• Title/Summary/Keyword: Freeze-drying process

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Synthesis of Porous Cu-Sn by Freeze Drying and Hydrogen Reduction Treatment of Metal Oxide Composite Powders (금속산화물 복합분말의 동결건조 및 수소분위기 환원처리에 의한 Cu-Sn 다공체 제조)

  • Kim, Min-Sung;Yoo, Ho-Suk;Oh, Sung-Tag;Hyun, Chang-Yong
    • Korean Journal of Materials Research
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    • v.23 no.12
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    • pp.722-726
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    • 2013
  • Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-$SnO_2$ and camphene. Camphene slurries with CuO-$SnO_2$ content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at $50^{\circ}C$. Freezing of a slurry was done at $-25^{\circ}C$ while the growth direction of the camphene was unidirectionally controlled. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies were hydrogen-reduced at $650^{\circ}C$ and then were sintered at $650^{\circ}C$ and $750^{\circ}C$ for 1 h. XRD analysis revealed that the CuO-$SnO_2$ powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above $100{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-$SnO_2$ content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from $650^{\circ}C$ to $750^{\circ}C$, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.

Fabrication of Al2O3 Dispersed Porous Cu by Freeze Drying of CuO-Al2O3/Camphene Slurry (CuO-Al2O3/camphene 슬러리의 동결건조 공정에 의한 Al2O3 입자분산 Cu 다공체 제조)

  • Kang, Hyunji;Riu, Doh-Hyung;Oh, Sung-Tag
    • Journal of Powder Materials
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    • v.25 no.1
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    • pp.25-29
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    • 2018
  • Porous Cu with a dispersion of nanoscale $Al_2O_3$ particles is fabricated by freeze-drying $CuO-Al_2O_3$/camphene slurry and sintering. Camphene slurries with $CuO-Al_2O_3$ contents of 5 and 10 vol% are unidirectionally frozen at $-30^{\circ}C$, and pores are generated in the frozen specimens by camphene sublimation during air drying. The green bodies are sintered for 1 h at $700^{\circ}C$ and $800^{\circ}C$ in $H_2$ atmosphere. The sintered samples show large pores of $100{\mu}m$ in average size aligned parallel to the camphene growth direction. The internal walls of the large pores feature relatively small pores of ${\sim}10{\mu}m$ in size. The size of the large pores decreases with increasing $CuO-Al_2O_3$ content by the changing degree of powder rearrangement in the slurry. The size of the small pores decreases with increasing sintering temperature. Microstructural analysis reveals that 100-nm $Al_2O_3$ particles are homogeneously dispersed in the Cu matrix. These results suggest that a porous composite body with aligned large pores could be fabricated by a freeze-drying and $H_2$ reducing process.

Processing and Quality properties of Chestnut Paste (밤페이스트의 제조와 품질 특성)

  • 문광덕;서영호;김준한;임정호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.3
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    • pp.572-578
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    • 1999
  • This study was conducted to investigate processing condition and characteristics of chestnut paste. The kinds of chestnut powder processed with blanching and drying of raw material were four named RH(not blanched, hot air dried), RF(not blanched, freeze dried), BH(blanched, hot air dried) and BF(blanched, freeze dried). Blanching affected the reduction of drying time in chestnut. Water absorption index of the blanched samples were higher than the nonblanched. Blanching affected the viscosity of pastes when water was added to process paste also, but drying methods did not affected to it. The proper ratio of water to the powder to process paste was 1.3 to 1.5 times in RH and RF, whereas 2.7 times in BH and BF by sensory evaluation. Soluble tannin content of paste was higher in RF and RH paste than BF and BH. Vitamin C content was the highest(88.49mg/100g) in RF paste and reducing sugar content was the highest in RF paste. Hunter's L and a values were the highest in BF and RH pastes, respectively, among the all paste samples. Volatile compounds detected from chestnutpastes were hydrocarbons, alcohols, phenols, ketones. The major volatile compound in all the pastes was 2,6 bis(1,1 dimethylethyl) 4 methyl phenol.

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Characteristics and Drug Release Profiles of Multilamellar Vesicle(MLV) and Microemulsified Liposome(MEL) Entrapped 5-Fluorouracil and Its derivatives (5-Fluorouracil과 그 유도체를 봉입한 Multilamellar Vesicle(MLV)과 Microemulsified Liposome(MEL)의 특성 및 약물방출 거동)

  • Jee, Ung-Kil;Park, Mok-Soon;Lee, Gye-Won;Lyu, Yeon-Geun
    • Journal of Pharmaceutical Investigation
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    • v.25 no.3
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    • pp.249-264
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    • 1995
  • Although liposome has many advantages as a pharmaceutical dosage form, its application in the industrial field has been limited because of some problems such as preparation method, reproducibility, scale-up, stability and sterilization etc. Liposomes prepared by microemulsification method had defined size, narrow size distribution, reproducibility and high entrapment efficiency. For enhancing the stability, the dry form of liposome was recommended. These types of liposome are proliposome and freeze-dried liposome. The liposome must have some properties for preparing of freeze-dried liposome; small size $(50{\sim}200\;nm)$, narrow size distribution and cryoprotectant. In this experiment, the liposomes containing 5-Fluorouracil(5-FU) and its prodrug(pentyl-5-FU-1-acetate; PFA, hexyl-5-FU-1-acetate; HFA) were made with soybean phosphatidylcholine, cholesterol, stearylamine(SA) and dicetyl phosphate(DCP) employing hydration method or microemulsification method using $Microfluidizer^{TM}$. Both or liposome types were MLV and MEL. After preparation, freeze drying and rehydration were performed. In the process of freezing, trehalose(Tr) was added as a cryoprotectant. Their evaluation methods were as follows; entrapment efficiency, mean particle size and size distribution, dissolution test, retain of entrapment efficiency and turbidity after freeze-drying. The results are summarized as belows. The entrapment efficiency of 5-FU was dependent on total lipid concentration and cholesterol content but that of PFA and HFA was decreased when cholesterol was added. When DCP and SA were added, entrapment efficiency was decreased. As the partition coefficient of drug was increased, entrapment efficiency was increased. Under the same condition, entrapment efficiency of MEL is similar to that of MLV. The mean particle size and size distribution of MEL were smaller than those of MLV. Dissolution rates of drug from both liposome types were comparatively similar. Dissolution rates of drugs with serum and liver homogenate were faster than without these material. After preparation of liposome, free drug was removed efficiency by Dowex 50W-X4. When liposome was freeze-dried and then rehydrated in the presence of Tr, characteristics of liposome were maintained well in MEL than MLV. Tr Was used successfully as a cryoprotectant in the process of freeze drying and the optimal ratio of Tr:Lipid was 4:1(g/g).

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Analysis of Characteristics and Aroma Pattern of Powdered Chungkookjang from Hot-Air and Freeze Drying (열풍 및 동결 건조 분말 청국장의 특성 및 향기 패턴 분석)

  • Lee, Hyo-Suk;Nam, Ha-Young;Lee, Ki-Teak
    • Journal of the East Asian Society of Dietary Life
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    • v.16 no.6
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    • pp.724-730
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    • 2006
  • Two types of powdered chungkookjang, were prepared by a hot air-drying process, and the freeze-drying, and composition and aroma patterns were examined. The fresh chungkookjang was composed of 53.8% moisture, while the hot air-dried and freeze-dried powdered chungkookjang contained 5.2% moisture, $39.3{\sim}39.4%$ crude protein, $18.6{\sim}18.7%$ crude lipid, $4.7{\sim}5.0%$ crude ash, and $31.7{\sim}32.2%$ carbohydrate. The pH of the each powered chungkookjang was similar, ranging from 6.5 to 6.7. The freeze-dried powdered chungkookjang showed the highest lightness (67.30), yellowness (59.37) while the highest redness (43.1) was observed in the hot air-dried chungkookjang. Each chungkookjang was analysed by an electronic nose with metal oxide 12 sensors and SPME-GC/MS. The response by the electronic nose was analysed by principal component analysis (PCA). The proportion of the first principal component was 90.47%, suggesting that each aroma pattern of the prepared chungkookjang was discriminated. SPME-GC/MS was used to identify the pyrazines. The percentage of pyrazines observed in the fresh chungkookjang, freeze-dried powdered chungkookjang, and hot air-dried powdered chungkookjang was 6.6, 3.8 and 15.9%, respectively. A higher overall preference was obtained from the hot air-dried powdered chungkookjang than with the freeze-dried powdered chungkookjang.

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A Study on the Cyclic Pressure Function in Freeze Drying of Foodstuff (식품의 냉동 건조에서 주기 압력 함수에 대한 연구)

  • Mun, Jae-Choel;Kim, Soo-Ho;Hwang, Kap-Sung;Hong, Song-Sun
    • Applied Chemistry for Engineering
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    • v.8 no.1
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    • pp.1-7
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    • 1997
  • We show that the usage of the cyclic pressure function in the freeze drying is more effective than the drying rate of the constant pressure process. The ultimate object of this process is to reduce energy costs by shortening the drying time. In this work, the concept of cyclic pressure function to decrease the drying time and the effects of the following factors on drying rate are considered ; pulse type, size in amplitude of pressure, size of intermediate time. Temperature for drying has always been maintained constantly at $20^{\circ}C$ and the pulse type could have found to give useful results than the constant pressure by altering chamber pressure from low pressure to high pressure Also, when the amplitude of the pulse is 0.4 torr and the intermediate time is six hour the drying rate was increased considerably.

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Mathematical Relationship between Ice Dendrite Size and Freezing Conditions in Tuna

  • Choi, Mi-Jung;Hong, Geun-Pyo;In, Dae-Sik;Min, Sang-Gi
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.330-335
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    • 2009
  • The principal objective of this study was to investigate changes in ice dendrite size during the freezing of tuna, in order to formulate a mathematical model of ice dendrite size. The tuna was frozen via a uni-directional heat transfer. Thermogram analysis allowed us to determine the position of the freezing front versus time, which is referred to as the freezing front rate. The morphology of the ice dendrites was assessed via scanning electron microscopy after freeze-drying, and the retained pore size was measured as ice dendrites. We noted that the mean size of ice dendrites increased with the distance to the cooling plate; however, it decreased with reductions in the cooling rate and the cooling temperature. In addition, shorter durations of the freeze-drying process decreased the freezing front rate, resulting in a larger size of the ice dendrite pores that operate as water vapor sublimation channels. According to our results, we could derive a linear regression as an empirical mathematical model equation between the ice dendrite size and the inverse of the freezing front rate.

Freeze Drying Process and Pore Structure Characteristics of Porous Cu with Various Sublimable Vehicles (다양한 동결제를 이용하여 동결건조 공정으로 제조한 Cu 다공체의 기공구조 특성)

  • Lee, Gyuhwi;Oh, Sung-Tag;Suk, Myung-Jin;Jeong, Young-Keun
    • Journal of Powder Materials
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    • v.27 no.3
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    • pp.198-202
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    • 2020
  • The effect of sublimable vehicles on the pore structure of Cu fabricated by freeze drying is investigated. The 5 vol% CuO-dispersed slurries with camphene and various camphor-naphthalene compositions are frozen in a Teflon mold at -25℃, followed by sublimation at room temperature. After hydrogen reduction at 300℃ and sintering at 600 ℃, the green bodies of CuO are completely converted to Cu with various pore structures. The sintered samples prepared using CuO/camphene slurries show large pores that are aligned parallel to the sublimable vehicle growth direction. In addition, a dense microstructure is observed in the bottom section of the specimen where the solidification heat was released, owing to the difference in the solidification behavior of the camphene crystals. The porous Cu shows different pore structures, such as dendritic, rod-like, and plate shaped, depending on the composition of the camphornaphthalene system. The change in pore structure is explained by the crystal growth behavior of primary camphor and eutectic and primary naphthalene.

Freeze drying of a Wooden Comb Excavated at Shinchang-dong Wetland Site with Cetylalcohol (세틸알콜을 이용한 광주 신창동 저습지 출토 목제 빗의 동결건조)

  • Park, Youngman
    • Conservation Science in Museum
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    • v.11
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    • pp.49-52
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    • 2010
  • A wooden Comb excavated at Shinchang-dong wetland site was treated with cetylalcohol as a reinforcing agent. The conservation process was done by freeze drying the wooden artifact after substituting it with no.3 butyl alcohol and impregnating with 40wt% cetylalcohol solution. Consequently there was no noticeable surface damage. Also it showed 54% of remaining weight and a shrinkage of length 3.3%, width 2.1% and thickness 3.1%. Therefore using cetylalcohol for conservation of waterlogged archeological wood was effective dimensional stability and remaining weight.

Fabrication of Porous Mo by Freeze-Drying and Hydrogen Reduction of MoO3/Camphene Slurry (MoO3/camphene 슬러리의 동결건조 및 수소환원에 의한 Mo 다공체 제조)

  • Lee, Wonsuk;Oh, Sung-Tag
    • Journal of Powder Materials
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    • v.19 no.6
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    • pp.446-450
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    • 2012
  • In order to fabricate the porous Mo with controlled pore characteristics, unique processing by using $MoO_3$ powder as the source and camphene as the sublimable material is introduced. Camphene-based 15 vol% $MoO_3$ slurries, prepared by milling at $50^{\circ}C$ with a small amount of dispersant, were frozen at $-25^{\circ}C$. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green body was hydrogen-reduced at $750^{\circ}C$, and sintered at $1000-1100^{\circ}C$ for 1 h. After heat treatment in hydrogen atmosphere, $MoO_3$ powders were completely converted to metallic W without any reaction phases. The sintered samples showed large pores with the size of about $150{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal wall of large pores and near bottom part of specimen had relatively small pores due to the difference in the camphene growth rate during freezing process. The size of small pores was decreased with increase in sintering temperature, while that of large pores was unchanged. The results are strongly suggested that the porous metal with required pore characteristics can be successfully fabricated by freeze-drying process using metal oxide powders.