JP2003281948A - Manufacturing method for conductive paste - Google Patents
Manufacturing method for conductive pasteInfo
- Publication number
- JP2003281948A JP2003281948A JP2002082569A JP2002082569A JP2003281948A JP 2003281948 A JP2003281948 A JP 2003281948A JP 2002082569 A JP2002082569 A JP 2002082569A JP 2002082569 A JP2002082569 A JP 2002082569A JP 2003281948 A JP2003281948 A JP 2003281948A
- Authority
- JP
- Japan
- Prior art keywords
- paste
- conductive paste
- viscosity
- organic vehicle
- roll mill
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000004020 conductor Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004065 semiconductor Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229940116411 terpineol Drugs 0.000 description 2
- 229910002482 Cu–Ni Inorganic materials 0.000 description 1
- 229910017770 Cu—Ag Inorganic materials 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910008423 Si—B Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
Landscapes
- Conductive Materials (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、半導体素子等の各
種電子部品の電極形成に好適に用いられる、導電性ペー
ストの製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a conductive paste which is suitable for forming electrodes of various electronic parts such as semiconductor elements.
【0002】[0002]
【従来の技術】従来、半導体素子等の各種電子部品に電
極を形成するためのものとして、導電性ペーストが知ら
れている。このような導電性ペーストは、一般に、金属
粉末、ガラスフリット及び有機ビヒクルを有し、それら
を混ぜ合わせ、ミキサーで予備混合した後、ロールミル
等により均一に分散され、その後、所定の粘度値に調整
するという工法にて製造されている。2. Description of the Related Art Conventionally, a conductive paste has been known as a material for forming electrodes on various electronic components such as semiconductor elements. Such a conductive paste generally has a metal powder, a glass frit and an organic vehicle, which are mixed and premixed with a mixer, and then uniformly dispersed by a roll mill or the like, and then adjusted to a predetermined viscosity value. It is manufactured by the construction method called.
【0003】[0003]
【発明が解決しようとする課題】しかしながら、従来の
工法では、導電性ペーストの粘度における経時変化が発
生することがしばしば観察され、上記導電性ペーストを
用いて作製された電子部品の歩留りが低下するという問
題を生じている。However, in the conventional method, it is often observed that the viscosity of the conductive paste changes with time, and the yield of electronic parts manufactured using the conductive paste is reduced. Is causing the problem.
【0004】本発明者らは、上記経時変化の原因につい
て、鋭意検討したところ、上記原因が、均一分散後に粘
度調整の目的で添加した、有機ビヒクル中の樹脂と無機
フィラー(金属粉末及びガラスフリット)との間での吸
着が平衡に達していないためであることを見出した。そ
こで、本発明者らは、導電性ペーストの製造時に、上記
吸着が、より平衡に達する方法を検討した。The inventors of the present invention have diligently studied the cause of the above-described change with time. As a result, the cause is that the resin and the inorganic filler (metal powder and glass frit) in the organic vehicle added for the purpose of adjusting the viscosity after uniform dispersion. It has been found that the adsorption between (1) and () is not in equilibrium. Therefore, the present inventors have studied a method in which the above adsorption reaches more equilibrium during the production of the conductive paste.
【0005】本発明は、長期にわたり保存安定性の高
い、導電性ペーストの製造方法を提供することを目的と
している。An object of the present invention is to provide a method for producing a conductive paste which has a high storage stability for a long period of time.
【0006】[0006]
【課題を解決するための手段】上記目的を達成するため
に、本発明の導電性ペーストの製造方法は、少なくとも
金属粉末及び第一の有機ビヒクルを混合した後、ロール
ミルにて分散させてペーストとする第一工程と、分散済
みのペーストに第二の有機ビヒクルを混合して、上記ペ
ーストの粘度を調整する第二工程と、粘度調整済みのペ
ーストをロールミルで分散させる第三工程と、を備える
ことを特徴としている。In order to achieve the above object, a method for producing a conductive paste according to the present invention is to prepare a paste by mixing at least a metal powder and a first organic vehicle and then dispersing the mixture with a roll mill. A first step of mixing, a second step of mixing the second paste with the second organic vehicle to adjust the viscosity of the paste, and a third step of dispersing the viscosity-adjusted paste with a roll mill. It is characterized by that.
【0007】なお、第一及び第二の有機ビヒクルは、互
いに同一組成のもの、又は異なる組成のものを適宜用い
ることができる。そして、有機ビヒクルを構成する樹脂
としては、ニトロセルロース、エチルセルロース等が挙
げられ、溶剤としては、ジエチレングリコールモノブチ
ルエーテルアセテート、エチレングリコールモノブチル
エーテル、ターピネオール、ソルフィット、ブチルカル
ビトールアセテート、ジアセトンアルコール等が挙げら
れる。As the first and second organic vehicles, those having the same composition or different compositions can be appropriately used. And as the resin constituting the organic vehicle, nitrocellulose, ethyl cellulose and the like can be mentioned, and as the solvent, diethylene glycol monobutyl ether acetate, ethylene glycol monobutyl ether, terpineol, solfit, butyl carbitol acetate, diacetone alcohol and the like can be mentioned. To be
【0008】上記方法によれば、粘度調整を目的とし
た、第二の有機ビヒクルを添加した後、再度ロールミル
により再分散処理を実施することで、それにより製造さ
れた導電性ペーストは、金属粉末(無機フィラー)に対
する有機ビヒクル中の樹脂の吸着平衡を、より改善でき
るので、経時的な吸脱着による物性変化(粘度変化)を
抑制でき、導電性ペーストの粘度の保存安定性を向上で
きる。According to the above method, after adding the second organic vehicle for the purpose of adjusting the viscosity, the re-dispersion treatment is carried out again by the roll mill, so that the conductive paste produced thereby is a metal powder. Since the adsorption equilibrium of the resin in the organic vehicle with respect to the (inorganic filler) can be further improved, the physical property change (viscosity change) due to adsorption / desorption over time can be suppressed, and the storage stability of the viscosity of the conductive paste can be improved.
【0009】[0009]
【発明の実施の形態】本発明の導電性ペーストの製造方
法について、以下に示す実施例及び比較例により詳細に
説明する。なお、本発明は、これら実施例によって制限
されるものではない。BEST MODE FOR CARRYING OUT THE INVENTION The method for producing a conductive paste of the present invention will be described in detail with reference to the following examples and comparative examples. The present invention is not limited to these examples.
【0010】(実施例)本実施例の導電性ペーストの製
造方法を、図1に示すフローチャートに基づいて以下に
説明する。(Example) A method for producing a conductive paste of this example will be described below with reference to the flow chart shown in FIG.
【0011】まず、図1に示すように、Pb−Si−B
系ガラスフリット(平均粒径3μm)と、金属粉末とし
てのAg粉末(平均粒径0.5μm)と、第一の有機ビ
ヒクルとを、表1に記載の配合比にてミキサーで予備混
練した(ステップ1、以下、ステップをSと記す)。First, as shown in FIG. 1, Pb-Si-B
The system glass frit (average particle size 3 μm), Ag powder (average particle size 0.5 μm) as the metal powder, and the first organic vehicle were pre-kneaded in a mixer at the compounding ratio shown in Table 1 ( Step 1, hereinafter referred to as S).
【0012】その後、その混練物(ペースト)をロール
ミルのロール間に3回通して、上記混練物に対して分散
処理を実施した(S2)。続いて、上記分散処理後の混
練物に第二の有機ビヒクルを添加して、上記分散処理後
の混練物を所定の粘度に調整した(S3)。Then, the kneaded material (paste) was passed between the rolls of a roll mill three times to perform a dispersion treatment on the kneaded material (S2). Then, the second organic vehicle was added to the kneaded product after the dispersion treatment to adjust the kneaded product after the dispersion treatment to a predetermined viscosity (S3).
【0013】次に、粘度調整後の混練物を、再度ロール
ミルに3回通して分散処理(加圧による)を施す(S
4)ことで導電性ペーストを製造した。Next, the kneaded material whose viscosity has been adjusted is again passed through the roll mill three times for dispersion treatment (by pressure) (S).
4) The electrically conductive paste was manufactured by the above.
【0014】[0014]
【表1】 [Table 1]
【0015】第一の有機ビヒクル、及び第二の有機ビヒ
クルは、例えば、樹脂としてのニトロセルロース、溶剤
としてのジエチレングリコールモノブチルエーテルアセ
テート、溶剤としてのエチレングリコールモノブチルエ
ーテル、溶剤としてのターピネオールを互いに混合した
ものである。The first organic vehicle and the second organic vehicle are, for example, a mixture of nitrocellulose as a resin, diethylene glycol monobutyl ether acetate as a solvent, ethylene glycol monobutyl ether as a solvent, and terpineol as a solvent. Is.
【0016】一方、比較例として、上記S4の工程を省
いた以外は、上記実施例と同様に製造して、比較導電性
ペーストを製造した。On the other hand, as a comparative example, a comparative conductive paste was manufactured in the same manner as in the above example except that the step S4 was omitted.
【0017】次に、上記実施例の導電性ペースト、及び
比較導電性ペーストを、それぞれ25℃下にて保管し、
それらの粘度の経時変化を調べた。粘度測定は、リオン
粘度計VT-04 No.2 ローターを用いた。それらの粘度
の測定結果を表2に合わせて示す。実施例の導電性ペー
ストは、表2から明らかなように、比較導電性ペースト
と比較して、粘度が経時的に安定していることが分か
る。Next, the conductive paste of the above example and the comparative conductive paste were respectively stored at 25 ° C.,
The change with time of their viscosity was examined. For the viscosity measurement, a Rion viscometer VT-04 No. 2 rotor was used. The measurement results of those viscosities are also shown in Table 2. As is clear from Table 2, the conductive pastes of Examples are found to have stable viscosity over time as compared with the comparative conductive paste.
【0018】[0018]
【表2】 [Table 2]
【0019】また、上記粘度経時変化の評価に用いた導
電性ペーストのパターン形成性能の経時変化を図3に示
す。なお、同評価は、図2に示すスクリーン印刷(SU
S200メッシュ)パターンにより、アルミナ基板1上
に導電性ペーストのパターンを印刷し、150℃で10
分間乾燥した後、600℃で1分間(in-out 5分)の
条件で焼成し、上記パターンに基づく電極パターン2を
形成した後、図2に示す電極パターン2の各バスバー2
a間の抵抗値を測定し、抵抗値の高低によるペーストの
吐出性を比較して行った。FIG. 3 shows the change over time in the pattern forming performance of the conductive paste used in the evaluation of the change over time in the viscosity. The evaluation is based on the screen printing (SU
S200 mesh) pattern, a pattern of conductive paste is printed on the alumina substrate 1, and the pattern is printed at 150 ° C. for 10 minutes.
After drying for 1 minute, the electrode is patterned at 600 ° C. for 1 minute (in-out 5 minutes) to form an electrode pattern 2 based on the above pattern, and then each bus bar 2 of the electrode pattern 2 shown in FIG.
The resistance value between a and a was measured, and the dischargeability of the paste was compared by the resistance value.
【0020】本実施例の導電性ペーストは、図3から明
らかなように、製造直後(0カ月、初期)から、6ヶ月
間安定したパターニング性能を維持できるが、比較例の
比較導電性ペーストは、経時的な粘度変化と共に各バス
バー2a間のライン抵抗が上昇し、スクリーン印刷時の
メッシュパターンからのペースト吐出量が経時的に低下
していることが分かる。As is clear from FIG. 3, the conductive paste of this example can maintain stable patterning performance for 6 months immediately after production (0 months, initial period), but the comparative conductive paste of the comparative example does not. It can be seen that the line resistance between the bus bars 2a increases as the viscosity changes with time, and the amount of paste discharged from the mesh pattern during screen printing decreases with time.
【0021】これにより、比較導電性ペーストを用いて
電極を形成した半導体素子では、ライン抵抗値が上昇し
て規格値外となり、歩留りの低下を生じることは明らか
である。As a result, it is clear that in the semiconductor element in which the electrodes are formed by using the comparative conductive paste, the line resistance value rises and becomes out of the standard value, and the yield decreases.
【0022】一方、本実施例の導電性ペーストを用いて
電極を形成した半導体素子においては、ライン抵抗値の
上昇を比較例より抑制して、規格値外となる半導体素子
の発生を低減できて、上記半導体素子の歩留りを改善で
きる。On the other hand, in the semiconductor element in which the electrode is formed by using the conductive paste of the present embodiment, the increase of the line resistance value can be suppressed more than in the comparative example, and the occurrence of the semiconductor element out of the standard value can be reduced. The yield of the semiconductor device can be improved.
【0023】なお、金属粉末については、特に形状、サ
イズについて限定されるわけではなく、既存のAg、C
uまたはNiを主成分とする金属粉末を単独、もしくは
上記各主成分の任意の合金の金属粉末でもかまわない。
好適な上記金属粉末としては、Cu単体、Ag単体、N
i単体、Cu−Ni、Cu−Ag等が挙げられるが、A
g単体が最も好ましい。The metal powder is not particularly limited in shape and size, and the existing Ag and C may be used.
The metal powder containing u or Ni as a main component may be used alone, or the metal powder of any alloy of the above main components may be used.
Suitable metal powders include Cu simple substance, Ag simple substance, N
i simple substance, Cu-Ni, Cu-Ag, etc. are mentioned.
Most preferred is g.
【0024】また、ガラスフリットの種類については、
特に限定されるわけではなく、既存のガラスフリットを
単独もしくは複数以上使用してもかまわない。Regarding the type of glass frit,
There is no particular limitation, and existing glass frits may be used alone or in combination of two or more.
【0025】さらに、樹脂及び溶剤を有する有機ビヒク
ルについても、特に限定されるわけではなく、既存の有
機ビヒクルを単独もしくは複数以上使用してもかまわな
い。Further, the organic vehicle containing the resin and the solvent is not particularly limited, and existing organic vehicles may be used alone or in combination of two or more.
【0026】[0026]
【発明の効果】本発明の導電性ペーストの製造方法は、
以上のように、粘度調整済みのペーストをさらにロール
ミルで分散させる工程を含む方法である。The method for producing the conductive paste of the present invention comprises:
As described above, the method includes a step of further dispersing the viscosity-adjusted paste with a roll mill.
【0027】それゆえ、上記方法は、無機フィラー(金
属粉末等)に対する有機ビヒクル中の樹脂における吸着
平衡を、より改善できるので、経時的な吸脱着による物
性変化を抑制でき、導電性ペーストの粘度の保存(保
管)安定性を向上できる。Therefore, the above method can further improve the adsorption equilibrium of the resin in the organic vehicle with respect to the inorganic filler (metal powder or the like), so that the physical property change due to adsorption and desorption over time can be suppressed and the viscosity of the conductive paste can be suppressed. The storage stability of can be improved.
【0028】よって、上記方法による導電性ペーストを
半導体素子等の各種電子部品の電極の形成に用いること
により、上記半導体素子等の各種電子部品の歩留りを改
善できるという効果を奏する。Therefore, by using the conductive paste according to the above method for forming electrodes of various electronic parts such as semiconductor elements, it is possible to improve the yield of various electronic parts such as semiconductor elements.
【図1】本発明に係る実施例の導電性ペーストの製造方
法における各工程を示すフローチャートである。FIG. 1 is a flowchart showing each step in a method for manufacturing a conductive paste according to an example of the present invention.
【図2】上記実施例及び比較例の導電性ペーストの印刷
性評価に使用した電極パターンの平面図である。FIG. 2 is a plan view of an electrode pattern used for evaluation of printability of the conductive pastes of the examples and comparative examples.
【図3】上記実施例及び比較例の導電性ペーストのペー
スト吐出量を比較して示すための、ライン抵抗の経時変
化を示すグラフである。FIG. 3 is a graph showing changes over time in line resistance for comparing and showing the paste discharge amounts of the conductive pastes of the above-described example and comparative example.
Claims (2)
ルを混合した後、ロールミルにて分散させてペーストと
する第一工程と、 分散済みのペーストに第二の有機ビヒクルを混合して、
上記ペーストの粘度を調整する第二工程と、 粘度調整済みのペーストをロールミルで分散させる第三
工程と、を備えることを特徴とする導電性ペーストの製
造方法。1. A first step of mixing at least a metal powder and a first organic vehicle and then dispersing with a roll mill to form a paste, and mixing the dispersed paste with a second organic vehicle,
A method for producing a conductive paste, comprising: a second step of adjusting the viscosity of the paste, and a third step of dispersing the paste whose viscosity has been adjusted by a roll mill.
ラスフリットを混合することを特徴とする請求項1記載
の導電性ペーストの製造方法。2. The method for producing a conductive paste according to claim 1, wherein a glass frit is further mixed with the paste in the first step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002082569A JP2003281948A (en) | 2002-03-25 | 2002-03-25 | Manufacturing method for conductive paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002082569A JP2003281948A (en) | 2002-03-25 | 2002-03-25 | Manufacturing method for conductive paste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003281948A true JP2003281948A (en) | 2003-10-03 |
Family
ID=29230701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002082569A Pending JP2003281948A (en) | 2002-03-25 | 2002-03-25 | Manufacturing method for conductive paste |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2003281948A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006156204A (en) * | 2004-11-30 | 2006-06-15 | Tdk Corp | Manufacturing method of conductor paste for printing, and manufacturing method of laminated ceramic components |
| JP2006351348A (en) * | 2005-06-16 | 2006-12-28 | Matsushita Electric Ind Co Ltd | Method for producing conductive paste and method for producing multilayer ceramic electronic component |
| KR20200066076A (en) * | 2018-11-30 | 2020-06-09 | 엘에스니꼬동제련 주식회사 | Method for producing the conductive paste reducing change of elapsed time in viscosity |
-
2002
- 2002-03-25 JP JP2002082569A patent/JP2003281948A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006156204A (en) * | 2004-11-30 | 2006-06-15 | Tdk Corp | Manufacturing method of conductor paste for printing, and manufacturing method of laminated ceramic components |
| JP2006351348A (en) * | 2005-06-16 | 2006-12-28 | Matsushita Electric Ind Co Ltd | Method for producing conductive paste and method for producing multilayer ceramic electronic component |
| KR20200066076A (en) * | 2018-11-30 | 2020-06-09 | 엘에스니꼬동제련 주식회사 | Method for producing the conductive paste reducing change of elapsed time in viscosity |
| KR102152841B1 (en) | 2018-11-30 | 2020-09-07 | 엘에스니꼬동제련 주식회사 | Method for producing the conductive paste reducing change of elapsed time in viscosity |
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