CN1781630A - 银粉及其制造方法 - Google Patents
银粉及其制造方法 Download PDFInfo
- Publication number
- CN1781630A CN1781630A CNA2005101287156A CN200510128715A CN1781630A CN 1781630 A CN1781630 A CN 1781630A CN A2005101287156 A CNA2005101287156 A CN A2005101287156A CN 200510128715 A CN200510128715 A CN 200510128715A CN 1781630 A CN1781630 A CN 1781630A
- Authority
- CN
- China
- Prior art keywords
- silver powder
- silver
- acid
- powder
- reaction system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims description 33
- 238000001354 calcination Methods 0.000 claims description 22
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 12
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 11
- 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 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 6
- 125000001931 aliphatic group Chemical group 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
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- 239000004094 surface-active agent Substances 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 4
- 239000000138 intercalating agent Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000000344 soap Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 abstract description 16
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- 239000004020 conductor Substances 0.000 description 12
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- 230000000052 comparative effect Effects 0.000 description 8
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
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- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
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- KJUGUADJHNHALS-UHFFFAOYSA-N 1H-tetrazole Chemical compound C=1N=NNN=1 KJUGUADJHNHALS-UHFFFAOYSA-N 0.000 description 2
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
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Abstract
在含银离子的水反应体系中加入还原剂,还原沉积出银颗粒后,干燥银颗粒获得银粉,该银粉在高于100℃但低于400℃温度进行热处理。热处理后的银粉在50-800℃的最大热膨胀系数不大于1.5%,且银粉由50℃加热至800℃时没有加热峰。所述银粉被灼烧直到在800℃银粉重量恒定时的银粉灼烧损失不大于1.0%。银粉的堆密度不小于2g/cm3,BET比表面积不大于5m2/g。
Description
技术领域
概括地说,本发明涉及银粉及其制造方法。更具体地说,本发明涉及用于电子部件,如多层电容器的内部电极、电路板印刷电路的银粉,及其制造方法。
背景技术
为形成混合集成电路的电极、多层电容器、芯片电阻等,一直使用金属陶瓷型导电糊剂(或待焙烧型的导电糊剂)。常规的金属陶瓷型糊剂包含银粉、含溶解在有机溶剂中的乙基纤维素或丙烯酸类树脂的载体、玻璃料、无机氧化物、有机溶剂、分散剂等组分。金属陶瓷型糊剂通过浸涂或印刷形成预定的图案,然后焙烧形成导体。作为制备这种导电糊剂用银粉的方法,已知的是湿还原法,它是在水反应体系中加入还原剂,该体系含有银离子,通过还原沉淀出银颗粒(例如,可参见日本专利公开公报8-176620)。
但是,某些情况下,用常规湿还原法制备的银粉含有还原时反应母液夹带的杂质。因此,如果使用含有这种银粉的糊剂来形成导体,某些情况下,由于气体组分等在焙烧时蒸发而使导体拱起和/或发生破裂。
发明内容
因此,本发明的一个目的是解决前述这些问题,并提供一种用来形成糊剂的银粉,该糊剂能焙烧形成没有拱起和破裂的导体,还提供了该种银粉的制备方法。
为了达到前述目的及其它目的,本发明者进行了深入研究,发现在含有银离子的水反应体系中加入还原剂,还原沉积出银颗粒,干燥后获得银粉,如果再将获得的银粉在高于100℃但低于400℃,较好在120-300℃,更好在150-250℃进行热处理,用来形成经过焙烧能形成导体的糊剂,则能够获得没有拱起和破裂部分的导体。因此,本发明者作出了本发明。
根据本发明的一个方面,提供了一种制造银粉的方法,该方法包括以下步骤:制备含银离子的水反应体系;将还原剂加入含有银离子的水反应体系中,还原沉积出银颗粒;干燥银颗粒,制得银粉;获得的银粉在高于100℃但低于400℃,较好在120-300℃,更好在150-250℃进行热处理。在所述制造银粉的方法中,在沉积银颗粒之前或之后,较好是在浆状反应体系中含有分散剂。所述分散剂宜为至少一种选自脂肪酸、脂肪酸盐、表面活性剂、有机金属、鳌合剂和保护胶体的分散剂。还原剂宜为至少一种选自抗坏血酸、链烷醇胺、氢醌、肼和甲醛水的还原剂。较好的是,还原剂的加入速率不小于相对于含银离子的水反应体系中银含量的1当量/分钟。
根据本发明的另一个方面,提供了在50-800℃范围其最大热膨胀系数不大于1.5%,较好不大于1.0%,更好不大于0.5%的银粉,该银粉被灼烧直到800℃时重量恒定的银粉灼烧损失不大于1.0%。该银粉较好在由50℃加热至800℃时没有加热峰。较好的是,银粉的堆密度不小于2g/cm3,BET比表面积不大于5m2/g。
根据本发明,可以制造用来形成糊剂的银粉,该糊剂能焙烧形成没有拱起和破裂部分的导体。
附图简要说明
图1所示是实施例1和比较例1的DTA曲线,表示加热值随温度的变化。
具体实施方式
在根据本发明制造银粉的方法的一个优选的实施方式中,还原剂加入含有银离子的水反应体系中,还原沉积出银颗粒之后,干燥银颗粒获得银粉,然后,将获得的银粉在在高于100℃但低于400℃,较好在120-300℃,更好在150-250℃进行热处理。如果不进行热处理,或热处理温度不高于100℃,银粉的热膨胀系数增大,使银粉有一个加热峰。如果将含这种银粉的糊剂用来形成导体,在焙烧期间引起气体组分等挥发,致使导体拱起和/或破裂。另一方面,如果加热温度不低于400℃,得到聚积的银粉,在制备糊剂等时会有薄片形成的问题。此外,热处理可以在大气中、真空中、或惰性气体如氮气或氩气的气氛中进行。要求根据热处理温度以及所需的银粉特性来控制热处理时间。
作为含银离子的水反应体系,可以使用含硝酸银、银盐络合物或银中间体的水溶液或浆料。银盐络合物可以通过加入氨水、铵盐、螯合化合物等形成。银中间体可以通过加入氢氧化钠、氯化钠、碳酸钠等来制备。其中,优选使用在硝酸银水溶液中加入氨酸获得的胺络合物,这样获得银粉具有适合的粒径,且为球形。由于胺络合物的配位数为2,对每摩尔银加入2摩尔或更多的氨。
还原剂选自下列物质:抗坏血酸、亚硫酸盐、链烷醇胺、含水过氧化氢、甲酸、甲酸铵、甲酸钠、乙二醛、酒石酸、次亚磷酸钠、氢硼化钠、肼、肼化合物、氢醌、焦棓酸、葡萄糖、五倍子酸盐、甲醛水、干燥的硫酸钠和雕白粉。其中,还原剂较好是选自下面的一种或多种物质:抗坏血酸、链烷醇胺、氢醌、肼和甲醛水。如果使用这些还原剂,可以获得适当粒径的银粉。
还原剂加入速率宜大于或等于1当量/分钟,为的是防止银粉聚积。虽然对此原因还不清楚,但可以认为,如果在短时间内加入还原剂,在短时间完全还原后立刻引起银颗粒还原沉积出来,这样就很难产生晶核的聚积,从而改善分散性。因此,加入还原剂的时间宜短。进行还原时,还宜搅拌进行反应的溶液,在短时间内完成反应。
为了进一步提高分散性,在沉积银颗粒之前或之后,在浆状反应体系中宜加入分散剂。分散剂较好是选自下列的一种或多种物质:脂肪酸、脂肪酸盐、表面活性剂、有机金属、鳌合剂和保护胶体。
脂肪酸的例子有:丙酸、辛酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山嵛酸、丙烯酸、油酸、亚油酸和花生四烯酸。
脂肪酸盐的例子是由脂肪酸和金属,如锂、钠、钾、钡、镁、钙、铝、铁、钴、锰、铅、锌、锡、锶、锆、银和铜形成的盐。
表面活性剂的例子有:阴离子表面活性剂,如烷基苯磺酸盐;两性表面活性剂如咪唑鎓甜菜碱;和非离子表面活性剂如聚氧乙烯烷基醚和聚氧乙烯脂肪酸酯。
有机金属的例子有:乙酰丙酮三丁醇锆、柠檬酸镁、二乙基锌、氧化二丁基锡、二甲基锌、四正丁醇锆、三乙基铟、三甲基镓、氧化单丁基锡、四异氰酸酯硅烷、四甲基硅烷、四甲氧基硅烷、聚甲氧基硅氧烷、三异氰酸单甲酯硅烷、硅烷偶联剂、钛酸盐偶联剂和铝偶联剂。
鳌合剂的例子有:咪唑、噁唑、噻唑、硒唑、吡唑、异噁唑、异噻唑、1H-1,2,3-三唑、2H-1,2,3-三唑、1H-1,2,4-三唑、4H-1,2,4-三唑、1,2,3-噁二唑、1,2,4-噁二唑、1,2,5-噁二唑、1,3,4-噁二唑、1,2,3-噻二唑、1,2,4-噻二唑、1,2,5-噻二唑、1,3,4-噻二唑、1H-1,2,3,4-四唑、1,2,3,4-噁三唑、1,2,3,4-噻三唑、2H-1,2,3,4-四唑、1,2,3,5-噁三唑、1,2,3,5-噻三唑、吲唑、苯并咪唑、苯并三唑、以及它们的盐,和草酸、琥珀酸、丙二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、双十二烷酸(didodecanoic acid)、马来酸、富马酸、邻苯二甲酸、间苯二甲酸和对苯二酸、乙醇酸、乳酸、羟基丁酸、甘油酸、酒石酸、苹果酸、丙醇二酸、羟基丙酸、扁桃酸、柠檬酸和抗坏血酸。
保护胶体的例子有:明胶、清蛋白、阿拉伯树胶、protarbic酸和卵清酸。
通过上述根据本发明制造银粉方法的优选实施方式,能够制备在50-800℃最大热膨胀系数不大于1.5%,较好不大于1.0%,更好不大于0.5%的银粉,该银粉灼烧到在800℃银粉重量恒定时的银粉灼烧损失不大于1.0%,银粉的堆密度不小于2g/cm3,BET比表面积不大于5m2/g。
如果用这种的银粉来形成经表示形成导体的糊剂,能减小导体由于挥发组分的挥发产生的膨胀,并且能够减少由于加热部件导致的突然加热,因此能够形成没有拱起和/或破裂部分的导体。如果银粉为球形,这种银粉适合用来进行光敏糊剂法。而如果银粉具有不规则的形状或者是片形,就会因为引起紫外线的不规则反射和/或散射,存在银粉的光敏特性不佳的缺点。然而,如果银粉为球形,这种银粉也适合用来进行印刷和转移法。此外,如果堆密度小于2g/cm3,会引起银粉颗粒强烈聚积,这样即使采用上述任何一种方法也难以形成精细线路。如果BET比表面积大于5m2/g,则糊剂的粘度太高,致使其加工性不佳。
下面,将详细地描述本发明的银粉及其制造方法。
实施例1
向3600ml含有12g/l硝酸银作为银离子的水溶液中加入180ml工业级氨水形成银氨络合物的水溶液。在该银氨络合物水溶液中加入1g氢氧化钠,控制溶液的pH。在5秒内,将192ml工业级甲醛水作为还原剂加到上述溶液中。然后,立刻在该溶液中加入0.1g硬脂酸,获得银浆料。然后,对获得的银浆料过滤,用水洗涤,干燥后获得银粉。再将获得的银粉在大气中,150℃热处理6小时。
测定该银粉的热膨胀系数、加热值、灼烧损失、BET比表面积和堆密度。此外,对含这种银粉的糊剂制备的烧结体减小评价。还用扫描电子显微镜(SEM)证实了在此实施例和下面描述的实施例以及比较例1和2中获得的银粉是银粉。
用热膨胀系数测定装置(DILATO METAER 5000,由MAC SCIENCE/BRUKERaxs制造),由下面表达式,根据银粉的片形(直径5mm)样品的高度变化获得热膨胀系数,所述样品是向模具中的银粉施加250kg/cm2压力,单轴向压制形成的,样品以10℃/分钟升温速度从50℃加热至800℃:
在T℃时热膨胀系数(%)=(LT-L50)/L50×100
式中,L50和LT分别是样品温度为50℃和T℃时银粉的片形样品的高度(mm)。
用加热值测定装置(TG-DTA 2000测定装置,由MAC SCIENCE/BRUKER axs制造),进行银粉加热值测定,具体是在一个盘子(氧化铝测量盘,由Rigaku Co.,Ltd制造)中放入20±1mg银粉样品,以10℃/分钟速度,在大气压(不通风)下将样品从50℃加热至800℃。此外,用20.0mg氧化铝作为标准样品,用该测定装置的软件进行分析,获得加热峰温度。
在一个陶瓷熔化罐中称取2g银粉样品(W1),灼烧30分钟,直到样品重量在800℃时恒定,将样品冷却,称出重量(W2)。然后,由下面表达式获得灼烧损失。
灼烧损失(%)=(W1-W2)/W1×100
按照下面方面评价烧结体。首先,将84重量份银粉、6重量份丙烯酸类树脂(BR-105,可从Mitsubisi Rayon Co.,Ltd.获得)、9重量份有机溶剂(二甘醇单乙醚乙酸酯(试剂))和1重量份PbO-B2O3-SiO2玻璃料用三辊磨捏合,制备糊剂。然后,用一个线宽150微米的丝网印刷板将该糊剂丝网印刷在一个坯料片上进行干燥,该坯料片含有B2O3-SiO2-Al2O3玻璃料和氧化铝粉。制备五个相同的丝网印刷片,将它们叠加,然后在加热条件下进行压制。之后,该压制成的片在800℃焙烧30分钟。观察其拱起和破裂部分,来评价获得的烧结体。
结果,250℃时的最大热膨胀系数为0.35%,图1上没有加热峰。灼烧损失为0.86%,BET比表面积为0.26m2/g,堆密度为4.0g/cm3。该烧结体没有拱起和破裂部分。此外,在图1中,坐标纵轴指示测定的样品和标准样品之间的温度差,表示为热电偶的电动势(μV)测出的加热值。
实施例2
按照和实施例1相同的方法获得银粉,不同之处是,在250℃热处理2小时。采用和实施例1相同的方法测定银粉的热膨胀系数、灼烧损失、加热值、BET比表面积和堆密度,并按照和实施例1相同的方法评价烧结体。
结果,170℃时的最大热膨胀系数为0.12%,没有出现加热峰。灼烧损失为0.53%,BET比表面积为0.22m2/g,堆密度为5.1g/cm3。烧结体没有拱起和破裂部分。
实施例3
向3600ml含有12g/l硝酸银作为银离子的水溶液中加入140ml工业级氨水形成银氨络合物的水溶液。在该银氨络合物水溶液中加入17ml含60%肼的水溶液作为还原剂。之后,立刻在该溶液中加入0.2g油酸作为分散剂,获得银浆料。然后,对获得的银浆料过滤,用水洗涤,干燥后获得银粉。再将获得的银粉在大气压下,150℃热处理6小时。
对上述获得的银粉,采用和实施例1相同的方法测定银粉的热膨胀系数、灼烧损失、加热值、BET比表面积和堆密度,并按照和实施例1相同的方法评价烧结体。
结果,160℃时的最大热膨胀系数为0.04%,没有出现加热峰。灼烧损失为0.21%,BET比表面积为0.89m2/g,堆密度为2.5g/cm3。烧结体没有拱起和破裂部分。
比较例1
按照和实施例1相同的方法获得银粉,不同之处是,不进行热处理。采用和实施例1相同的方法测定银粉的热膨胀系数、灼烧损失、加热值、BET比表面积和堆密度,并按照和实施例1相同的方法评价烧结体。
结果,灼烧损失为0.68%,BET比表面积为0.25m2/g,堆密度为5.4g/cm3。但是,290℃时的最大热膨胀系数达到4.7%,并且如图1所示,有一个217.4℃的加热峰。此外,烧结体有拱起和破裂部分。
比较例2
按照和实施例1相同的方法获得银粉,不同之处是,在100℃热处理20小时。采用和实施例1相同的方法测定银粉的热膨胀系数、灼烧损失、加热值、BET比表面积和堆密度,并按照和实施例1相同的方法评价烧结体。
结果,灼烧损失为0.67%,BET比表面积为0.27m2/g,堆密度为5.6g/cm3。但是,290℃时的最大热膨胀系数达到3.8%,并且有一个217.4℃的加热峰。此外,烧结体有拱起和破裂部分。
比较例3
按照和实施例1相同的方法获得银粉,不同之处是,在450℃热处理2小时。采用和实施例1相同的方法测定银粉的热膨胀系数、灼烧损失、加热值、BET比表面积和堆密度,并按照和实施例1相同的方法评价烧结体。
结果,150℃时的最大热膨胀系数为0.01%,没有加热峰。灼烧损失为0.13%,BET比表面积为0.06m2/g,堆密度为4.6g/cm3。但是,由于在用三辊磨捏合时产生大量薄片,未能对烧结体进行评价。
此外,SEM证实了该热处理后的银粉约为是一烧结体,因而不能确定银粉的形状。
表
最大热膨胀系数(%) | 加热峰温度(℃) | 灼烧损失(%) | 比表面积(m2/g) | 堆密度(g/cm3) | 银粉形状 | |
实施例1 | 0.35 | - | 0.86 | 0.26 | 4.0 | 球形 |
实施例2 | 0.12 | - | 0.53 | 0.22 | 4.1 | 球形 |
实施例3 | 0.04 | - | 0.21 | 0.89 | 2.5 | 球形 |
比较例1 | 4.7 | 218.4 | 0.68 | 0.25 | 5.4 | 球形 |
比较例2 | 3.8 | 217.4 | 0.67 | 0.27 | 5.6 | 球形 |
比较例3 | 0.01 | - | 0.13 | 0.06 | 4.6 | 烧结 |
Claims (8)
1.一种制造银粉的方法,所述方法包括以下步骤:
制备含银离子的水反应体系;
在所述含银离子的水反应体系中加入还原剂,以还原沉积出银颗粒;
干燥所述银颗粒,以产生银粉;并
在高于100℃但低于400℃的温度下,对所述银粉进行热处理。
2.如权利要求1所述的制造银粉的方法,其特征在于,在所述银颗粒沉积之前或之后,在浆状反应体系中加入分散剂。
3.如权利要求2所述的制造银粉的方法,其特征在于,所述分散剂选自下组中的至少一种:脂肪酸、脂肪酸盐、表面活性剂、有机金属、鳌合剂和保护胶体。
4.如权利要求1所述的制造银粉的方法,其特征在于,所述还原剂选自下组中的至少一种:抗坏血酸、链烷醇胺、氢醌、肼和甲醛水。
5.如权利要求1所述的制造银粉的方法,其特征在于,所述还原剂以不低于相对于所述含银离子的水反应体系中银含量的1当量/分钟的速率加入。
6.一种银粉,所述银粉在50-800℃的最大热膨胀系数不大于1.5%,且所述银粉在800℃灼烧直到银粉重量恒定时的银粉灼烧损失不大于1.0%。
7.如权利要求6所述的银粉,其特征在于,所述银粉由50℃加热至800℃时没有加热峰。
8.如权利要求6所述的银粉,其特征在于,所述银粉的堆密度不小于2g/cm3,且BET比表面积不大于5m2/g。
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Family Cites Families (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62280308A (ja) | 1986-05-30 | 1987-12-05 | Mitsui Mining & Smelting Co Ltd | 銀−パラジウム合金微粉末の製造方法 |
US5045141A (en) * | 1988-07-01 | 1991-09-03 | Amoco Corporation | Method of making solderable printed circuits formed without plating |
JPH04269403A (ja) | 1991-02-25 | 1992-09-25 | Nec Kagoshima Ltd | 導電性ペースト |
JPH05239502A (ja) * | 1992-02-28 | 1993-09-17 | Daido Steel Co Ltd | 金属フレークの処理方法 |
TW261554B (zh) * | 1992-10-05 | 1995-11-01 | Du Pont | |
JP4025839B2 (ja) * | 1996-09-12 | 2007-12-26 | Dowaエレクトロニクス株式会社 | 銀粉および銀粉の製造方法 |
JP4012960B2 (ja) * | 1996-09-12 | 2007-11-28 | Dowaエレクトロニクス株式会社 | 銀粉の製造方法 |
JPH10183209A (ja) * | 1996-12-25 | 1998-07-14 | Sumitomo Metal Mining Co Ltd | 鱗片状銀粉末の製造方法 |
JPH11177240A (ja) * | 1997-12-11 | 1999-07-02 | Taiyo Yuden Co Ltd | セラミック積層体の製造方法 |
JP3457879B2 (ja) * | 1998-02-25 | 2003-10-20 | 石福金属興業株式会社 | 白金ペーストに用いる球形状白金粉末の製造方法 |
JP3751154B2 (ja) * | 1998-10-22 | 2006-03-01 | 同和鉱業株式会社 | 銀粉の製造方法 |
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2004
- 2004-11-25 JP JP2004340789A patent/JP5028695B2/ja active Active
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- 2005-11-21 US US11/285,140 patent/US8282702B2/en active Active
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- 2005-11-23 EP EP05025568A patent/EP1666174B1/en not_active Ceased
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- 2005-11-25 KR KR1020050113277A patent/KR101141839B1/ko active IP Right Grant
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CN103339685A (zh) * | 2011-01-26 | 2013-10-02 | 纳美仕有限公司 | 导电性糊剂及其制造方法 |
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CN107983946A (zh) * | 2016-10-26 | 2018-05-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | 一种降低银粉比表面积的方法 |
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Also Published As
Publication number | Publication date |
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DE602005023402D1 (de) | 2010-10-21 |
CN101513671A (zh) | 2009-08-26 |
US20120219453A1 (en) | 2012-08-30 |
KR20060058655A (ko) | 2006-05-30 |
TWI367137B (en) | 2012-07-01 |
EP1666174B1 (en) | 2010-09-08 |
CN101513671B (zh) | 2010-12-08 |
EP1666174A3 (en) | 2006-09-13 |
JP2006152327A (ja) | 2006-06-15 |
US8992701B2 (en) | 2015-03-31 |
TW200626262A (en) | 2006-08-01 |
ATE480350T1 (de) | 2010-09-15 |
CN1781630B (zh) | 2010-08-04 |
US8282702B2 (en) | 2012-10-09 |
JP5028695B2 (ja) | 2012-09-19 |
KR101141839B1 (ko) | 2012-05-07 |
EP1666174A2 (en) | 2006-06-07 |
US20060107791A1 (en) | 2006-05-25 |
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