-resolved [34] characterization. In particular, among the recent achievements, the works of various research groups devoted to absolute density of sputtered atoms in the DCMS discharges [31,34,35], including those amplified by an RF coil [30], as well as the works of devoted to flux measurements in DCMS [36], should be mentioned. What is related to the utilization of ROAS in the HiPIMS domain, the works dealing with the determination of time-resolved absorption line profile [33], which have been realized using tunable diode laser absorption spectroscopy (TD-LAS), should be emphasized. In addition, a detailed time evolution of the Ar metastable 1s5 states (Armet) has been investigated in a long-pulsed (200 μs) HiPIMS discharge by Vitelaru et al. [26], where the Armet density growth, followed by its rarefication after about 50 μs, and a gradual refill afterward have been clearly demonstrated. These results are generally in a good agreement with the recent studies in HiPIMS involving LIF [37] and ROAS [38] techniques, which are partially overviewed here. The last two works ([37,38]) are devoted to the short-pulsed HiPIMS discharges studying the propagation of the ground state and metastable sputtered particles, being mainly targeted to the systematic time-resolved characterization of HIPIMS discharges in terms of absolute density of species, 2-D imaging of the main atomic states corresponding to the studied discharge species (LIF+ROAS), as well as to the study of several optically available energy states of the discharge species and their sublevels.
Unifying the recent achievements in the domain of the absolute density measurements for two “extreme” magnetron sputtering cases, namely, DCMS and HiPIMS, this chapter is mainly focused on the particularities of the mentioned sputtering discharges in terms of the absolute density of species where resonant absorption is used as a main diagnostics technique. The resonant absorption method overviewed in this chapter is considered as a reliable tool for the determination of the absolute density of species in the discharge volume and for understanding the sputtering processes at the atomic level.
The main principles of the resonant absorption are described in details in the work of Mitchell and Zemansky [24]. This method is based on resonant absorption of radiation emitted by a reference source and absorbed (by atoms or molecules) in an optically thin gaseous discharge. At a definite spectral line the absolute density of states corresponding to a lower level of a chosen spectral transition can be determined by measuring so-called line absorption, i.e., an integral under spectral absorption line of interest, if the effective absorption lengths as well as the line width of both plasma and source spectral lines are known. This approach can be applied for the case when the spectral lines in the discharge are Doppler-limited [31], as well as can be generalized for more general cases [39]. The biggest advantage of ROAS technique is its nonintrusiveness. In this regard, this technique is different from the other methods used for density determination, which are based on the introduction of additional gases to the discharge (such as titration [40]), which may potentially change the electron energy distribution and the discharge kinetics. In addition, the fact ROAS uses external source of radiation and does not depend on the discharge emission itself is critical for characterization of the pulsed discharges, such as HiPIMS, especially during the afterglow time when optical emission spectroscopy (OES), cannot be applied.
As mentioned above, ROAS can be implemented in two different ways, namely, using a gaseous discharge emitting the spectral lines of interest, as well as using a monochromatic laser (e.g., a continuous tunable laser diode). Despite the fact that the laser-based diagnostics has several advantages [21,33], the discharge-based ROAS should be implemented. Among the main reasons for this are the following: (i) discharge-based ROAS setup is normally less expensive than the one based on a tunable laser; (ii) discharge-based ROAS depends on the line width ratio between the plasma and the reference source, which can be easily taken into account [24]; (iii) several spectral transitions can be studied in parallel in this case, as far as the emitters in the reference source coincide with the absorbers of interest, which is not possible with a monochromatic laser; and (iv) in case of a large spectral separation (few nm) between the lines of interest, laser-based absorption setup requires separate laser diodes for each transition, which involves additional calibration procedures. Due to the mentioned advantages, for example, the absolute density at the energy sublevels corresponding to a certain electronic state can be probed in a straightforward way, by simply following the changes in the emission intensity of the corresponding peaks from the reference source, as performed in the numerous studies [30,31,34,35,39]. Let us consider the main relations necessary to understand the ROAS method.
This chapter deals with the classical ROAS method described by Mitchell and Zemansky [24]. In the case of temperature-limited emission (absorption) lines in the reference source (and in the studied discharge), the application of the resonant absorption method is rather straightforward, and the details of its implementation in magnetron discharges can be found elsewhere [35,38]. In this section, only the essential relations important for understanding the absolute density determination using ROAS method are given. The number density of the absorbing species in the lower (often ground) state can be determined using the following relation:
where
where
The absorption coefficient
where L is the effective absorption length (~30 cm in our case), and
where
Schematic illustration of the absorption technique and the physical meaning of the quantities IP, IS, and IPS.
After the experimental determination of line absorption
Several important remarks on the line broadening of plasma and reference source spectral lines should be made for proper interpretation of ROAS data. As mentioned above, this chapter deals with discharge-based ROAS when an HCL is primarily used as reference source. Since the gas pressure in HCL normally exceeds few Torr, and the mean free path of the gas particles is in the µm-range, the total particle thermalization can be assumed. The temperature in HCLs under the reviewed conditions, additionally measured by a high-resolution planar Fabry–Perot interferometer [42], is in the range of about 700–1100 K (see Table 1). Despite much lower pressure (~20–30 mTorr) in the magnetron discharges considered here (Table 1), similar considerations are also valid for the bulk gas atoms (Ar) in the studied DCMS and HiPIMS cases, which can be considered quasi-thermalized. The Ar temperature can be often assumed to be in the range of 300–500 K in this case, depending on the discharge type and its conditions [21,30,35,43].
\n\t\t\t\tParameter\n\t\t\t | \n\t\t\t\n\t\t\t\tValue\n\t\t\t | \n\t\t\t\n\t\t\t\tComment\n\t\t\t | \n\t\t
\n\t\t\t\tDCMS system parameters\n\t\t\t | \n\t\t||
Target | \n\t\t\t99.99% Ti | \n\t\t\tWith water cooling | \n\t\t
Target diameter/thickness | \n\t\t\t5 cm/0.5 cm | \n\t\t\t10 cm/1 cm for Figure 9 | \n\t\t
Working gas | \n\t\t\t99.999% Ar | \n\t\t\t\n\t\t |
Working pressure | \n\t\t\t20 mTorr | \n\t\t\t30 mTorr for Figure 9 | \n\t\t
Base pressure | \n\t\t\t~10–6 Torr or less | \n\t\t\t\n\t\t |
Time-averaged power | \n\t\t\t~200 W | \n\t\t\t500 W for Figure 9 | \n\t\t
Monocromator used | \n\t\t\tPrinceton Instrument SpectraPro-500i | \n\t\t\tJobin-Yvon HR-460 for Figure 9 | \n\t\t
Monocromator slit width | \n\t\t\t10 µm | \n\t\t\t\n\t\t |
Spectral resolution | \n\t\t\t0.05 nm | \n\t\t\t\n\t\t |
Optical detector used | \n\t\t\tPrinceton Instrument PI-MAX ICCD | \n\t\t\tHamamatsu R928 photomultiplier tube | \n\t\t
\n\t\t\t\tHiPIMS system parameters\n\t\t\t | \n\t\t||
Target | \n\t\t\t99.99% Ti | \n\t\t\tWith water cooling | \n\t\t
Target diameter/thickness | \n\t\t\t10 cm/1 cm | \n\t\t\t\n\t\t |
Working gas | \n\t\t\t99.999% Ar | \n\t\t\t\n\t\t |
Working pressure | \n\t\t\t20 mTorr | \n\t\t\t\n\t\t |
Base pressure | \n\t\t\t<10–6 Torr | \n\t\t\t\n\t\t |
pulse duration/frequency | \n\t\t\t20 μs/1 kHz | \n\t\t\tUnless stated otherwise | \n\t\t
Supplied energy per pulse(at 20 μs pulse) | \n\t\t\t≈0.26 J | \n\t\t\tCorresponding to ~260 W of time-averaged power | \n\t\t
Monocromator used | \n\t\t\tAndor Shamrock 750 | \n\t\t\t\n\t\t |
Monocromator slit width | \n\t\t\t20–100 µm | \n\t\t\t\n\t\t |
Spectral resolution | \n\t\t\t0.04–0.1 nm typically | \n\t\t\t\n\t\t |
Optical detector used | \n\t\t\tAndor iStar DH740-18F ICCD | \n\t\t\tWith ~103 pulses averaged | \n\t\t
\n\t\t\t\tResonant absorption parameters\n\t\t\t | \n\t\t||
Beam diameter | \n\t\t\t≈1 cm | \n\t\t\t\n\t\t |
Distance above the target, z\n\t\t\t | \n\t\t\t≈5 cm | \n\t\t\t\n\t\t\t\tz = 0..10 cm for Figure 8, z = 8 cm for Figure 9. | \n\t\t
Effective absorption length, L | \n\t\t\t30 cm | \n\t\t\tVariable for Figure 8, L=25 cm for Figure 9. | \n\t\t
Reference source type | \n\t\t\tAr-Ba and Ne-Ti hollow cathode lamps | \n\t\t\t\n\t\t |
Reference source pulse duration | \n\t\t\t40–100 µs | \n\t\t\tContinuous for Figure 8, 150 µs for Figure 9. | \n\t\t
Reference source temperature | \n\t\t\t≈1100 K (in pulsed mode [38]) | \n\t\t\t950 K for Figure 8 [34], 630 K for Figure 9 [54]. | \n\t\t
DCMS plasma temperature | \n\t\t\t580 K (Figure 8), 300 K (Figure 9) | \n\t\t\t\n\t\t |
HiPIMS plasma temperature (Ar) | \n\t\t\t≈500 K | \n\t\t\tBased on OES measurements [43] | \n\t\t
HiPIMS plasma line width (Ti) | \n\t\t\t≈5.5 GHz | \n\t\t\tBased on LIF measurements [44] | \n\t\t
Main parameters of the DCMS and HiPIMS discharges described in this work and characterized by resonant optical absorption spectroscopy.
The broadening of spectral lines corresponding to the sputtered particles may differ from those of the bulk gas (Ar), however. In the DCMS case, despite the fact the sputtered particles are far from thermalization, their velocity distribution function (VDF) can be often approximated by a Gaussian profile. This VDF does not change in time, by definition of DCMS discharge [37], and often can be associated with the particle temperature in the range of 300–700 K for the conditions described here (see Table 1). Due to the directional motion of the sputtered particles in magnetron plasma, the spectral line in the direction of measurements (i.e., along the ROAS line-of-sight) might be significantly broadened, as compared to the one of the reference source. This situation is schematically illustrated in Figure 4. In this case, the resonant absorption will happen only for a part of the total line width, and the ratio between the mentioned broadenings has to be introduced (
Illustration of the spectral line broadening (FWHM) of the reference source (emission) and plasma (absorption) lines along with their broadening notations.
The situation is yet different for HiPIMS discharges, which are far from thermalization during the plasma on time, especially in the target vicinity [37,43]. The distribution of the velocity component parallel to the target (
The typical experimental arrangement for characterization of magnetron sputtering discharge by resonant spectroscopy is shown in Figure 5. The main parameters related to the discharges overviewed in this work are summarized in Table 1. Both in DCMS and HiPIMS cases, a cylindrical vacuum chamber with either horizontally or vertically placed balanced magnetron sputtering source holding a planar circular magnetron target has been used. The Ti magnetron targets, 5 or 10 cm in diameter, attached to a magnet-supporting water-cooled copper base, have been utilized. The commercial power supplies have been used to sustain the DCMS discharges, as described elsewhere [30,34]. In the HiPIMS case, the discharge current and voltage along with the pulse parameters have been controlled by the Lab.-made power supply, described by Ganciu et al. [46]. The HiPIMS discharge typically had 20 µs of the pulse duration and 1 kHz of the repetition frequency (thus having 980 µs of the plasma off time). The typical current–voltage waveforms can be found elsewhere [43,44,47]. The base pressure in the magnetron reactor has been kept <10–6 Torr, whereas the bulk gas (99.999% Ar) pressure was normally fixed at 20 mTorr during all the ROAS measurements, unless stated otherwise. In order to avoid deposition on the quartz window surface, the special collimators (Ni tubes) with high length-to-radius ratio have been installed in front of each viewport inside the reactor.
Top (a) and side (b) view of the experimental setup utilized for absolute density measurements in a magnetron sputtering discharge by ROAS. Role of the reference source is played by a hollow cathode lamp. Reproduced with permission from Britun et al. [38]. Copyright 2015 AIP Publishing.
The Perkin Elmer hollow cathode lamps (one with Ti cathode filled by Ne, and another one with Ba cathode filled by Ar) have been used as the reference sources. The HCLs have been running either in the continuous or pulsed regime (mainly in the HiPIMS case) in order to increase the emission intensity and make it comparable with the HiPIMS plasma emission, aiming at reducing the measurements error during the plasma on time [43,48]. Apart from this, the pulse regime of HCL source favors the ionization of the cathode material inside the lamp, which is critical for analysis of the Ti+ states [30]. During the measurements, the HCLs have a pulse duration typically ranging from 40 to 100 µs. About 103 pulses from the reference source have been averaged by the detector during the measurements of the absorption coefficient. The HCL pulse sequence was triggered by the HiPIMS power supply using the external transistor-transistor logic (TTL) trigger and was time shifted relatively to the HiPIMS plasma pulse using an additional analog TGP-110 pulse generator.
In some cases, when the density of absorbers in the studied discharge is too low, an improved detection scheme, including a triple optical fiber and allowing simultaneous acquisition of the
Scheme of the experimental setup for absorption measurements with increased reliability utilizing simultaneous acquisition of the plasma and source optical signals (IP, IS, and IPS) necessary for calculation of the line absorption AL.
A monochromator equipped with an intensified charge-coupled device (ICCD) camera and connected to the discharge reactor by an optical fiber has been used for spectral acquisition in most cases. The spectral resolution of the monochromator was typically ≈0.05–0.1 nm. The typical emission spectra acquired in Ar-Ti HiPIMS discharge at the end of plasma on time are presented in Figure 7. From the general emission spectrum (Figure 7(a)), the relevant spectral regions containing Ti and Ti+ emission lines are visible (Figure 7(b–d)). The representative emission lines used in this work for resonant absorption are marked by arrows (see also Table 2). In most cases, the studied emission lines are well-resolved from the neighboring peaks. Due to this fast, rather low spectral resolution is normally sufficient for ROAS measurements. The total procedure for the number density determination consisted of the emission peaks intensities measurements (
General emission spectrum (a) obtained in Ar-Ti HiPIMS discharge showing the spectral regions of interest used for the determination of the absolute density of different atomic species. The spectral regions corresponding to Ti ground state atoms (b), Ti metastables (c), as well as Ti ions (d) are shown separately. The HiPIMS and HCL spectra (b–d) are normalized arbitrary. Reproduced with permission from Britun et al. [38]. Copyright 2015 AIP Publishing.
\n\t\t\t\tSpectral\n\t\t\t\t \n\t\t\t\tparameter\n\t\t\t\t \n\t\t\t\tStudied\n\t\t\t\t \n\t\t\t\tatom\n\t\t\t | \n\t\t\tNature of the probed state | \n\t\t\tEnergy of the probed state (eV) | \n\t\t\tEmission wavelength λ (nm) | \n\t\t\tSpectral transition (lower–upper level, j–i) | \n\t\t\tStatistical weight of the lower level, gj\n\t\t\t\t\n\t\t\t | \n\t\t\tOscillator strength, fji\n\t\t\t\t\n\t\t\t\ta\n\t\t\t | \n\t\t
\n\t\t\t\tTi\n\t\t\t | \n\t\t\tGround | \n\t\t\t0.000 0.021 0.048 | \n\t\t\t363.55 364.27 365.35 | \n\t\t\t3d\n\t\t\t\t24s\n\t\t\t\t2 a3F2–3d\n\t\t\t\t2(3F)4s4p(1P°) y3G°3\n\t\t\t\t 3d\n\t\t\t\t24s\n\t\t\t\t2 a3F3–3d\n\t\t\t\t2(3F)4s4p(1P°) y3G°4\n\t\t\t\t 3d\n\t\t\t\t24s\n\t\t\t\t2 a3F4–3d\n\t\t\t\t2(3F)4s4p(1P°) y3G°5\n\t\t\t | \n\t\t\t5 7 9 | \n\t\t\t0.20 0.16 0.14 | \n\t\t
\n\t\t\t\tTimet\n\t\t\t\t\n\t\t\t | \n\t\t\tMetastable | \n\t\t\t0.813 0.818 0.826 0.836 0.848 | \n\t\t\t501.43 500.72 499.95 499.11 498.17 | \n\t\t\t3d\n\t\t\t\t3(4F)4s a5F1–3d\n\t\t\t\t3(4F)4p y5G°2\n\t\t\t\t 3d\n\t\t\t\t3(4F)4s a5F2–3d\n\t\t\t\t3(4F)4p y5G°3\n\t\t\t\t 3d\n\t\t\t\t3(4F)4s a5F3–3d\n\t\t\t\t3(4F)4p y5G°4\n\t\t\t\t 3d\n\t\t\t\t3(4F)4s a5F4–3d\n\t\t\t\t3(4F)4p y5G°5\n\t\t\t\t 3d\n\t\t\t\t3(4F)4s a5F5–3d\n\t\t\t\t3(4F)4p y5G°6\n\t\t\t | \n\t\t\t3 5 7 9 11 | \n\t\t\t0.38 0.26 0.22 0.17 0.22 | \n\t\t
\n\t\t\t\tTi+\n\t\t\t\t\n\t\t\t | \n\t\t\tGround | \n\t\t\t0.000 0.012 0.028 0.049 | \n\t\t\t338.38 337.28 336.12 334.94 | \n\t\t\t3d\n\t\t\t\t2(3F)4s a4F3/2–3d\n\t\t\t\t2(3F)4p z4G°5/2\n\t\t\t\t 3d\n\t\t\t\t2(3F)4s a4F5/2–3d\n\t\t\t\t2(3F)4p z4G°7/2 3d\n\t\t\t\t2(3F)4s a4F7/2–3d\n\t\t\t\t2(3F)4p z4G°9/2 3d\n\t\t\t\t2(3F)4s a4F9/2–3d\n\t\t\t\t2(3F)4p z4G°11/2 | \n\t\t\t4 6 8 10 | \n\t\t\t0.28 0.25 0.26 0.27 | \n\t\t
\n\t\t\t\tTi+met\n\t\t\t\t\n\t\t\t | \n\t\t\tMetastable | \n\t\t\t0.574 0.607 | \n\t\t\t376.13 375.93 | \n\t\t\t3d\n\t\t\t\t2(3F)4s a2F5/2–3d\n\t\t\t\t2(3F)4p z2F°5/2\n\t\t\t\t 3d\n\t\t\t\t2(3F)4s a2F7/2–3d\n\t\t\t\t2(3F)4p z2F°7/2\n\t\t\t | \n\t\t\t6 8 | \n\t\t\t0.22 0.21 | \n\t\t
\n\t\t\t\tArmet\n\t\t\t\t\n\t\t\t | \n\t\t\tMetastable | \n\t\t\t11.548 11.723 | \n\t\t\t811.53 794.82 | \n\t\t\t3s\n\t\t\t\t23p\n\t\t\t\t54s(1s\n\t\t\t\t5)–3p\n\t\t\t\t54p(2p\n\t\t\t\t9)b 3s23p54s(1s\n\t\t\t\t3)–3p54p(2p\n\t\t\t\t4)b | \n\t\t\t5 1 | \n\t\t\t0.51 0.56 | \n\t\t
Spectral parameters of the optical transitions for Ti, Timet, Ti+, and Armet atomic states used in this work for ROAS diagnostics. Spectroscopic data are taken from the online NIST spectral database [74] unless stated otherwise. Reproduced with permission from Britun et al. [38]. Copyright 2015 AIP Publishing.
Even though the main plasma parameters of the DCMS discharges do not alter in time, the plasma density as well as the density of the sputtered species may vary significantly as a function of the spatial position in the discharge. The first parameter in this case defines mainly the excitation level of the bulk and sputtered species as well as their ionization degree, whereas the (ground state) density of the sputtered species is mainly affected by the applied power, sputtering yield, target size, diffusion processes in the discharge volume, as well as by the other processes. The effects of ground state density depletion also may take place, as recently shown for DCMS discharges by LIF [49], but these effects are rather minor, especially comparing with HiPIMS case [37,38], since the ionization degree in the DCMS discharges generally remains at the level of few percent [15].
The optical diagnostics applied to a DCMS discharge clearly visualizes the plasma region corresponding to the confined electrons, which is represented by the bright area near the target surface observable by a naked eye, as shown in Figure 8. This region clearly corresponds to a spatial segment formed by the magnetic lines in the target vicinity, as shown in Figure 8(b), where the simulated magnetron magnetic field lines are drawn. The target diameter in this case is equal to 5 cm, but nevertheless the obtained data can be compared to the typical absolute density measured with larger targets (see Table 1), as soon as the target materials are the same and the current density are known, due to the scalability of the magnetron discharges [15]. In addition to this, as shown by Britun et al. [34], the emission lines in the plasma region decay exponentially along z direction, where an exponential dependence with significantly lower decrement is found at higher z, which corresponds to the diffusion region.
A photograph of the actual DCMS discharge operating at 4 mTorr of Ar pressure (a) along with the simulated magnetic field lines (b), and the distribution of the absolute density of Ti ground state atoms and Ti metastables measured by ROAS as a function of z at 30 mTorr of Ar pressure (c). Reproduced with permission from Britun et al. [34]. Copyright 2006 IOP Publishing.
In addition, the ground state density of the sputtered Ti as well as Ti metastables, measured by ROAS, follows the trend found for the emission lines by Britun et al. [34], as shown in Figure 8(c). As one can observe, the number density of Ti neutrals reaches nearly 1012 cm–3 near the target at the examined conditions (see Table 1), dropping about 5 times already at z = 2 cm, which is mainly due to the diffusion and the angular particularities of sputtering [50]. The Ti metastable atoms (the energy level is about 0.8 eV, see Table 2) reveal the same tendency having the total density 2–5 times smaller. The presented absolute values of Ti density are in the good agreement with related measurements performed in DCMS under the similar conditions [31]. We have to note that the found particularities of spatial distribution for the sputtered particles in DCMS should resemble those for HiPIMS discharges, as far as the magnetic field topology and the average power are similar. In HiPIMS discharge, however, the additional physical effects, such as the time-dependent broadening of the emission [22] and absorption spectral lines [44], cross-field ion transport [15,51], ionization-induced density depletion near the target [37], time-dependent current-induced changes of the magnetic field [52], etc., may not allow a direct comparison between the DCMS and the HiPIMS discharges in terms of the absolute density of particles. These differences should be even more essential with increasing of the plasma density, i.e., the magnetron current density, as briefly mentioned below.
Another interesting possibility that ROAS provides is visualization and control of the physical processes during the so-called reactive sputtering. This process is mainly known for synthesis of oxide, nitride, and oxynitride thin films [21,53]. Reactive sputtering normally involves standard magnetron sputtering sources, where a certain percentage of, e.g., molecular oxygen or nitrogen, is added to the bulk gas (typically Ar) in order to finally synthesize oxide or nitride compounds. Physically, during the reactive sputtering, oxidation (nitriding, etc.) of the cathode superficial layer takes place, which is often referred to as “poisoned” regime. This process is characterized by a significant drop of the density of metallic species in the discharge volume [54]. Apart from this, a hysteresis effect (in terms of discharge voltage or metal atom density) depending on the direction of change of the reactive gas content is often considered to be among the main characteristics of reactive sputtering [15,55–57].
The example of measurements of the absolute number density of Ti atoms sputtered in a DCMS discharge at z = 8 cm away from the target using resonant absorption is given in Figure 9. Molecular nitrogen has been added to the bulk gas in this case in order to synthesize nitride films, as described in details in [54]. As we can see, as a result of nitrogen addition, a clear drop in the density of the metal (Ti) atoms can be detected. Due to the target poisoning, the density of sputtered Ti drops by a factor of about 4 when the nitrogen content in the discharge exceeds ≈5%. The relative density of Ti ions in this case is measured using mass-spectrometry, demonstrating the same effect. Based on this example, we can conclude that the (real-time) measurements of the absolute density using absorption spectroscopy, contrary to the well-known plasma emission monitoring method [58], may have additional benefits for reactive sputtering since the emission is always defined by electron excitation and may be weak at the high distances from the target. In addition, the spatial selectivity of ROAS may also be better than that of OES, since the collimated beam used in this case can be highly focalized and thin, especially if a laser is used as a reference source [27].
Evolution of the absolute Ti ground state density measured by ROAS (filled squares) and Ti+ relative density obtained by mass spectrometry (open squares) in a reactive DCMS discharge as a function of the nitrogen content. Ar pressure = 30 mTorr, applied power = 500 W, z = 8 cm. Reproduced with permission from Konstantinidis et al. [54]. Copyright 2005 Elsevier Publishing.
HiPIMS discharges, possessing very short plasma on time, as illustrated in Figure 2, demonstrate different physics from that known for the DCMS discharges. The main reason for this is significantly elevated plasma density as well as the ionization degree related to both the bulk gas and the sputtered particles in HiPIMS, as mentioned in the Introduction and analyzed in the numerous works. Despite the fact that DCMS and HiPIMS sputtering processes can be realized using the same magnetron source, the direct comparison between these discharges is rather difficult, especially at the high values of the peak power applied to HiPIMS (or cathode current density), even though the time-averaged level of the applied power might be the same. In this section, for the sake of illustration of the dynamics of HiPIMS discharge in terms of the absolute density of species, the time-resolved evolution of the main discharge species in an Ar-Ti short-pulsed HiPIMS discharge analyzed by ROAS is presented. The experimental details on the HiPIMS system used for diagnostics are listed in Table 1, whereas the corresponding spectroscopic data are available in Table 2, or can be found elsewhere [31,38].
The time-resolved evolution of the absolute densities of Ti and Ti+ atomic species sputtered in a 20-µs pulse Ar-Ti HiPIMS discharge measured at z = 5 cm above the target is shown in Figure 10. The total density in this case represents the sum of populations of the corresponding ground state sublevels (see Table 2). As we can observe from this figure, after a small density decrease (depletion) during the plasma on time, the Ti density is peaking at the time delay ∆t ≈100 µs and reaches the value of about 6 × 1011 cm–3. The number density is found to be proportional to the pulse duration in this case, as far as the other discharge parameters are the same, which should be due to the change in the pulse energy (0.13 vs. 0.26 J). The pulse duration effect is also valid for the Ti ions in HiPIMS (not shown). The decrease in Ti density at the end of the plasma on time (roughly twice) is likely related to the VDF broadening of the sputtered particles during this time, neglected during the density calculation, as explained in [38]. In this case, an increase in the VDF width during the plasma on time observed by Palmucci et al. [44] results only in ~20% of the total density drop, which is less than the depletion visible in Figure 10(a) for Ti. This implies a presence of the additional factors responsible for density depletion, such as ionization of the sputtered particles, as discussed by Britun et al. [37]. Quantitative estimation of the different contributions is barely possible in this case, primarily due to the strong plasma emission in this time interval, which results in high deviation of the obtained data. The error bar shown in Figure 7(a) represents a standard deviation of the data points corresponding to several independent ROAS measurements, whereas the density data correspond to the values averaged among several measurements, as well as among three Ti ground state energy sublevels listed in Table 1.
Time-resolved evolution of the Ti (a) and Ti+ (b) number density in Ar-Ti HiPIMS discharge measured by ROAS. The A and B time intervals correspond to the density depletion and the current self-organization, respectively. Six independent measurements have been undertaken in the case of Ti+ continuously showing the density instabilities in the interval B. Ar pressure = 20 mTorr, z = 5 cm. Reproduced with permission from Britun et al. [38]. Copyright 2015 AIP Publishing.
The evolution of the Ti ion density shown in Figure 10(b) reveals similar tendencies, especially during the plasma off time, where the density has a maximum at 100–200 µs, reaching ~3 × 1011 cm–3. During the plasma on time, two phenomena can be observed: the first one is the beginning of density depletion interval, which is similar to that found for Ti neutrals (called interval A), and the second one which characterized by the strong instabilities of the measured Ti+ density at the end of the plasma on time, resembling the stochastic density behavior (called interval B). Note that six independent density measurements made during the plasma on time always lead to the different Ti+ density evolution. Since Ti ionization is likely defined by the electrons presented in the discharge volume during this time (
(where
Typical example of the time evolution of Ti+ (a) and Ti (b) emission line intensity in Ar-Ti HiPIMS discharge comparing to the intensity of the same emission lines in the reference source (HCL) showing a dramatic increase in the emission intensity at the end of the HiPIMS pulse. Ar pressure = 20 mTorr, z ~1 cm.
Summary of time evolution of the absolute density corresponding to the main discharge species in Ar-Ti HiPIMS discharge measured by ROAS. Three main time intervals corresponding to the secondary electron wave propagation, rarefaction, and refill are indicated. Ar pressure = 20 mTorr, z = 5 cm. Reproduced with permission from Britun et al. [21] (Copyright 2014 IOP Publishing) and Britun et al. [22] (Copyright 2015 WILEY-VCH Publishing).
The summary of the time evolution of several atomic species studied in a 20-µs Ar-Ti HiPIMS discharge at z = 5 cm is given in Figure 12. From this figure, the main stages of HiPIMS discharge can be distinguished. First, after the discharge ignition, the excitation of Ar and Ti atoms remaining from the previous plasma pulse is taking place, as a result of propagation of the secondary electrons away from the cathode. The background Ti density is found to be ~2 × 1011 cm–3, whereas the density of Ti metastables is much lower (~1010 cm–3) for the considered conditions. The propagation of the hot electrons [64,65] results in formation of the Ar and Ti metastable states (Armet, Timet) as well as in the intensive Ti ionization during the plasma on time–beginning of the plasma off time, which is accompanied by the inversion of population of the Ti energy sublevels, as discussed below. At the beginning of the plasma off time, the density of metal ions increases (red triangles in Figure 12), corresponding to their transport toward the volume analyzed by ROAS. Second, the depletion of Ti density at the end of the plasma on time is also visible. This depletion can be induced by the VDF broadening of Ti neutrals at the end of the plasma pulse [44]. Apart from this, a strong ionization of the sputtered neutrals in this region should also contribute to the observed density depletion [37,38]. Third, the strong excitation and ionization above the target are followed by rarefication of the bulk gas, resulted by the sputtered Ti species incoming to the studied volume, which is clearly observable together with a decrease in the Armet density, and also supported by the recent 2D density mapping results [37]. This process should be accompanied by electron cooling, as a result of collisions with the incoming heavy particles [64]. The ionization of sputtered Ti is taking place during the same time interval (20–100 µs), presumably as a result of the direct electron impact (
\n\t\t\t\tTime\n\t\t\t | \n\t\t\t\n\t\t\t\tParticle\n\t\t\t | \n\t\t\t\n\t\t\t\tProcesses\n\t\t\t | \n\t\t\t\n\t\t\t\tMain reaction(s)\n\t\t\t | \n\t\t\t\n\t\t\t\tEvidence\n\t\t\t | \n\t\t
\n\t\t\t\t0–5 µs\n\t\t\t | \n\t\t\tElectrons | \n\t\t\tGeneration | \n\t\t\t\n\t\t\t | \n\t\t |
Ar | \n\t\t\tIonization + acceleration toward the cathode | \n\t\t\t | \n\t\t\tRelated works [15] | \n\t\t|
Ti | \n\t\t\tHave their “background” density level, remaining from previous plasma pulse. | \n\t\t|||
Timet\n\t\t\t | \n\t\t||||
Ti+\n\t\t\t | \n\t\t||||
\n\t\t\t\t5–20 µs\n\t\t\t | \n\t\t\tElectrons | \n\t\t\t\n\t\t\t\tElectron wave propagation (secondary hot electrons— | \n\t\t\t\n\t\t\t | LIF imaging data [37], Langmuir probe measurements [77] | \n\t\t
Armet\n\t\t\t | \n\t\t\tGeneration by | \n\t\t\t | \n\t\t\tLIF imaging data [37] | \n\t\t|
Ti | \n\t\t\tVDF broadening and strong ionization, resulting in density depletion | \n\t\t\t\n\t\t\t | LIF imaging data [37], measured VDF width [44] | \n\t\t|
Timet\n\t\t\t | \n\t\t\tGeneration by | \n\t\t\t | \n\t\t\tPresence of Armet during this interval [37] | \n\t\t|
Ti+\n\t\t\t | \n\t\t\tGeneration by | \n\t\t\t | \n\t\t\tNot visible, probably due to the discharge current instabilities [59,60] | \n\t\t|
\n\t\t\t\t20–50 µs\n\t\t\t | \n\t\t\tElectrons | \n\t\t\t\n\t\t\t\tElectron wave (gradual cooling) | \n\t\t\t\n\t\t\t | LIF imaging data [37], inversion of sublevel populations [67] (Figures 13 and 14). | \n\t\t
Armet\n\t\t\t | \n\t\t\t1. Saturation, rarefication 2. Quenching by incoming Ti neutrals | \n\t\t\t2. | \n\t\t\t1. Decrease in [Armet], Related studies [15,26] 2. LIF imaging data [37] | \n\t\t|
Ti | \n\t\t\t1. Propagation of sputtered Ti 2. Ti VDF relaxation | \n\t\t\t\n\t\t\t | 1. LIF imaging data [37]2. Related studies [44,45] | \n\t\t|
Timet\n\t\t\t | \n\t\t\tFollow the growth of [Ti] | \n\t\t\t | \n\t\t\tSame growth rate for Ti and Timet (Figure 12) | \n\t\t|
Ti+\n\t\t\t | \n\t\t\tGeneration (following Ti wave) | \n\t\t\t1. | \n\t\t\t1. Faster growth of [Ti+] and slower growth of [Ti] at the same time 2. Negligible, due to very small drop in [Armet] (Figure 12) | \n\t\t|
\n\t\t\t\t50–200 µs\n\t\t\t | \n\t\t\tElectrons | \n\t\t\tThermalization | \n\t\t\twhere | \n\t\t\tLoss of the inversion of sublevel populations (Figure 14), Langmuir probe data [64,65], modeling [78] | \n\t\t
Armet\n\t\t\t | \n\t\t\t\n\t\t\t\tRarefication\n\t\t\t | \n\t\t\t\n\t\t\t | Figure 12 | \n\t\t|
Ti | \n\t\t\tDiffusion | \n\t\t\t\n\t\t\t | Gradual decrease of [Ti | \n\t\t|
Timet\n\t\t\t | \n\t\t\tQuenching, diffusion | \n\t\t\twhere | \n\t\t\tPermanent density drop, as well as [Timet]/[Ti] ratio drop (Figure 12) | \n\t\t|
Ti+\n\t\t\t | \n\t\t\tDensity saturation (production-loss balance) | \n\t\t\t\n\t\t\t | Figure 12 | \n\t\t|
\n\t\t\t\t200–1000 µs\n\t\t\t | \n\t\t\tElectrons | \n\t\t\tThermalized | \n\t\t\t\n\t\t\t | Related works [64,65,78] | \n\t\t
Armet\n\t\t\t | \n\t\t\t\n\t\t\t\tRefill \n\t\t\t | \n\t\t\t\n\t\t\t | Increase in [Armet], refill time estimations [26,66] | \n\t\t|
Ti | \n\t\t\tContinuing diffusion | \n\t\t\t\n\t\t\t | Gradual decrease of [Ti | \n\t\t|
Timet\n\t\t\t | \n\t\t\tReaching background [Timet] level ~1010 cm–3. | \n\t\t\t\n\t\t\t | Figure 12 | \n\t\t|
Ti+\n\t\t\t | \n\t\t\tSlight drop after 600 µs, might be due to: | \n\t\t\t1. 2. where | \n\t\t\t1. [Ti+] drop + [Armet] increase 2. [Ti+] drop (Figure 12) | \n\t\t
An interesting effect can be observed if the measured density is represented separately for each energy sublevel at the studied electronic state, as shown in Figure 13. As one can observe, a clear inversion among the studied energy states is achieved for five Ti sublevels corresponding to the metastable Ti a5FJ states (see Table 2). An inversion of the considered energy sublevels (i.e., when the population of the state corresponding to higher energy is found to be higher) takes place in Figure 13(a) during the 20- to 100-µs time interval. The maximum of the mentioned inversion for Timet case is located around Δt ≈60 µs. Similar but much weaker effect for Ar metastables (only two levels are considered) is also visible in Figure 13(b).
Time-resolved number density evolution for Ti (a) and Ar (b) metastable atoms measured by ROAS in Ar-Ti HiPIMS showing the populations of the corresponding energy sublevels (see Table 2). The total density evolution is given by gray lines for comparison. Ar pressure = 20 mTorr, z = 5 cm. Reproduced with permission from Britun et al. [38]. Copyright 2015 AIP Publishing.
Despite the fact that the inversion effect is rather new for HiPIMS, it is well known for the other low-temperature discharges, such as Ti hollow cathode plasma [67], and RF-amplified DCMS discharge [30]. In the former case, it is explained by the (partial) equilibrium of the heavy discharge species with the energetic electrons during the short plasma on time interval. Besides this, the inversion of the sublevel populations might be also responsible for the apparent density depletion in the magnetron target vicinity detected in the DCMS discharges [30,49,68,69]. The sublevel inversion can be explained based on the Boltzmann distribution of the corresponding energy sublevel populations. Assuming the presence of the dense flux of hot electrons during certain time in the discharge, the heavy particles should be intensively excited by the electrons during this time. Under these conditions, for the close energy sublevels, the factor
where
which, after normalization to
The sublevel inversion is even more clear if a “stabilized” modification of the resonant absorption method is implemented, when a pulsed reference source is synchronized with the time gate of the ICCD detector, as discussed above. The relative error of the ROAS measurements can be significantly reduced in this case, and fine spectral effects in the discharge, such as inversion of the energy sublevels, can be easily visualized. The example of these measurements using three Ti ground state energy sublevels is given in Figure 14. In Figure 14(a), the experimental ROAS results, clearly showing the presence of the Ti ground state sublevel inversion (roughly between 20 and 300 µs), are shown. At the same time, a sketch of the same level populations drawn in accordance to the inversion model described by Eqs. (6) and (7) is given in Figure 14(b) for the sake of clarification of the experimental data. We have to note that before the inversion interval, the studied Ti sublevels do not perfectly follow the Boltzmann distribution, as the middle level is mostly populated in this case. This fact might be due to the complicated HiPIMS discharge kinetics, which is not well studied yet. Let us also note that the inversion interval might be significantly shifted in time depending on position of the ROAS line of sight, and the inversion should happen much earlier if the measurements are performed closer to the target surface.
The time-resolved populations of three ground state Ti energy sublevels (a) measured in Ar-Ti HiPIMS discharge by ROAS using the dynamic source triggering. Ar pressure = 20 mTorr, z = 5 cm. A sketch (b) illustrating the dynamics of the Ti sublevels population as a function of time in HiPIMS. The beginning of the inversion interval should depend on the observation point (z) and should start earlier if the ROAS line-of-sight is located closer to the target.
Fitting the experimental data corresponding to Ti sublevels, the Ti excitation temperature can be obtained, which is a measure of excitation of the corresponding energy sublevels by the hot electrons. In our case, the estimations lead to
It is also interesting to consider some selected phenomena in the case of reactive HiPIMS discharge. The behavior of the number density of the sputtered species in reactive HiPIMS should follow the same tendency as in the reactive DCMS case (shown in Figure 9), i.e., a density drop by several times in the poisoned regime of sputtering should be expected. Let us consider the behavior of the absolute density of reactive species here. The presented example is related to the time-behavior of the absolute density of the atomic oxygen measured by ROAS. This question has been particularly studied by Vitelaru et al. [71] using a tunable diode laser and giving the dynamics of the atomic oxygen in the HiPIMS discharge, however, without measuring its absolute density, which is a very important parameter, as mentioned in Section 1. In the considered case, a discharge-based ROAS with simultaneous signal acquisition (see Figure 6) has been applied for measurements of the absolute density of O atoms in the HiPIMS discharge volume. Due to the spectral limitations, however, the ground state O atoms are not accessible by ROAS (the corresponding transitions are located in the deep UV range [72]), so only the O metastable atoms (Omet, 3s 5S°2 level with the energy = 9.15 eV) are analyzed in this case. A microwave surfaguide discharge [73] operating at 2.5 GHz and using Ar–7% O2 gas mixture has been utilized as a reference source in this case.
Analyzing the Omet atoms in any discharge, one should bear in mind that these are excited species which keep the dynamics of the plasma electrons as well as the dynamics of the ground state O2 and O. The time evolution of Omet atoms measured by ROAS at z = 5 cm in the HiPIMS discharges working with Ar–20% O2 gas mixture and using Ti and Ag targets is shown in Figure 15. The typical stages of nonreactive sputtering discharge can be observed in this case (compare to Figure 12). The first noticeable processes are the Omet density depletion at the beginning of the plasma on time (visible in the Ti target case only) followed by the density increase at the end of the plasma on time. These processes are followed by the rarefication of Omet and the gas refill afterward (exists both for Ti and Ag target cases). We would like to emphasize that both in Ti and Ag cases the Omet density starts to increase already at the end of the plasma on time, unlike in the nonreactive case. Such an increase correlates well with the time-resolved dynamics of the Ar metastables in the nonreactive case, as shown in Figure 12. This similarity, as well as the proximity of the excitation thresholds for these species (11.55 eV for Armet vs. 9.15 eV for Omet [74]) point out on the role of the secondary electrons in formation of the Omet state, which should take place already during the plasma on time (i.e.,
Time-resolved evolution of the absolute density of O metastable atoms (3s 5S02 state) measured by ROAS in HiPIMS discharge using Ar–20% O2 gas mixture for the case of Ti (a) and Ag (b) cathode. Ar pressure = 20 mTorr, z = 5 cm. Pulse duration, discharge frequency, and pulse energy (EP) are, respectively, 20 ms, 1 kHz, 0.3 J (a) and 50 ms, 0.1 kHz, 0.42 J (b). Reproduced with permission from Britun et al. [22]. Copyright 2015 WILEY-VCH Publishing.
Since in the case of Ar–20% O2 gas mixture magnetron target is supposed to be completely oxidized [47], the sputtering of oxide material from (i.e., MxOy molecules, where M is a metal atom) followed by formation of O atoms and finally Omet should be another possible mechanism of the observed Omet density elevation at the end of the plasma on time. This mechanism, however, is supposed to be rather minor since the wave of the sputtered species arrives in the volume of measurements much later, having the maximum at Δt ≈100 µs, as shown in Figure 12.
Resonant absorption analysis of the direct current sputtering discharges shows that the absolute density of the sputtered particles is ranged in a relatively narrow interval, being always in the range of 1010–1012 cm–3 in the Ti case (assuming the average power level to be several hundred Watt). These values may be somewhat different varying the cathode materials with essentially different sputtering yield and/or in the sputtering systems, which use significantly higher power levels. The spatial distribution of the sputtered particles is mainly determined by their diffusion (at high pressure), by the angular directivity of sputtering (low pressure), as well as by the magnetic field topology (critical mainly for the sputtered ions), which lead to nearly exponential decay of the observed density of species as a function of the distance from cathode, so the density might decay at least by one order of magnitude already at few cm away from the target surface (for 5 cm diameter round target).
One of the advantages of using ROAS technique for diagnostics of sputtering processes is its ability to probe the species in a wide range of absolute density, starting from roughly 107–108 cm–3, where the signal-to-noise ratio of the used detector is a limiting factor, and finishing by the values several orders of magnitude higher, when the increase of the optical thickness of the volume of interest becomes the limiting factor. The bottom sensitivity level may be additionally affected by the type of the absorption scheme used (e.g., single-pass, multipass, with or without simultaneous signal acquisition, etc.). The variety of the ROAS implementation schemes allow real time monitoring of the sputtered species also during reactive sputtering, which is very demandable, as the synthesis of the compound (oxides, nitrides, etc.) coatings is one of the main sputtering workflow nowadays. Since the density drop between the “metallic” and “reactive” mode of sputtering normally drop by about one order of magnitude, the absolute density levels in both modes can be easily real time monitored by absorption technique, which might be useful for research-oriented as well as for industry applications. This conclusion is valid both for DCMS (as shown in this work), pulsed-DC, as well as for HiPIMS discharges.
The physical phenomena in the HiPIMS discharges are rather different from those observed in DCMS and P-DCMS cases, first of all in terms of the plasma density and much shorter timing (µs scale). As a result, numerous dynamic effects should be taken into account explaining the properties of the HiPIMS discharges. Among these effects, the following time-dependent phenomena should be mentioned: the propagation of the fast electron wave the dynamic gas rarefaction and refill, the ionization and excitation of various discharge particles, quenching of the excited states as a result of collisions, the anomalous electron transport, etc. ROAS technique, being essentially limited by only the time-resolution of the used optical detector, suits very well for systematic characterization of these discharges in terms of the absolute density. In addition, the modern ICCD detectors typically provide ns time resolution, which surpasses the typical HiPIMS time scale by few orders of magnitude.
In terms of the time-resolved evolution of the discharge particles density, there are several processes in HiPIMS discharge, which can be visualized using ROAS technique. The time-resolved summary of these processes is given in Table 3, considering the main discharge species studied in the Ar-Ti nonreactive HiPIMS case. The presence of such dynamic effects as the density depletion, gas rarefaction, gas refill, quenching of the metastable states, ionization, as well as the propagation of the electron wave away from the target surface can be concluded based on the undertaken ROAS analysis. Despite a rather high HiPIMS repetition rate considered in this work (1 kHz), the gradual relaxation for the majority of the listed processes till the end of the plasma off time can be observed. Even though the total range of the measured absolute density of the discharge species reaches nearly three orders of magnitude in the considered case, the detected densities are still well above the detection threshold (which is estimated to be roughly 107–108 cm–3 with the detection scheme used). The sensitivity of the used ROAS method can be additionally enhanced using the lock-in detection technique, dynamic triggering of reference source, and related approaches.
One of these approaches, namely, the simultaneous acquisition of the emission signals using a triple optical fiber, has been utilized for time-resolved detection of the oxygen metastable atoms during the reactive HiPIMS process. The results reveal the presence of the same discharge phases (such as gas rarefaction and refill, as well as the density depletion in some cases) as detected in the nonreactive HiPIMS case. The absolute density of the O metastable atoms detected in this case is still above the mentioned ROAS sensitivity threshold, being in the range of 108–109 cm–3. The optical diagnostics of the reactive HiPIMS discharges, however, is a relatively new area and the obtained results require additional verification by the other methods, such as LIF, in order to be understood completely.
The resonant absorption technique represents a powerful diagnostic tool suitable for the determination of the absolute density of the relevant species in sputtering discharges, such as DCMS, P-DCMS, HiPIMS, as well as the other types of magnetron discharges. This technique has several modifications allowing its optimization depending on the discharge geometry etc. For example, using a plasma discharge as a reference source, ROAS setup can be rather simple, requiring only the additional optics for reference source beam collimation, and (sometimes) additional synchronization between the source and the discharge of interest. Both direct current and pulsed reference sources can be used for resonant absorption purposes. In addition to this, in case a broad range spectral detector, such as ICCD, is utilized, a parallel detection of several spectral transitions as well as the corresponding absolute densities becomes possible. These advantages open new possibilities to study the basic effects in the discharge volume. Among these effects are the population of the metastable levels of the various discharge species, the population of the atomic energy sublevels of the atoms and their time-resolved dynamics, the study of the excitation temperature across the discharge volume, etc. These possibilities are important for studying magnetron sputtering processes at the fundamental level, whereas rather basic configuration of the ROAS setup may be helpful in industry, e.g., for real-time density monitoring of the relevant species during a certain process.
The sensitivity of the absorption method can also be significantly improved by varying the detection schemes, such as lock-in amplification (improving the sensitivity by 1–2 orders of magnitude typically), multipass methods, as well as by simultaneous signal acquisition, dynamic source triggering, etc. Using the simultaneous signal acquisition for example, the sensitivity below 108 cm–3 has been achieved for O metastable atoms in a reactive HiPIMS discharge case, as illustrated in this chapter. This value is far below the typical concentrations of the sputtered atoms in the discharge (1010–1012 cm–3) achieved under the laboratory conditions, which is enough for most applications. For very weakly populated energy states, like those appearing in molecular discharges, the multipass absorption, including the ring-down spectroscopy method, could be suggested, which are, being out of the scope of this chapter, still based on the same fundamental principles.
This work is supported by the Belgian Government through the “Pôle d’Attraction Interuniversitaire” (PAI, P7/34, “Plasma-Surface Interaction,” Ψ). N. Britun is a postdoctoral researcher; S. Konstantinidis is a research associate of the Fonds National de la Recherche Scientifique (FNRS), Belgium.
Sikkim enjoys a wide range of climate, physiographic, geology, and vegetation that influence formation of different kinds of soils. Hills of Sikkim mainly consist of gneissose and half-schistose rocks, producing generally poor and shallow brown soils [1, 2]. The soil is coarse, with large concentrations of iron oxide, and ranges from neutral to acidic, making it lacking in mineral nutrients. This type of soil tends to support evergreen and deciduous forests [3]. Rock consists of phyllites and schists, which is much younger in age and is highly susceptible to weathering and erosion [4, 5, 6, 7, 8]. This combined with the state’s heavy rainfall causes extensive soil erosion and the loss of soil nutrients through leaching. Soils of Sikkim belong to 3 orders, 7 suborders, 12 great groups, and 26 subgroups. It is observed that inceptisols are dominant (42.84%) followed by entisols and mollisols occupying 42.52 and 14.64%, respectively. Percentage area under Zn deficiency (<0.6 mg kg−1) in Sikkim is 15.69% (202.35 sq. km) of the geographic area having highest Zn deficiency in South Sikkim district (82.07 sq. km, 19.1% of TGAD) followed by East (56.84 sq. km, 13.3% of TGAD), West (48.91 sq. km, 15.7 of TGAD), and North (14.53 sq. km, 11.8% of TGAD). Percentage area under Mn deficiency (<3.5 mg kg−1) in Sikkim is 10.16% (131.02 sq. km) of the geographic area having highest Mn deficiency in South Sikkim (48.72 sq. km, 11.3 of TGAD) followed by East (34.52 sq. km, 8.1% of TGAD), North (28.82 sq. km, 23.13% of TGAD), and West (18.96 sq. km, 6.1% of TGAD). Total degraded area in Sikkim is 60,000 ha (9% of TGA), of which West Sikkim is highly degraded, followed by South Sikkim and North Sikkim [9, 10, 11, 12, 13]. Erosional hazard has affected about 2000 ha (0.28% of TGA of the state). South Sikkim is the worst affected district, followed by West Sikkim and North Sikkim [14, 15]. Sikkim being hilly state practicing terraced agriculture on an extensive scale could successfully control soil erosion [16].
\nThe major challenge in organic agriculture is the availability of huge quantities of organic inputs for satisfying the farm demand. The use of animal excreta-based manure alone is not sufficient for meeting the nutrient needs of the crops. It is, therefore, necessary to utilize all the sources available on and off farm effectively [17]. The resource components available for nutrient management in organic horticulture are the following: farmyard manure (FYM), crop residue, weed biomass, green manures, biofertilizers, composts/phospho-compost, vermicomposting, oil cakes, mulching/cover crop, liquid manures, biodynamic preparation, botanicals, legumes in cropping sequence, and certified commercial products. Maintenance of soil fertility may be achieved through organic matter recycling, enrichment of compost, vermicomposting, animal manures, urine, farmyard manure, litter composting, use of botanicals, green manuring, etc. Biofertilizers like Azolla, Azospirillum, Azotobacter, Rhizobium culture, PSB, etc. can be used. Sawdust from untreated wood, calcified seaweed, limestone, gypsum, chalk, magnesium rock, and rock phosphate can be used [18]. Various sprays like vermiwash, liquid manure, etc. can be used in crops for nourishing the soil and plant. Farmyard manure, compost, and green manure are the most important and widely used bulky organic manures. Partially decomposed FYM has to be applied 3–4 weeks before sowing, while well-decomposed FYM should be applied immediately before sowing [19]. Manuring with different short-duration legumes is suitable for maintenance of soil quality in terms of adding nitrogen to soil. Nitrogen addition by sun hemp (150–200 kg/ha N) and dhaincha (125–175 kg/ha N) is highly beneficial for the succeeding crops and even for the subsequent crops too. Crop residue can also produce 2.47 kg N, 0.53 kg P, and 8.87 kg K per ha. Edible oil cakes of mustard and nonedible oil cakes from neem, karanj, and castor can serve the dual purpose of manure and bio-pest control [20, 21, 22, 23, 24, 25]. Vermicompost can be used for a wide variety of horticultural, ornamental, and vegetable crops at any stage. Generally vermicompost is applied at 3–5 t/ha in row zones for field crops, whereas, for fruit crops, it is preferred to use the same mixing with equal amount of FYM in periodic interval. The general recommendation dose of vermicompost is 6–8 t/ha for field crop and 3–5 t/ha for subtropical fruits [26, 27]. In case of soil application, desired strain of biofertilizer is normally mixed with 20 times well-decomposed FYM to maintain uniformity of mixture and applied in furrows. However, for seedling treatments, biofertilizer slurry is made (1:10 ratio) in water, and roots are emerged in suspension for about 30 minutes. For cereals like, maize, baby corn, buckwheat, upland rice, and finger millet, it was suggested to apply 10–20 t/ha FYM along with 5.0 t/ha vermicompost, whereas, for low P and low K, the dosages are 6–12 t/ha FYM and 3–4 t/ha vermicompost. It is suggested that goat/pig/poultry at 3.0 t/ha along with FYM at 5.0 t/ha is a good source of organic zinc supplement in zinc-deficient soils. For spices like ginger, turmeric, and large cardamom, it is suggested to apply well-decomposed FYM along with neem cake at 3.0 t/ha and biofertilizer slurry in rows at planting time in variable dosages under low NPK situations [28]. The temperate climate with high organic matter is highly suitable for fruits like mandarin, chayote, strawberry, pear, etc. in the state. Application of well-decomposed FYM along with neem cake and vermicompost at variable dosages during land preparation and biofertilizer treatment before transplanting can be beneficial for improving fruit quality even under the stress of NPK in soils [29].
\nFor rainfed areas, the predominant cropping systems are maize + beans-vegetable pea; maize + beans-barley; maize + beans-rajma; maize + beans-buckwheat; maize + beans-toria; soybean-buckwheat; and soybean-toria. For irrigated areas, the predominant cropping systems are maize (green cobs)-pahenlo dal-buckwheat; maize-vegetable pea; rice-vegetable pea-maize (green cobs); rice-fenugreek (leafy vegetable)-baby corn; rice-sunflower-dhaincha (green manuring); and rice-vegetable pea. Important vegetable cropping systems under low-cost plastic tunnels are broccoli-spinach-coriander-broccoli-coriander system; broccoli-coriander-cabbage-radish-coriander system; coriander-radish-fenugreek-spinach-coriander system; cabbage-local rayo sag-broccoli-coriander system; cabbage-spinach-broccoli-coriander system; and coriander-radish-fenugreek-cauliflower-pak choi system [30, 31]. Important vegetable cropping sequences for low-cost plastic rain shelter are tomato-pea-tomato system; bitter gourd-pea-tomato system; bottle gourd-capsicum-pea system; and sponge gourd-pea-tomato system. Important vegetable cropping sequences for low-cost polyhouse are cucumber-cabbage-tomato system; capsicum-broccoli-tomato system; and cucumber-cauliflower-tomato system. Important vegetable cropping sequences for open condition are okra-pea-cole crops system; okra-cole crops-local rayo sag/leafy vegetables system; dalley chili + local rayo sag/leafy vegetables as intercrop; okra-garlic-local rayo sag/leafy vegetables system; ginger-pea system; and okra-potato-local rayo sag/leafy vegetables system. Table 1 represents the organic nutrient available in Sikkim from all possible sources.
\nSl. no. | \nAnimal | \nLivestock population of Sikkim (19th livestock census 2012) | \nManure production rate per animal per day in kilograms | \nAmount of manure produced per day (in kilograms) | \nManure/year (tons) | \nManure/year On dry weight basis (in tons) | \n
---|---|---|---|---|---|---|
1 | \nCattle | \n140,467 CB—126,519 Ind.—13,948 | \n25–30 | \n3,511,675–4,214,010 | \n1281761.375–1538113.65 | \n384528.4125–461434.095 | \n
2 | \nBuffalo | \n703 | \n25–30 | \n17,575–21,090 | \n6414.875–7697.85 | \n1924.4625–2309.355 | \n
3 | \nSheep | \n2634 | \n2–3 | \n5268–7903 | \n1922.82–2884.595 | \n576.846–865.3785 | \n
4 | \nGoat | \n113,364 | \n2–3 | \n226,728–340,092 | \n82755.72–124133.58 | \n24826.716–37240.074 | \n
5 | \nPig | \n29,907 | \n5 | \n149,535 | \n54580.275 | \n16374.0825 | \n
6 | \nYak | \n4036 | \n25 | \n100,900 | \n36828.5 | \n11048.55 | \n
7 | \nPoultry | \n451,966 | \n0.6 | \n271179.6 | \n98980.554 | \n29694.1662 | \n
Total | \n4282860.6–5104709.6 | \n1563243.9–1863219 | \n468973.17–558965.7 | \n
Organic nutrient available in Sikkim from all possible sources.
\n
Maize (Zea mays L.): Application of dolomite at 2 t/ha + mixed compost at 2.5 t/ha + neem cake at 0.5 t/ha + vermicompost at 2.5 t/ha (ICAR Sikkim, 2011). Apply FYM at 15 t/ha 20 days before planting along with 150 kg rock phosphate. Neem cake at 150 kg/ha for nutrient supply and control of soilborne insect pests. Green manuring: sun hemp and dhaincha another alternative. Seed inoculant: Azospirillum, Azotobacter, and PSB at 20 g/kg seed.
Rice (Oryza sativa L.): Apply FYM at 10 t/ha to supplement recommended dose of N + P + K for maintaining soil fertility. Practice of raising a pre-kharif crop like green gram, cowpea, sun hemp, or Sesbania for use as green manure. Biofertilizers (blue-green algae or Azolla) capable of providing 20–25 kg N/ha. Neem cake at 150 kg/ha provides protection against soilborne diseases and improves nutrition of rice crops. 5 t FYM + 2 t vermicompost + green manures/weed biomass before 20 days transplanting and 250–300 kg neem cakes during transplanting of rice crop are best nutrient management options. Mixed compost at 15 t/ha + neem cake at 1 t/ha. Green manure crops like dhaincha, sun hemp, and cowpea capable of accumulation of 4–5 t/ha of dry biomass and 100 kg N2/ha in 50–60 days.
Rapeseed and mustard (Brassica sp.): Apply FYM at 10 t/ha or vermicompost at 5 t/ha during last field preparation. Vermicompost along with Azotobacter and PSB considerably enhances mustard yield. Apply different oil cakes at 0.5 to 1.0 t /ha to meet demand of micronutrient and S demand of the crop. Mixed compost at 5 t/ha + vermicompost at 1.0 t/ha + neem cake at 1.0 t/ha + dolomite at 1.0 t/ha was recommended (ICAR Sikkim, 2011).
Soybean (Glycine max) (L.) Merr.: Being a leguminous crop, require less N than other crops. Apply FYM at 5–10 t/ha and incorporate into soil during final land preparation. Apply neem cake at 1 t/ha + mixed compost at 2.5 t/ha + dolomite at 1 t/ha (ICAR Sikkim, 2011). Seed inoculation with Bradyrhizobium japonicum culture (500 g/75 kg seed) + PSB/PSM (6.5 g/ kg seed).
Buckwheat (Fagopyrum esculentum Moench.): Application of vermicompost at 1.5 t/ha recorded the higher grain yield of buckwheat. Efficient crop in extracting phosphorus of low availability from the soil. Azophos seed treatment (APST) + mixed compost at 5 t/ha + neem cake at 0.5 t/ha (ICAR Sikkim, 2011).
Baby corn (Zea mays L.): Well-decomposed FYM at 10 t/ha should be applied 20 days before sowing of crop. Baby corn should be inoculated with N-fixing nonsymbiotic microorganism like Azospirillum, Azotobacter, etc. and PSB at 20 g/kg seed.
Finger millet (Eleusine coracana): Apply 5 t FYM/ha 15 days prior to sowing of the crop. Biofertilizers like Azospirillum brasilense (N-fixing) and Aspergillus awamori (P-solubilizing) apply at 25 g/kg seed.
Black gram (Vigna mungo L.): FYM or mixed compost at 5 tons/ha enhances the yield. Seed inoculation with Rhizobium strains increases seed yield and uptake of nutrients. Additional nutrient may be supplied through water-soluble organic granules at 5 kg/acre mixed with FYM, vermicompost, or mixed compost.
Large cardamom (Amomum subulatum Roxb.): If the land is not terraced, soil base may be made by cutting topsoil from upper half and placed on lower half followed by mulching. At plant base, mulching with easily degradable organic materials is good for conserving both moisture and soil. Mulching improves soil physical condition and fertility. Dried organic matter, leaves, weeds, etc. can be used as mulch. During planting, pits are filled with topsoil mixed with FYM at 1–2 kg/pit. FYM/compost at 5 kg/plant at least twice a year in April to May and August to September is beneficial.
Ginger (Zingiber officinale L.): Well-decomposed and dried cattle manure or compost at 25–30 t/ha + neem cake at 2 t/ha + biofertilizer (Azospirillum + PSB) at 5–6 kg/ha helps in reducing incidence of rhizome rot of ginger and increases yield. Two months after planting, vermicompost at 5 t/ha should also be applied for better growth and production. Since edible part is rhizome, prior to planting of seed rhizome in soil, a half foot layer (6″) of leaf increases production of ginger by loosening soil texture around seed rhizome at later stages.
Turmeric (Curcuma longa L.): Needs heavy manuring. Apply FYM at 15–20 t/ha along with 250 kg neem cake or vermicompost at 10 t/ha. Integrated application of FYM at 10 t/ha and vermicompost at 5 t/ha along with 250 kg neem cake. O.M. along with biofertilizers like Azospirillum and Bacillus for better nutrition. Dolomite at 2 t/ ha to ameliorate soil acidity.
Mandarin (Citrus reticulata Blanco.): Young plants manured once/year, bearing plants twice/year (June to July and after harvesting in December to January) at 10–20 kg FYM/tree or 2–2.5 kg vermicompost/tree. Micronutrients through foliar sprays of water-soluble organic sources or nano-fertilizers at 0.2%. Dolomite at 100–200 g/plant for every second year. Neem cake at 2 t/ha during active growth stage in July to August.
Kiwifruit (Actinidia chinensis): Plants are heavy nitrogen feeders. Apply well-decomposed FYM at 25–30 t/ha and neem cake at 2 t/ha after vines have several inches of new growth during early spring. During active fruit growth stage, vermicompost at 2 kg/plant should also be given for better growth, production, and fruit quality.
Cole crops (Brassica spp.): Well-decomposed FYM or compost should be applied at 5.0 kg/m2 along with neem cake at 200 g/m2 at the time of final land preparation. Root dipping of seedlings in Azospirillum + PSB (20%) for 15 minutes at the time of planting. Additional application of vermicompost in cole crops at 1 kg/m2 further improves production.
Potato (Solanum tuberosum L.): Proper soil fertility management alone accounts for 20.7% of all yield contributing factors. Well-decomposed and dried cattle manure or compost at 25–30 t/ha and neem cake at 2 t/ha should be applied.
The most important crops which have been identified in Sikkim as commercial crop for marketing outside state are large cardamom, ginger, turmeric, buckwheat, cymbidium (flower), and tea. Table 2 represents the marketing of organic produce in Sikkim.
\nAgency | \nJurisdiction of marketing | \nProducts | \n
---|---|---|
Sikkim Marketing Federation (SIMFED) | \nWithin and outside Sikkim | \nSikkim mandarin, kiwi, ginger, turmeric, buckwheat, rajma, and vegetables | \n
Farmers Producers Organizations | \nWithin Sikkim | \nVegetables | \n
Nature’s gift (private entity) | \nOutside Sikkim | \nGinger, turmeric, buckwheat | \n
Marketing of organic produce in Sikkim.
Single-cropping should be avoided and preferably 2–3 crops should be grown together. If for any reason it is not possible to grow mixed or intercrops, then grow different crops in adjacent plots to maintain diversity. At any given time, legumes must occupy at least 30% of total cropping area. The legumes are nitrogen-fixing and can also be good source of mulching from the crop residues. High-yielding varieties require high nutrient inputs; they should be replaced with improved varieties suitable for organic management [31, 32, 33, 34, 35]. The same crop or same cropping sequence should not be repeated in the same field in two consecutive seasons/years (except for some legume crops such as mung bean or cowpea), and the field must be rotated every 2–3 years. Adoption of conservation tillage practices for improving soil quality and conserving soil moisture. Cover cropping, in situ residue management and restoration of degraded lands for soil moisture conservation, and improved C-sequestration should be practiced [36, 37]. Integrated farming systems and watershed development with animal, fishery, and suitable cropping for soil and moisture conservation and nutrient recycling should be practiced. The use of water-saving and nutrient-saving technologies, viz., system of rice intensification (SRI) and aerobic rice, should be popularized [38]. Rainwater harvesting: in situ (land configuration, mulching with locally available biomass, etc.) and ex situ (ponds, micro-water harvesting structures like jalkund\n
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