KR101733165B1 - 고온 소결형 도전성 페이스트용 은 분말의 제조방법 - Google Patents
고온 소결형 도전성 페이스트용 은 분말의 제조방법 Download PDFInfo
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- KR101733165B1 KR101733165B1 KR1020150113932A KR20150113932A KR101733165B1 KR 101733165 B1 KR101733165 B1 KR 101733165B1 KR 1020150113932 A KR1020150113932 A KR 1020150113932A KR 20150113932 A KR20150113932 A KR 20150113932A KR 101733165 B1 KR101733165 B1 KR 101733165B1
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- Prior art keywords
- reaction solution
- silver
- solution
- silver powder
- parts
- Prior art date
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000005245 sintering Methods 0.000 title description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052709 silver Inorganic materials 0.000 claims abstract description 35
- 239000004332 silver Substances 0.000 claims abstract description 35
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 29
- -1 silver halide Chemical class 0.000 claims abstract description 29
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 17
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 32
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 239000002738 chelating agent Substances 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 239000000843 powder Substances 0.000 abstract description 10
- 239000000243 solution Substances 0.000 description 98
- 239000011259 mixed solution Substances 0.000 description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 24
- 229910001961 silver nitrate Inorganic materials 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 9
- 101710134784 Agnoprotein Proteins 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000005416 organic matter Substances 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000011231 conductive filler Substances 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000010946 fine silver Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007573 shrinkage measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- B22F1/0007—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020150113932A KR101733165B1 (ko) | 2015-08-12 | 2015-08-12 | 고온 소결형 도전성 페이스트용 은 분말의 제조방법 |
JP2018527702A JP2018523758A (ja) | 2015-08-12 | 2016-08-01 | 高温焼結型導電性ペースト用銀粉末の製造方法 |
CN201680047257.XA CN107921543A (zh) | 2015-08-12 | 2016-08-01 | 高温烧结型导电性浆料用银粉末的制造方法 |
PCT/KR2016/008474 WO2017026722A1 (ko) | 2015-08-12 | 2016-08-01 | 고온 소결형 도전성 페이스트용 은 분말의 제조방법 |
Applications Claiming Priority (1)
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KR1020150113932A KR101733165B1 (ko) | 2015-08-12 | 2015-08-12 | 고온 소결형 도전성 페이스트용 은 분말의 제조방법 |
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Publication Number | Publication Date |
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KR20170019727A KR20170019727A (ko) | 2017-02-22 |
KR101733165B1 true KR101733165B1 (ko) | 2017-05-08 |
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KR1020150113932A KR101733165B1 (ko) | 2015-08-12 | 2015-08-12 | 고온 소결형 도전성 페이스트용 은 분말의 제조방법 |
Country Status (4)
Country | Link |
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JP (1) | JP2018523758A (ja) |
KR (1) | KR101733165B1 (ja) |
CN (1) | CN107921543A (ja) |
WO (1) | WO2017026722A1 (ja) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR102007856B1 (ko) * | 2017-10-13 | 2019-08-06 | 엘에스니꼬동제련 주식회사 | 분산성이 개선된 은 분말의 제조방법 |
KR102061719B1 (ko) * | 2017-10-30 | 2020-01-02 | 엘에스니꼬동제련 주식회사 | 은 분말 및 이의 제조방법 |
KR102061718B1 (ko) * | 2017-10-30 | 2020-01-02 | 엘에스니꼬동제련 주식회사 | 표면 처리된 은 분말 및 이의 제조방법 |
KR102122317B1 (ko) * | 2017-10-31 | 2020-06-12 | 엘에스니꼬동제련 주식회사 | 은 분말의 제조방법 및 은 분말을 포함하는 도전성 페이스트 |
KR102081183B1 (ko) * | 2017-10-31 | 2020-02-25 | 엘에스니꼬동제련 주식회사 | 은 분말의 제조방법 |
KR102061720B1 (ko) * | 2017-10-31 | 2020-01-02 | 엘에스니꼬동제련 주식회사 | 표면 처리된 은 분말 및 이의 제조방법 |
JP6857166B2 (ja) * | 2017-12-15 | 2021-04-14 | Dowaエレクトロニクス株式会社 | 球状銀粉およびその製造方法 |
KR101953619B1 (ko) * | 2018-05-08 | 2019-03-05 | 대주전자재료 주식회사 | 방사형 중공형 은 입자를 포함하는 은 분말 및 이의 제조방법 |
CN108941609A (zh) * | 2018-09-10 | 2018-12-07 | 河南金渠银通金属材料有限公司 | 太阳能电池导电银浆用高性能球形超细银粉及其制备方法 |
KR102178009B1 (ko) * | 2018-11-30 | 2020-11-12 | 엘에스니꼬동제련 주식회사 | 수축률 조절이 가능한 은 분말의 제조방법 |
KR102197542B1 (ko) * | 2018-11-30 | 2020-12-31 | 엘에스니꼬동제련 주식회사 | 세척 특성이 개선된 은 분말의 제조방법 |
CN109637693A (zh) * | 2018-12-17 | 2019-04-16 | 中国计量大学 | 一种基于自烧结银框架的导电银浆及其制备方法 |
KR102454264B1 (ko) * | 2020-03-25 | 2022-10-14 | 엘에스니꼬동제련 주식회사 | 점도 안정성이 향상된 전도성 페이스트용 은 분말 및 이의 제조방법 |
CN115464147A (zh) * | 2022-09-16 | 2022-12-13 | 北京曙光航空电气有限责任公司 | 一种银粉制造方法 |
Citations (2)
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JP2007270312A (ja) * | 2006-03-31 | 2007-10-18 | Mitsui Mining & Smelting Co Ltd | 銀粉の製造方法及び銀粉 |
JP2010070793A (ja) * | 2008-09-17 | 2010-04-02 | Dowa Electronics Materials Co Ltd | 球状銀粉およびその製造方法 |
Family Cites Families (11)
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---|---|---|---|---|
JP2001107101A (ja) * | 1999-10-12 | 2001-04-17 | Mitsui Mining & Smelting Co Ltd | 高分散性球状銀粉末及びその製造方法 |
JP4489389B2 (ja) * | 2003-07-29 | 2010-06-23 | 三井金属鉱業株式会社 | 微粒銀粉の製造方法 |
JP4976642B2 (ja) * | 2004-02-10 | 2012-07-18 | 三井金属鉱業株式会社 | 高結晶性銀粉及びその製造方法 |
KR101061841B1 (ko) * | 2009-01-13 | 2011-09-05 | 충남대학교산학협력단 | 화학환원법에 의한 단분산 구형 은 분말의 제조방법 |
TW201043359A (en) * | 2009-05-01 | 2010-12-16 | Du Pont | Silver particles and a process for making them |
TW201100185A (en) * | 2009-05-01 | 2011-01-01 | Du Pont | Silver particles and a process for making them |
JP5354041B2 (ja) * | 2012-02-24 | 2013-11-27 | 住友金属鉱山株式会社 | 銀粉の製造方法 |
JP5763869B2 (ja) * | 2013-06-25 | 2015-08-12 | 化研テック株式会社 | 薄片状銀粉、導電性ペースト、および薄片状銀粉の製造方法 |
CN103724805A (zh) * | 2013-12-18 | 2014-04-16 | 芜湖万润机械有限责任公司 | 一种综合性能优良的电容器用金属化薄膜及其制备方法 |
CN104376900A (zh) * | 2014-11-18 | 2015-02-25 | 苏州东辰林达检测技术有限公司 | 一种透明导电薄膜及其制备方法 |
CN104599737B (zh) * | 2014-12-17 | 2017-01-04 | 华南理工大学 | 一种微纳米银/高分子导电复合材料及其制备方法与应用 |
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2015
- 2015-08-12 KR KR1020150113932A patent/KR101733165B1/ko active IP Right Grant
-
2016
- 2016-08-01 JP JP2018527702A patent/JP2018523758A/ja active Pending
- 2016-08-01 CN CN201680047257.XA patent/CN107921543A/zh active Pending
- 2016-08-01 WO PCT/KR2016/008474 patent/WO2017026722A1/ko active Application Filing
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2007270312A (ja) * | 2006-03-31 | 2007-10-18 | Mitsui Mining & Smelting Co Ltd | 銀粉の製造方法及び銀粉 |
JP2010070793A (ja) * | 2008-09-17 | 2010-04-02 | Dowa Electronics Materials Co Ltd | 球状銀粉およびその製造方法 |
Also Published As
Publication number | Publication date |
---|---|
JP2018523758A (ja) | 2018-08-23 |
WO2017026722A1 (ko) | 2017-02-16 |
KR20170019727A (ko) | 2017-02-22 |
CN107921543A (zh) | 2018-04-17 |
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