• Title/Summary/Keyword: thermal vacuum

Search Result 1,509, Processing Time 0.036 seconds

Recoverty of Lithium Carbonate and Nickel from Cathode Active Material LNO(Li2NiO2) of Precursor Process Byproducts (전구체 공정부산물 LNO(Li2NiO2)계 양극활물질로부터 탄산리튬 및 니켈 회수연구)

  • Pyo, Je-Jung;Wang, Jei-Pil
    • Resources Recycling
    • /
    • v.28 no.4
    • /
    • pp.30-36
    • /
    • 2019
  • In this study, Li powder was recovered from the by-product of LNO ($Li_2NiO_2$) process, which is the positive electrode active material of waste lithium ion battery, through the $CO_2$ thermal reaction process. In the process of recovering Li powder, the $CO_2$ injection amount is 300 cc/min. The $Li_2NiO_2$ award was phase-separated into the $Li_2CO_3$ phase and the NiO phase by holding at $600^{\circ}C$ for 1 min. After this, the collected sample:distilled water = 1:50 weight ratio, and after leaching, the solution was subjected to vacuum filtration to recover $Li_2CO_3$ from the solution, and the NiO powder was recovered. In order to increase the purity of Ni, it was maintained in $H_2$ atmosphere for 3 hours to reduce NiO to Ni. Through the above-mentioned steps, the purity of Li was 2290 ppm and the recovery was 92.74% from the solution, and Ni was finally produced 90.1% purity, 92.6% recovery.

Study on Structural Changes and Electromagnetic Interference Shielding Properties of Ti-based MXene Materials by Heat Treatment (열처리에 의한 Ti 기반 MXene 소재의 구조 변화와 전자파 간섭 차폐 특성에 관한 연구)

  • Han Xue;Ji Soo Kyoung;Yun Sung Woo
    • Journal of the Microelectronics and Packaging Society
    • /
    • v.30 no.3
    • /
    • pp.111-118
    • /
    • 2023
  • MXene, a two-dimensional transition metal carbide or nitride, has recently attracted much attention as a lightweight and flexible electromagnetic shielding material due to its high electrical conductivity, good mechanical strength and thermal stability. In particular, the Ti-based MXene, Ti3C2Tx and Ti2CTx are reported to have the best electrical conductivity and electromagnetic shielding properties in the vast MXene family. Therefore, in this study, Ti3C2Tx and Ti2CTx films were prepared by vacuum filtration using Ti3C2Tx and Ti2CTx dispersions synthesized by interlayer metal etching and centrifugation of Ti3AlC2 and Ti2AlC. The electrical conductivity and electromagnetic shielding efficiency of the films were measured after heat treatment at high temperature. Then, X-ray diffraction and photoelectron spectroscopy were performed to analyze the structural changes of Ti3C2Tx and Ti2CTx films after heat treatment and their effects on electromagnetic shielding. Based on the results of this study, we propose an optimal structure for an ultra-thin, lightweight, and high performance MXene-based electromagnetic shielding film for future applications in small and wearable electronics.

Highly Doped Nano-crystal Embedded Polymorphous Silicon Thin Film Deposited by Using Neutral Beam Assisted CVD at Room Temperature

  • Jang, Jin-Nyeong;Lee, Dong-Hyeok;So, Hyeon-Uk;Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2012.08a
    • /
    • pp.154-155
    • /
    • 2012
  • The promise of nano-crystalites (nc) as a technological material, for applications including display backplane, and solar cells, may ultimately depend on tailoring their behavior through doping and crystallinity. Impurities can strongly modify electronic and optical properties of bulk and nc semiconductors. Highly doped dopant also effect structural properties (both grain size, crystal fraction) of nc-Si thin film. As discussed in several literatures, P atoms or radicals have the tendency to reside on the surface of nc. The P-radical segregation on the nano-grain surfaces that called self-purification may reduce the possibility of new nucleation because of the five-coordination of P. In addition, the P doping levels of ${\sim}2{\times}10^{21}\;at/cm^3$ is the solubility limitation of P in Si; the solubility of nc thin film should be smaller. Therefore, the non-activated P tends to segregate on the grain boundaries and the surface of nc. These mechanisms could prevent new nucleation on the existing grain surface. Therefore, most researches shown that highly doped nc-thin film by using conventional PECVD deposition system tended to have low crystallinity, where the formation energy of nucleation should be higher than the nc surface in the intrinsic materials. If the deposition technology that can make highly doped and simultaneously highly crystallized nc at low temperature, it can lead processes of next generation flexible devices. Recently, we are developing a novel CVD technology with a neutral particle beam (NPB) source, named as neutral beam assisted CVD (NBaCVD), which controls the energy of incident neutral particles in the range of 1~300eV in order to enhance the atomic activation and crystalline of thin films at low temperatures. During the formation of the nc-/pm-Si thin films by the NBaCVD with various process conditions, NPB energy directly controlled by the reflector bias and effectively increased crystal fraction (~80%) by uniformly distributed nc grains with 3~10 nm size. In the case of phosphorous doped Si thin films, the doping efficiency also increased as increasing the reflector bias (i.e. increasing NPB energy). At 330V of reflector bias, activation energy of the doped nc-Si thin film reduced as low as 0.001 eV. This means dopants are fully occupied as substitutional site, even though the Si thin film has nano-sized grain structure. And activated dopant concentration is recorded as high as up to 1020 #/$cm^3$ at very low process temperature (< $80^{\circ}C$) process without any post annealing. Theoretical solubility for the higher dopant concentration in Si thin film for order of 1020 #/$cm^3$ can be done only high temperature process or post annealing over $650^{\circ}C$. In general, as decreasing the grain size, the dopant binding energy increases as ratio of 1 of diameter of grain and the dopant hardly be activated. The highly doped nc-Si thin film by low-temperature NBaCVD process had smaller average grain size under 10 nm (measured by GIWAXS, GISAXS and TEM analysis), but achieved very higher activation of phosphorous dopant; NB energy sufficiently transports its energy to doping and crystallization even though without supplying additional thermal energy. TEM image shows that incubation layer does not formed between nc-Si film and SiO2 under later and highly crystallized nc-Si film is constructed with uniformly distributed nano-grains in polymorphous tissues. The nucleation should be start at the first layer on the SiO2 later, but it hardly growth to be cone-shaped micro-size grains. The nc-grain evenly embedded pm-Si thin film can be formatted by competition of the nucleation and the crystal growing, which depend on the NPB energies. In the evaluation of the light soaking degradation of photoconductivity, while conventional intrinsic and n-type doped a-Si thin films appeared typical degradation of photoconductivity, all of the nc-Si thin films processed by the NBaCVD show only a few % of degradation of it. From FTIR and RAMAN spectra, the energetic hydrogen NB atoms passivate nano-grain boundaries during the NBaCVD process because of the high diffusivity and chemical potential of hydrogen atoms.

  • PDF

PROCESSING OF DRILL SOLUBLE AND ITS AMINO ACID COMPOSITION (Krill solube의 가공 및 아미노산 조성)

  • LEE Eung-Ho;KIM Se-Kwon;CHO Duck-Jae;HAN Bong-Ho
    • Korean Journal of Fisheries and Aquatic Sciences
    • /
    • v.12 no.4
    • /
    • pp.235-240
    • /
    • 1979
  • A study on the amino acid composition of raw frozen krill, and krill solubles manufactured in forms of paste and powder has been carried out. The raw frozen krill was thawed, chopped, mixed and homogenized with same amount of water. The mixture was autolyzed or hydrolyzed by tile addition of $0.2\%$ pronase-p, a commercial proteolytic enzyme, to the weight of the raw frozen krill at $45^{\circ}C$ for 4 hours. After a thermal inactivation of enzymes at $95^{\circ}C$ for 15 minutes, the autolysate and the hydrolysate were centrifuged and filtered through gauzes, respectively, and then tile lipid layer in the supernatant was removed, The autolysate and the hydrolysate were finally concentrated under reduced atmospheric pressure in a rotary vacuum evaporator at $45^{\circ}C$ for 1 hour to produce the krill solubles in form of paste. The powdered krill solubles were prepared by the addition of $5\%$ starch to the autolysate and hydrolysate and by means of concentration in the rotary vacuum evaporator at $45^{\circ}C$ for 30 minutes and a forced air drying at $58^{\circ}C$ for 3 hours with a air velocity of 3m/sec. Among the amino acids in raw frozen krill, glutamic acid, lysine, and aspartic acid showed high values in quantity and then followed leucine, alanine, arginine, glycine and proline. The qnantity of histidine was very small and that of cystine was only in trace. The krill solubles in forms of paste and powder prepared by autolysis and hydrolysis with pronase-p revealed almost the same patterns in amino acid composition as in raw frozen krill. In case of free amino acids, a large quantity of it in raw frozen krill consisted of lysine, arginine, proline, alanine and leucine. The quantities of cystine, histidine and glutamic acid were, in contrast, very small. In the soluble krill paste prepared by autolysis, lysine, leucine, threonine and alanine existed in large quantities among the free amino acids and cystine, aspartic acid and histidine existed in small quantities. The contents of almost all of the free amino acids ill soluble krill paste perpared by hydrolysis with pronase-p were increased slightly as compared with those in soluble krill paste prepared by autolysis. In this product, the contents of cystine, histidine and serine were very low and lysine, leucine, arginine and proline were the dominant group in quantities among the free amino acids. The krill solubles in forms of paste and powder were not inferior to whole egg in the view point of its essential amino acid composition.

  • PDF

New Approaches for Overcoming Current Issues of Plasma Sputtering Process During Organic-electronics Device Fabrication: Plasma Damage Free and Room Temperature Process for High Quality Metal Oxide Thin Film

  • Hong, Mun-Pyo
    • Proceedings of the Korean Vacuum Society Conference
    • /
    • 2012.02a
    • /
    • pp.100-101
    • /
    • 2012
  • The plasma damage free and room temperature processedthin film deposition technology is essential for realization of various next generation organic microelectronic devices such as flexible AMOLED display, flexible OLED lighting, and organic photovoltaic cells because characteristics of fragile organic materials in the plasma process and low glass transition temperatures (Tg) of polymer substrate. In case of directly deposition of metal oxide thin films (including transparent conductive oxide (TCO) and amorphous oxide semiconductor (AOS)) on the organic layers, plasma damages against to the organic materials is fatal. This damage is believed to be originated mainly from high energy energetic particles during the sputtering process such as negative oxygen ions, reflected neutrals by reflection of plasma background gas at the target surface, sputtered atoms, bulk plasma ions, and secondary electrons. To solve this problem, we developed the NBAS (Neutral Beam Assisted Sputtering) process as a plasma damage free and room temperature processed sputtering technology. As a result, electro-optical properties of NBAS processed ITO thin film showed resistivity of $4.0{\times}10^{-4}{\Omega}{\cdot}m$ and high transmittance (>90% at 550 nm) with nano- crystalline structure at room temperature process. Furthermore, in the experiment result of directly deposition of TCO top anode on the inverted structure OLED cell, it is verified that NBAS TCO deposition process does not damages to the underlying organic layers. In case of deposition of transparent conductive oxide (TCO) thin film on the plastic polymer substrate, the room temperature processed sputtering coating of high quality TCO thin film is required. During the sputtering process with higher density plasma, the energetic particles contribute self supplying of activation & crystallization energy without any additional heating and post-annealing and forminga high quality TCO thin film. However, negative oxygen ions which generated from sputteringtarget surface by electron attachment are accelerated to high energy by induced cathode self-bias. Thus the high energy negative oxygen ions can lead to critical physical bombardment damages to forming oxide thin film and this effect does not recover in room temperature process without post thermal annealing. To salve the inherent limitation of plasma sputtering, we have been developed the Magnetic Field Shielded Sputtering (MFSS) process as the high quality oxide thin film deposition process at room temperature. The MFSS process is effectively eliminate or suppress the negative oxygen ions bombardment damage by the plasma limiter which composed permanent magnet array. As a result, electro-optical properties of MFSS processed ITO thin film (resistivity $3.9{\times}10^{-4}{\Omega}{\cdot}cm$, transmittance 95% at 550 nm) have approachedthose of a high temperature DC magnetron sputtering (DMS) ITO thin film were. Also, AOS (a-IGZO) TFTs fabricated by MFSS process without higher temperature post annealing showed very comparable electrical performance with those by DMS process with $400^{\circ}C$ post annealing. They are important to note that the bombardment of a negative oxygen ion which is accelerated by dc self-bias during rf sputtering could degrade the electrical performance of ITO electrodes and a-IGZO TFTs. Finally, we found that reduction of damage from the high energy negative oxygen ions bombardment drives improvement of crystalline structure in the ITO thin film and suppression of the sub-gab states in a-IGZO semiconductor thin film. For realization of organic flexible electronic devices based on plastic substrates, gas barrier coatings are required to prevent the permeation of water and oxygen because organic materials are highly susceptible to water and oxygen. In particular, high efficiency flexible AMOLEDs needs an extremely low water vapor transition rate (WVTR) of $1{\times}10^{-6}gm^{-2}day^{-1}$. The key factor in high quality inorganic gas barrier formation for achieving the very low WVTR required (under ${\sim}10^{-6}gm^{-2}day^{-1}$) is the suppression of nano-sized defect sites and gas diffusion pathways among the grain boundaries. For formation of high quality single inorganic gas barrier layer, we developed high density nano-structured Al2O3 single gas barrier layer usinga NBAS process. The NBAS process can continuously change crystalline structures from an amorphous phase to a nano- crystalline phase with various grain sizes in a single inorganic thin film. As a result, the water vapor transmission rates (WVTR) of the NBAS processed $Al_2O_3$ gas barrier film have improved order of magnitude compared with that of conventional $Al_2O_3$ layers made by the RF magnetron sputteringprocess under the same sputtering conditions; the WVTR of the NBAS processed $Al_2O_3$ gas barrier film was about $5{\times}10^{-6}g/m^2/day$ by just single layer.

  • PDF

Property of Nickel Silicide with 60 nm and 20 nm Hydrogenated Amorphous Silicon Prepared by Low Temperature Process (60 nm 와 20 nm 두께의 수소화된 비정질 실리콘에 따른 저온 니켈실리사이드의 물성 변화)

  • Kim, Joung-Ryul;Park, Jong-Sung;Choi, Young-Youn;Song, Oh-Sung
    • Journal of the Korean Vacuum Society
    • /
    • v.17 no.6
    • /
    • pp.528-537
    • /
    • 2008
  • 60 nm and 20 nm thick hydrogenated amorphous silicon(a-Si:H) layers were deposited on 200 nm $SiO_2$/single-Si substrates by inductively coupled plasma chemical vapor deposition(ICP-CVD). Subsequently, 30 nm-Ni layers were deposited by an e-beam evaporator. Finally, 30 nm-Ni/(60 nm and 20 nm) a-Si:H/200 nm-$SiO_2$/single-Si structures were prepared. The prepared samples were annealed by rapid thermal annealing(RTA) from $200^{\circ}C$ to $500^{\circ}C$ in $50^{\circ}C$ increments for 40 sec. A four-point tester, high resolution X-ray diffraction(HRXRD), field emission scanning electron microscopy(FE-SEM), transmission electron microscopy(TEM), and scanning probe microscopy(SPM) were used to examine the sheet resistance, phase transformation, in-plane microstructure, cross-sectional microstructure, and surface roughness, respectively. The nickel silicide from the 60 nm a-Si:H substrate showed low sheet resistance from $400^{\circ}C$ which is compatible for low temperature processing. The nickel silicide from 20 nm a-Si:H substrate showed low resistance from $300^{\circ}C$. Through HRXRD analysis, the phase transformation occurred with silicidation temperature without a-Si:H layer thickness dependence. With the result of FE-SEM and TEM, the nickel silicides from 60 nm a-Si:H substrate showed the microstructure of 60 nm-thick silicide layers with the residual silicon regime, while the ones from 20 nm a-Si:H formed 20 nm-thick uniform silicide layers. In case of SPM, the RMS value of nickel silicide layers increased as the silicidation temperature increased. Especially, the nickel silicide from 20 nm a-Si:H substrate showed the lowest RMS value of 0.75 at $300^{\circ}C$.

Effects of High Temperature Sterilization on Qualities Characteristics of the Canned Boiled Oyster (가열살균처리가 굴 보일드통조림의 품질특성에 미치는 영향)

  • Kong, Chung-Sik;Yun, Jae-Ung;Oh, Dong-Hun;Park, Jun-Yong;Kang, Jin-Yeong;Oh, Kwang-Soo
    • Journal of agriculture & life science
    • /
    • v.43 no.6
    • /
    • pp.85-93
    • /
    • 2009
  • The boiled oyster vacuum-packed in cylindrical can(No. 301-3) were thermally processed at $115^{\circ}C$ to reach Fo values of 5~20 min. The yield was slightly decreased with the increasing of Fo-values (79.2~ 83.7%), and volatile basic nitrogen (VBN) contents increased markedly with the increasing of Fo-value. In fatty acid composition of canned oyster, the composition ratio of saturates and monoenes such as 14:0, 16:0 and 18:1n9 increased, while polyunsaturated fatty acids such as 20:5n-3 and 22:6n-3 decreased with the increasing of Fo-value. In taste compounds, content of total free amino acid in raw oyster was 1,533.5 mg%, and this total content was slightly increased (1,140.8~1,266.2 mg%) with the increasing of Fo values. But contents of betaine and ionic minerals such as Na, K, Mg and P decreased markedly by thermal processing at $115^{\circ}C$. As compared with Fo 5 min. heat treatment; Fo 20 min. heat treatment at $115^{\circ}C$ became more hardened in texture of oyster meat. In sensory evaluations on organoleptic characteristics, no significant difference at 5% level was observed among the canned boiled oyster meats heated at Fo 5~15 min.

Background effect on the measurement of trace amount of uranium by thermal ionization mass spectrometry (열이온화 질량분석에 의한 극미량 우라늄 정량에 미치는 바탕값 영향)

  • Jeon, Young-Shin;Park, Yong-Joon;Joe, Kih-Soo;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
    • /
    • v.21 no.6
    • /
    • pp.487-494
    • /
    • 2008
  • An experiment was performed for zone refined Re-filament and normal (nonzone refined) Re-filament to reduce the background effect on the measurement of low level uranium samples. From both filaments, the signals which seemed to come from a cluster of light alkali elements, $(^{39}K_6)^+$, $(^{39}K_5+^{41}K)^+$ and $PbO_2$ were identified as the isobaric effect of the uranium isotopes. The isobaric effect signal was completely disappeared by heating the filament about $2000^{\circ}C$ at < $10^{-7}$ torr of vacuum for more than 1.5 hour in zone refined Refilaments, while that from the normal Re-filaments was not disappeared completely and was still remained as 3 pg. of uranium as the impurities after the degassing treatment was performed for more than 5 hours at the same condition of zone refined filaments. A threshold condition eliminating impurities were proved to be at 5 A and 30 minutes of degassing time. The uranium content as an impurity in rhenium filament was checked with a filament degassing treatment using the U-233 spike by isotope dilution mass spectrometry. A 0.31 ng of U was detected in rhenium filament without degassing, while only 3 pg of U was detected with baking treatment at a current of 5.5 A for 1 hr. Using normal Re-filaments for the ultra trace of uranium sample analysis had something problem because uranium remains to be 3 pg on the filament even though degassed for long hours. If the 1 ng uranium were measured, 0.3% error occurred basically. It was also conformed that ionization filament current was recommended not to be increased over 5.5 A to reduce the background. Finally, the contents of uranium isotopes in uranium standard materials (KRISS standard material and NIST standard materials, U-005 and U-030) were measured and compared with certified values. The differences between them showed 0.04% for U-235, 2% for U-234 and 2% for U-236, respectively.

Effect of Package Size and Pasteurization Temperature on the Quality of Sous Vide Processed Spinach (Sous Vide 가공 시금치의 품질에 미치는 포장단위 및 살균온도의 영향)

  • 장재덕;김기태;이동선
    • Food Science and Preservation
    • /
    • v.11 no.2
    • /
    • pp.195-200
    • /
    • 2004
  • Microbial lethal value and nutrient retention of sous vide processed spinach were evaluated with mathematical model prediction and experimental trial for different package sizes and pasteurization temperatures. The package size covers 500 g, 1 kg and 2 kg, while the pasteurization temperature includes 80, 90 and 97$^{\circ}C$. The basic process scheme consists of filling blanched spinach into barrier plastic film pouch, sealing under vacuum, pasteurization in hot water with over pressure and final cooling to 3$^{\circ}C$. Pasteurization condition was designed based on attainment of 6 decimal inactivation of Listeria monocytogenes at geometric center of the pouch package by heating cycle, which was determined by general method. Heat penetration property of the package and thermal destruction kinetics were combined to estimate the retention of ascorbic acid and chlorophyll. Smaller packages with shorter pasteurization time gave better nutrient retention, physical and chemical qualities. Larger package size was estimated and confirmed experimentally to give higher pasteurization value at center, lower ascorbic acid and chlorophyll contents caused by longer heat process time. Lower pasteurization temperature with longer process time was predicted to give lower pasteurization value at center and lower ascorbic acid, while chlorophyll content was affected little by the temperature. Experimental trial showed better retention of ascorbic acid and chlorophyll for smaller package and higher pasteurization temperature with shorter heating time. The beneficial effect of smaller package and higher pasteurization temperature was also observed in texture, color retention and drip production.