JPH0319283B2 - - Google Patents
Info
- Publication number
- JPH0319283B2 JPH0319283B2 JP59104358A JP10435884A JPH0319283B2 JP H0319283 B2 JPH0319283 B2 JP H0319283B2 JP 59104358 A JP59104358 A JP 59104358A JP 10435884 A JP10435884 A JP 10435884A JP H0319283 B2 JPH0319283 B2 JP H0319283B2
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- silver powder
- silver
- particle size
- added
- 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.)
- Expired - Lifetime
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 25
- 239000007864 aqueous solution Substances 0.000 claims description 18
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- HAAYBYDROVFKPU-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.N.[Ag+].[O-][N+]([O-])=O HAAYBYDROVFKPU-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- VMKYLARTXWTBPI-UHFFFAOYSA-N copper;dinitrate;hydrate Chemical compound O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O VMKYLARTXWTBPI-UHFFFAOYSA-N 0.000 claims description 3
- FOSPKRPCLFRZTR-UHFFFAOYSA-N zinc;dinitrate;hydrate Chemical compound O.[Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O FOSPKRPCLFRZTR-UHFFFAOYSA-N 0.000 claims description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 18
- 239000002245 particle Substances 0.000 description 17
- 150000002500 ions Chemical class 0.000 description 11
- 239000002244 precipitate Substances 0.000 description 10
- 239000000853 adhesive Substances 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 9
- 229910001961 silver nitrate Inorganic materials 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 101710134784 Agnoprotein Proteins 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 239000003518 caustics Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 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 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高純度で残留イオン濃度の少ない銀
粉末の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing silver powder with high purity and low residual ion concentration.
近年、IC・LSI等の集積回路用の導電材として
銀系導電性接着剤が多用されるようになつてい
る。この接着剤に用いられる銀粉末はデスペンサ
ーのつまりを発生させる粗大な粒子を含まず、然
も樹脂に混入した場合に分離、沈降を生じないた
め、平均粒径が1μm以下と微細で粒度分布巾
1.5μm以下と小さく、しかも集積回路に害を与え
るイオン化しやすい物質、例えばハロゲン元素や
アルカリ金属等の残留イオン性物質が50ppm以下
の高純度の品質特性が要求される。 In recent years, silver-based conductive adhesives have come into widespread use as conductive materials for integrated circuits such as ICs and LSIs. The silver powder used in this adhesive does not contain coarse particles that can clog the dispenser, and does not separate or settle when mixed with the resin, so it is fine with an average particle size of 1 μm or less. dish towel
It is required to have a small size of 1.5 μm or less, and high purity with less than 50 ppm of residual ionic substances such as halogen elements and alkali metals that easily ionize and harm integrated circuits.
本発明はこの集積回路用の導電性接着剤に使用
する銀粉末の製造方法に関するものである。 The present invention relates to a method for producing silver powder used in a conductive adhesive for integrated circuits.
導電性接着剤に用いる銀粉末の一般的製造方法
は、化学還元置換析出法により製造される。この
方法は銀塩水溶液に還元剤を添加し銀粉末を析出
させる方法であり、ここで用いられる還元剤は主
として苛性アルカリである。こうして得られる銀
粉末は、苛性アルカリが残留イオンとして
100ppm以上銀粉末に付着しているため、集積回
路に適用するのは好ましくない。又、還元剤とし
て苛性アルカリを使用しない場合、例えばヒドラ
ジンで還元した場合、析出する銀粉末の平均粒径
が1μmより大きく、粒度分布巾も1.5μmより大き
く、さににはこれらの値がバラツキ再現性のない
ものであつた。
A general method for producing silver powder used in conductive adhesives is a chemical reduction substitution precipitation method. In this method, a reducing agent is added to an aqueous silver salt solution to precipitate silver powder, and the reducing agent used here is mainly caustic alkali. The silver powder obtained in this way contains caustic alkali as residual ions.
Since more than 100 ppm is attached to the silver powder, it is not recommended to apply it to integrated circuits. In addition, when caustic alkali is not used as a reducing agent, for example when reduction is performed with hydrazine, the average particle size of the precipitated silver powder is larger than 1 μm and the particle size distribution width is also larger than 1.5 μm, and these values vary depending on the situation. It was not reproducible.
本発明者は、前記の従来の技術の欠点を改良
し、半導体に有害となる残留イオン濃度が50ppm
以下と少ない銀粉末、及び粉末特性のバラツキが
少なく、平均粒径が1μm以下で粒度分布巾が
1.5μm以内の品質の優れた銀粉末の製造方法につ
いて鋭意研究した結果、本発明を完成した。
The present inventor has improved the drawbacks of the above-mentioned conventional technology, and has achieved a method that reduces the concentration of residual ions harmful to semiconductors to 50 ppm.
The silver powder is as small as 1μm or less, and there is little variation in powder properties, with an average particle size of 1μm or less and a particle size distribution width.
The present invention was completed as a result of intensive research into a method for producing silver powder of excellent quality within 1.5 μm.
本発明は、アンモニア性硝酸銀水溶液に、硝酸
銅水和物又は硝酸亜鉛水和物の１種もしくは２種
を硝酸銀100重量部に対し0.5〜10重量部添加した
のち、ヒドラジンを添加することにより銀粉末を
析出させることを特徴とする銀粉末の製造方法で
ある。
In the present invention, 0.5 to 10 parts by weight of one or both of copper nitrate hydrate or zinc nitrate hydrate are added to 100 parts by weight of silver nitrate to an ammoniacal silver nitrate aqueous solution, and then hydrazine is added. This is a method for producing silver powder, which is characterized by precipitating the powder.
本発明に言うアンモニア性硝酸銀水溶液とは、
硝酸銀100重量部に対して30％アンモニア水30重
量部以上（アンモニアとして９重量部以上、以下
同じ）を硝酸銀水溶液に添加したものである。 The ammoniacal silver nitrate aqueous solution referred to in the present invention is
30 parts by weight or more of 30% ammonia water (9 parts by weight or more as ammonia, the same applies hereinafter) is added to an aqueous silver nitrate solution based on 100 parts by weight of silver nitrate.
本発明で水溶性硝酸塩の効果は粒度分布巾を狭
くすることと、粒径の調整をするためである。 In the present invention, the effect of water-soluble nitrate is to narrow the particle size distribution width and adjust the particle size.
ここで用いる水溶性硝酸塩は、硝酸銅水和物又
は硝酸亜鉛水和物の１種以上であり、添加量は、
アンモニア性硝酸銀水溶液中の硝酸銀100重量部
に対し0.5重量部〜10重量部の範囲とするのが好
ましい。その理由は、0.5重量部以下では上記の
ような効果が少なく、10重量部以上では、粒径調
整の効果が飽和の状態になり、これ以上多く添加
しても効果の増大が得られないばかりでなく、逆
に残留不純物が増大し、高純度の銀粉末が得られ
なくなるためである。 The water-soluble nitrate used here is one or more types of copper nitrate hydrate or zinc nitrate hydrate, and the amount added is:
The amount is preferably in the range of 0.5 parts by weight to 10 parts by weight per 100 parts by weight of silver nitrate in the ammoniacal silver nitrate aqueous solution. The reason for this is that below 0.5 parts by weight, the above effect is small, and above 10 parts by weight, the effect of particle size adjustment reaches a saturated state, and even if more is added, no increase in effect can be obtained. This is because, on the contrary, residual impurities increase, making it impossible to obtain highly pure silver powder.
本発明に用いる還元剤はホルマリン等のアルデ
ヒドやヒドラジン又はアルカリ（例えば、
NaOH，KOH，Na2CO3等）が考えられるが、
シドラジンを用いる方が還元効率及び残留イオン
濃度（特にNa+，K+，C1-）が少なくなるので好
ましい。 The reducing agent used in the present invention is an aldehyde such as formalin, hydrazine, or an alkali (e.g.
NaOH, KOH, Na 2 CO 3 , etc.) are possible, but
It is preferable to use cidrazine because reduction efficiency and residual ion concentration (particularly Na + , K + , C1 − ) are reduced.
以下本発明の実施例について述べる。 Examples of the present invention will be described below.
実施例 １
硝酸銀水溶液（AgNO3100ｇ／H2O300ml）に
30％アンモニア水溶液40ｇを添加し、アンモニア
性硝酸銀水溶液とし硝酸銅（Cu（NO3）・
6H2O0.5ｇ）を添加した。次ぎに抱水ヒドラジン
を添加し、白色の沈澱物を生成させた。こうして
得られた沈澱物をデカンテーシヨンにより充分に
水洗し、濾過した後低温乾燥を行つた。こうして
得られた粉末は、平均粒径1.0μm、粒度分布巾
1.5μmで、水溶性のアルカリ物質及びハロゲン物
質を合わせた残留イオン濃度（以下、単に残留イ
オン濃度と言う）が30ppmの銀粉末であつた。Example 1 Silver nitrate aqueous solution (AgNO 3 100g/H 2 O 300ml)
Add 40g of 30% ammonia aqueous solution to make an ammoniacal silver nitrate aqueous solution and prepare copper nitrate (Cu(NO 3 ).
6H 2 O (0.5 g) was added. Hydrazine hydrate was then added to form a white precipitate. The precipitate thus obtained was thoroughly washed with water by decantation, filtered, and then dried at low temperature. The powder thus obtained had an average particle size of 1.0 μm and a particle size distribution width of
The silver powder had a diameter of 1.5 μm and a residual ion concentration (hereinafter simply referred to as residual ion concentration) of 30 ppm, including water-soluble alkaline substances and halogen substances.
以上のようにして得られた銀粉末80重量部とエ
ポキシ樹脂接着剤20重量部を均一混練してペース
トとしたものを150℃−30分間で硬化させると、
比抵抗１×10-4Ω・cm、接着力50Kg／cm2の特性を
もつた導電性接着剤が得られた。 When 80 parts by weight of the silver powder obtained in the above manner and 20 parts by weight of the epoxy resin adhesive were uniformly kneaded to form a paste, it was cured at 150°C for 30 minutes.
A conductive adhesive with specific resistance of 1×10 -4 Ω·cm and adhesive strength of 50 kg/cm 2 was obtained.
実施例 ２
硝酸銀水溶液（AgNO3100ｇ／H2O300ml）に
30％アンモニア水溶液40ｇを添加し、アンモニア
性硝酸銀水溶液とし硝酸亜鉛（Zn（NO3）2・
6H2O10ｇ）を添加する。次ぎに抱水ヒドラジン
を添加し、灰黄色の沈澱物を生成させた。こうし
て得られた沈澱物を実施例１と同じ方法で濾過水
洗を行つた。こうして得られた粉末は、平均粒径
0.2μm、粒度分布巾が0.2μmで、残留イオン濃度
が50ppmの銀粉末であつた。この銀粉末をペース
ト化したものは実施例１と同等の特性をもつてい
た。Example 2 Silver nitrate aqueous solution (AgNO 3 100g/H 2 O 300ml)
Add 40g of 30% ammonia aqueous solution to make an ammoniacal silver nitrate aqueous solution and make zinc nitrate (Zn(NO 3 ) 2 .
6H 2 O (10 g). Hydrazine hydrate was then added to form a gray-yellow precipitate. The precipitate thus obtained was filtered and washed with water in the same manner as in Example 1. The powder thus obtained has an average particle size of
The silver powder had a particle size distribution width of 0.2 μm and a residual ion concentration of 50 ppm. A paste obtained from this silver powder had properties equivalent to those of Example 1.
実施例 ３
硝酸銀水溶液（AgNO3100ｇ／H2O300ml）に
30％アンモニア水溶液40ｇ添加し、アンモニア性
硝酸銀水溶液とし硝酸銅・硝酸亜鉛を各々５ｇ添
加した。次ぎに抱水ヒドラジンを添加し、灰色の
沈澱物を生成させた。こうして得られた沈澱物を
実施例１と同じ方法で濾過水洗を行つた。こうし
て得られた粉末は平平均粒径0.08μm、粒度分布
巾0.05μmで、残留イオン濃度が50ppmの銀粉末
であつた。この銀粉末をペースト化したものの硬
化物は、比抵抗５×10-4Ω・cm、接着力50Kg／cm2
の特性をもつていた。Example 3 Silver nitrate aqueous solution (AgNO 3 100g/H 2 O 300ml)
40g of a 30% ammonia aqueous solution was added to form an ammoniacal silver nitrate aqueous solution, and 5g each of copper nitrate and zinc nitrate were added. Hydrazine hydrate was then added to form a gray precipitate. The precipitate thus obtained was filtered and washed with water in the same manner as in Example 1. The powder thus obtained was a silver powder with an average particle diameter of 0.08 μm, a particle size distribution width of 0.05 μm, and a residual ion concentration of 50 ppm. The cured product made from this silver powder paste has a specific resistance of 5×10 -4 Ω・cm and an adhesive strength of 50 Kg/cm 2
It had the characteristics of
比較例 １
硝酸銀水溶液（AgNO3100ｇ／H2O300ml）に
ホルマリン50mlを添加し、次いで苛性ソーダ水溶
液（NaCH100ｇ／H2O200ml）を添加し、白色
沈澱物を生成させる。こうして得られた沈澱物を
実施例１と同じ方法で濾過水洗を行つた。こうし
て得られた粉末は、粒径1.0μmで、残留イオン濃
度200ppmの銀粉末であつた。Comparative Example 1 50 ml of formalin is added to a silver nitrate aqueous solution (AgNO 3 100 g/H 2 O 300 ml), and then a caustic soda aqueous solution (NaCH 100 g/H 2 O 200 ml) is added to form a white precipitate. The precipitate thus obtained was filtered and washed with water in the same manner as in Example 1. The powder thus obtained was a silver powder with a particle size of 1.0 μm and a residual ion concentration of 200 ppm.
比較例 ２
硝酸銀水溶液（AgNO310ｇ／H2O300ml）に30
％アンモニア水溶液40ｇを添加し、アンモニア性
硝酸銀水溶液とした。次に抱水ヒドラジンを添加
し、白色の沈澱物を生成させた。こうして得られ
た沈澱物を実施例１と同じ方法で濾過水洗を行つ
た。こうして得られた粉末は、平均粒径3μmで、
粒度分布巾2μmで、残留イオン濃度50ppmの銀粉
末であつた。Comparative Example 2 30% in silver nitrate aqueous solution (AgNO 3 10g/H 2 O 300ml)
% ammonia aqueous solution was added to obtain an ammoniacal silver nitrate aqueous solution. Hydrazine hydrate was then added to form a white precipitate. The precipitate thus obtained was filtered and washed with water in the same manner as in Example 1. The powder thus obtained had an average particle size of 3 μm,
The silver powder had a particle size distribution width of 2 μm and a residual ion concentration of 50 ppm.
本発明により得られた銀粉末は、微細、均一で
あるため樹脂と混入した場合、分離、沈降を発生
せず、然も残留イオンの少ない高純度銀粉末であ
るため、半導体に使用される導電性接着剤の原料
として好適である。
The silver powder obtained by the present invention is fine and uniform, so when it is mixed with resin, it does not separate or settle, and since it is a high-purity silver powder with few residual ions, it is used as a conductive material for semiconductors. It is suitable as a raw material for adhesives.
Claims (1)
又は硝酸亜鉛水和物の１種もしくは２種を硝酸銀
100重量部に対し0.5〜10重量部添加したのち、ヒ
ドラジンを添加することにより銀粉末を析出させ
ることを特徴とする銀粉末の製造方法。1 Add one or two of copper nitrate hydrate or zinc nitrate hydrate to an ammoniacal silver nitrate aqueous solution.
A method for producing silver powder, which comprises adding 0.5 to 10 parts by weight per 100 parts by weight, and then adding hydrazine to precipitate silver powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10435884A JPS60248803A (en) | 1984-05-22 | 1984-05-22 | Production of silver powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10435884A JPS60248803A (en) | 1984-05-22 | 1984-05-22 | Production of silver powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60248803A JPS60248803A (en) | 1985-12-09 |
| JPH0319283B2 true JPH0319283B2 (en) | 1991-03-14 |
Family
ID=14378624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10435884A Granted JPS60248803A (en) | 1984-05-22 | 1984-05-22 | Production of silver powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60248803A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62280308A (en) * | 1986-05-30 | 1987-12-05 | Mitsui Mining & Smelting Co Ltd | Production of fine silver-palladium alloy power |
| JPS63115737A (en) * | 1986-11-05 | 1988-05-20 | 松下電工株式会社 | Electric laminated board |
| CA2585644A1 (en) * | 2004-10-29 | 2006-05-11 | Nanodynamics, Inc. | Aqueous-based method for producing ultra-fine metal powders |
| JP5415708B2 (en) * | 2008-03-26 | 2014-02-12 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder manufacturing method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4842782A (en) * | 1971-09-30 | 1973-06-21 |
-
1984
- 1984-05-22 JP JP10435884A patent/JPS60248803A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4842782A (en) * | 1971-09-30 | 1973-06-21 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60248803A (en) | 1985-12-09 |
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