JPH0443586A - Manufacture of platinum resistance heater - Google Patents
Manufacture of platinum resistance heaterInfo
- Publication number
- JPH0443586A JPH0443586A JP14933090A JP14933090A JPH0443586A JP H0443586 A JPH0443586 A JP H0443586A JP 14933090 A JP14933090 A JP 14933090A JP 14933090 A JP14933090 A JP 14933090A JP H0443586 A JPH0443586 A JP H0443586A
- Authority
- JP
- Japan
- Prior art keywords
- platinum
- heating element
- resistance heating
- heat
- platinum resistance
- 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
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 37
- 238000007747 plating Methods 0.000 claims description 10
- 229920002120 photoresistant polymer Polymers 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000007772 electroless plating Methods 0.000 abstract description 10
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001259 photo etching Methods 0.000 abstract description 4
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052763 palladium Inorganic materials 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 6
- 238000005238 degreasing Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 235000011150 stannous chloride Nutrition 0.000 description 2
- 239000001119 stannous chloride Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Landscapes
- Resistance Heating (AREA)
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、白金抵抗発熱体の製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for manufacturing a platinum resistance heating element.
（従来技術とその問題点）
従来、白金抵抗発熱体の製造方法としては、白金ペース
トを耐熱性基材上に塗布し、乾燥したのち、焼成して製
造するか、白金の化合物を有機溶剤に溶解した液状のも
のを耐熱性基材上に塗布、乾燥、焼成して製造されてい
る。(Prior art and its problems) Conventionally, platinum resistance heating elements have been manufactured by applying platinum paste on a heat-resistant base material, drying it, and then firing it, or by applying a platinum compound to an organic solvent. It is manufactured by applying a dissolved liquid onto a heat-resistant substrate, drying, and baking.
白金抵抗発熱体は、製品として数オーｌ、から１００オ
ーム程度の小さな抵抗値が要求される。As a product, a platinum resistance heating element is required to have a small resistance value of several ohms to about 100 ohms.
しかし、前者は電気伝導率が低く白金バルクの１５〜２
０％程度でありこれを解消するためには白金量を多くし
て調節するので経゛済的な問題が生じ、また後者は耐熱
性基材への密着性を高めるために白金以外の成分を含め
るため、やはり電気伝導率が低下することと、−回の塗
布、乾燥、焼成の操作では白金抵抗発熱体として不十分
であるため繰り返し操作が必要となる欠点がある。However, the former has a low electrical conductivity of 15 to 2
In order to solve this problem, the amount of platinum must be increased, which poses an economical problem.The latter also involves adding components other than platinum to improve adhesion to the heat-resistant substrate. However, since the platinum resistance heating element is not sufficiently coated, the electrical conductivity decreases, and the repeated coating, drying, and firing operations are insufficient as a platinum resistance heating element, so repeated operations are required.
実際に白金インクやペーストにおけるシート抵抗値は厚
さ１０μｍにおいて５０ミリオ一ム／口程度である。In fact, the sheet resistance value of platinum ink or paste is about 50 milliohms/ink at a thickness of 10 μm.
抵抗値の小さな抵抗体を得るには、回路幅を広くしたり
するなど主に白金使用量を増やして対応している。In order to obtain a resistor with a low resistance value, the main method is to increase the amount of platinum used, such as by widening the circuit width.
（発明の目的）
発明者は、白金使用量を減少させる目的で白金の薄膜形
成を無電解メツキによって行う白金抵抗発熱体の検討を
行ってきた。(Object of the Invention) The inventor has been studying a platinum resistance heating element in which a thin platinum film is formed by electroless plating for the purpose of reducing the amount of platinum used.
本発明は、従来法の欠点を解決するために成されたもの
で、簡便な方法で白金の使用量を減少させることと、電
気伝導率も白金バルクに近似させ、安定した白金抵抗発
熱体回路を耐熱性基材上に形成する白金抵抗発熱体の製
造方法を提供することを目的とする。The present invention was made in order to solve the drawbacks of the conventional method, and it is possible to reduce the amount of platinum used by a simple method, and to make the electrical conductivity close to that of bulk platinum, thereby creating a stable platinum resistance heating element circuit. An object of the present invention is to provide a method for manufacturing a platinum resistance heating element, which is formed on a heat-resistant base material.
（問題点を解決するための手段）
本発明は、耐熱性基材上に白金抵抗発熱体回路をホトレ
ジストを用いて形成する白金抵抗発熱体の製造方法にお
いて、白金抵抗発熱体回路形成が無電解白金メッキエ程
と、４５０〜６００℃で熱処理する工程とから成ること
を特徴とする白金抵抗発熱体の製造方法である。(Means for Solving the Problems) The present invention provides a method for manufacturing a platinum resistance heating element in which a platinum resistance heating element circuit is formed on a heat-resistant base material using a photoresist. A method for manufacturing a platinum resistance heating element characterized by comprising a platinum plating process and a heat treatment process at 450 to 600°C.
以下、本発明について詳細に説明する。The present invention will be explained in detail below.
耐熱性基材上に白金の薄膜回路を施すのは次の２つの工
程のいずれかによる。Platinum thin film circuits are applied to heat-resistant substrates by one of the following two steps.
１つは、該耐熱性基材に密着させるために耐熱性基材の
表面を活性化処理して次いでスズそしてパラジウムの金
属処理をしたのち、白金無電解メツキを施す。One method is to activate the surface of the heat-resistant base material in order to make it adhere to the heat-resistant base material, then perform metal treatment with tin and palladium, and then perform electroless plating with platinum.
次いで、白金メツキ部分を抵抗発熱体回路に形成するに
は、レジスト被膜を施しフォトエツチングにより任意の
回路の逆パターンを形成し、王水等の酸で露出部分の白
金メツキ被膜を溶解し、次いで、レジスト被膜を除去し
て抵抗発熱体回路を形成する方法である。Next, to form the platinum plating part into a resistance heating element circuit, a resist film is applied, a reverse pattern of the arbitrary circuit is formed by photoetching, the exposed part of the platinum plating film is dissolved with an acid such as aqua regia, and then , a method of forming a resistive heating element circuit by removing the resist film.
もうひとつは、耐熱性基材上にレジスト被膜を施し、抵
抗発熱体回路パターンをフォトエツチングにより形成し
、露出している耐熱性基材の表面を活性化処理して次い
でスズそしてパラジウムの金属処理をしたのち、白金無
電解メツキを施し、レジスト部分を除去して白金抵抗発
熱体回路を形成する方法である。The other method is to apply a resist film on a heat-resistant base material, form a resistive heating element circuit pattern by photoetching, activate the exposed surface of the heat-resistant base material, and then metallize it with tin and palladium. After that, electroless platinum plating is applied, and the resist portion is removed to form a platinum resistance heating element circuit.
無電解メツキによる白金薄膜は、白金バルクに近似した
電気伝導率が得やすい特徴があるが、白金メツキを付け
た直後と実際にヒータとしてしばらく使用した後の抵抗
値に差があり、使用を重ねるに連れて抵抗値が徐々に低
下する欠点がある。A thin platinum film produced by electroless plating has the characteristic that it is easy to obtain electrical conductivity close to that of bulk platinum, but there is a difference in resistance value immediately after platinum plating is applied and after it has actually been used as a heater for a while, making it difficult to use repeatedly. The disadvantage is that the resistance value gradually decreases over time.
電気伝導率を安定させるためと、白金の抵抗発熱体回路
の密着性を高めるために４５０〜６０００Ｃで熱処理す
る。Heat treatment is performed at 450 to 6000 C in order to stabilize the electrical conductivity and to improve the adhesion of the platinum resistance heating element circuit.
上記の熱処理温度とするのは６００℃以上では白金が溶
解して凝集することがあり、４５０℃以下では電気伝導
率が安定したものが得られず、特に抵抗発熱体として利
用するにあたり長時間において電気伝導率が変化して機
能を損なうことが生ずるからである。The above heat treatment temperature is required because platinum may melt and agglomerate at temperatures above 600°C, and below 450°C it is difficult to obtain stable electrical conductivity, especially for long periods when used as a resistance heating element. This is because the electrical conductivity changes and the function is impaired.
以上の工程を繰り返すことにより無電解メツキと熱処理
の組み合わせにより得られた白金抵抗発熱体の抵抗はペ
ーストやインクによるものの約１／２から１／３にする
ことができる。By repeating the above steps, the resistance of a platinum resistance heating element obtained by a combination of electroless plating and heat treatment can be reduced to about 1/2 to 1/3 of that obtained by paste or ink.
また、上記の温度で処理すれば白金薄膜が耐熱性基材に
密着させる効果もある。Furthermore, treatment at the above temperature has the effect of making the platinum thin film adhere to the heat-resistant substrate.
前記熱処理を白金無電解メツキし、抵抗発熱体回路を形
成したのちに限定するものでなく、白金無電解メツキを
施したのちに熱処理しても熱処理の効果は得られるもの
である。The heat treatment is not limited to being performed after electroless platinum plating and forming the resistance heating element circuit, but the effect of the heat treatment can be obtained even if the heat treatment is performed after electroless platinum plating.
以下、本発明に係わる実施例を記載するが、該実施例は
本発明を限定するものではない。Examples related to the present invention will be described below, but the examples are not intended to limit the present invention.
（実施例１）
セラミック基板（１０ｍｍＸ １０ｍｍＸ厚み０． ６
ｍｍ）４枚をそれぞれに前処理として電解脱脂液（ＥＥ
ＪＡ社製イードレックス１２）を用いて超音波脱脂を６
０°ＣＩ分間行い、次いで塩化第一スズ１０ｇ／ｆｆ溶
液に５分間浸漬し、次いで塩化パラジウム２ｇ／ｌ溶液
に４０°Ｃ５分間浸漬したのち、白金の無電解メツキと
してＥＥＪＡ社製レ社製コクトロレスＰｔメツキ溶液ｔ
２ ｇ／Ａ）を用い無電解メツキ時間を１５分間、３
０分間、４５分間および７０分間して白金薄膜１〜４μ
ｍの厚みの違うものを形成した。(Example 1) Ceramic substrate (10 mm x 10 mm x thickness 0.6
mm) 4 sheets were pretreated with electrolytic degreasing solution (EE).
Ultrasonic degreasing using JA Eedrex 12)
After immersing in a 10 g/ff solution of stannous chloride for 5 minutes, and then immersing in a 2 g/l palladium chloride solution at 40°C for 5 minutes, electroless plating of platinum was performed using EEJA Co., Ltd.'s Coctrores. Pt plating solution
2 g/A), electroless plating time was 15 minutes, 3
0 minutes, 45 minutes and 70 minutes, platinum thin film 1~4μ
Thicknesses with different thicknesses of m were formed.
次いで、ホトレジストを塗布し乾燥して被膜を形成し、
写真製版してホトレジストにて白金抵抗発熱体回路パタ
ーンを描き王水エツチングしたのちホトレジストはくす
して、洗浄し、乾燥したのち電気炉中で６００℃で３０
分間熱処理した回路（幅０．４ｍｍＸ長さ８５ｍｍ）の
抵抗値を測定したところ、５５オーム、４０オーム、２
０オーム、１５オームであった。Next, photoresist is applied and dried to form a film,
After photolithography, a platinum resistance heating element circuit pattern was drawn using photoresist, and etched with aqua regia.
When the resistance values of the circuit (width 0.4 mm x length 85 mm) were heat-treated for minutes, they were measured to be 55 ohms, 40 ohms, 2
They were 0 ohm and 15 ohm.
（実施例２）
セラミック基板（１０ｍｍＸ Ｉ ＯｍｍＸ厚み０．６
ｍｍ）にホトレジストを塗布し乾燥して被膜を形成し、
写真製版してホトレジストにて白金抵抗発熱体回路逆パ
ターンを描き、前処理として電解脱脂液（ＥＥＪＡ社製
イードレックス１２）を用いて超音波脱脂を６０°Ｃ１
分間行い、次いで塩化第一スズｌＯｇ／ｌ溶液に５分間
浸漬し、次いで塩化パラジウム２ｇ／ｌ溶液に４０℃５
分間浸漬したのち、白金の無電解メツキとしてＥＥＪＡ
社製レクトしレスｐｔメツキ溶液（Ｐ ｔ ２ ｇ／ｌ
）を用い無電解メツキ時間を４５分間して白金薄膜３μ
ｍの厚みを形成した。(Example 2) Ceramic substrate (10 mm x I Omm x thickness 0.6
Apply photoresist to the surface (mm) and dry to form a film,
After photolithography, a reverse pattern of the platinum resistance heating element circuit was drawn with photoresist, and as a pretreatment, ultrasonic degreasing was performed at 60°C using electrolytic degreasing liquid (Eedrex 12 manufactured by EEJA).
minutes, then immersed in a stannous chloride lOg/l solution for 5 minutes, and then immersed in a palladium chloride 2g/l solution at 40°C.
After soaking for a minute, use EEJA as electroless plating for platinum.
Rect Shires pt plating solution (P t 2 g/l
) and electroless plating time of 45 minutes to form a platinum thin film of 3 μm.
A thickness of m was formed.
次いでレジストは（すして、洗浄し、乾燥したのち、電
気炉中で５００℃で３０分間熱処理したしたのち、回路
（幅０．４ｍｍＸ長さ８５ｍｍ）の抵抗値を測定したと
ころ２１オームであった。Next, the resist was rinsed, washed, dried, and then heat treated in an electric furnace at 500°C for 30 minutes.The resistance of the circuit (width 0.4 mm x length 85 mm) was measured and found to be 21 ohms. .
なお、実施例２の方法では細かい回路の場合には線幅の
バラツキ、および厚みのバラツキが実施例１の方法より
やや大きくなる点がある。Note that in the method of the second embodiment, in the case of a fine circuit, the variation in line width and the variation in thickness are slightly larger than the method in the first embodiment.
また実施例１における白金抵抗発熱体回路形成は、ホト
エツチングの後に熱処理が行われているが、本発明はこ
れに限るものではなく、熱処理の後に白金をホトエツチ
ングしてもよいものである。Further, in the formation of the platinum resistance heating element circuit in Example 1, heat treatment is performed after photoetching, but the present invention is not limited to this, and platinum may be photoetched after heat treatment.
（発明の効果）
以上に説明したように、本発明の製造方法によれば、従
来法では得られなかった電気伝導率が白金バルクに近似
して白金抵抗発熱体回路を形成して用いた場合でも長期
に安定した抵抗値を得られるもので、また白金の使用量
も約１／２〜１／３に減少させることができ効果大なる
ものと言える。(Effects of the Invention) As explained above, according to the manufacturing method of the present invention, when a platinum resistance heating element circuit is formed and used, the electrical conductivity approximates that of bulk platinum, which could not be obtained with the conventional method. However, it is possible to obtain a stable resistance value over a long period of time, and the amount of platinum used can be reduced to about 1/2 to 1/3, so it can be said to be highly effective.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
トを用いて形成する白金抵抗発熱体の製造方法において
、白金抵抗発熱体回路形成が無電解白金メッキエ程と、
４５０〜６００℃で熱処理する工程とから成ることを特
徴とする白金抵抗発熱体の製造方法。(1) In a method for manufacturing a platinum resistance heating element in which a platinum resistance heating element circuit is formed on a heat-resistant base material using a photoresist, the formation of the platinum resistance heating element circuit is performed by an electroless platinum plating process;
A method for manufacturing a platinum resistance heating element, comprising a step of heat treatment at 450 to 600°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14933090A JPH0443586A (en) | 1990-06-07 | 1990-06-07 | Manufacture of platinum resistance heater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14933090A JPH0443586A (en) | 1990-06-07 | 1990-06-07 | Manufacture of platinum resistance heater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0443586A true JPH0443586A (en) | 1992-02-13 |
Family
ID=15472753
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14933090A Pending JPH0443586A (en) | 1990-06-07 | 1990-06-07 | Manufacture of platinum resistance heater |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0443586A (en) |
-
1990
- 1990-06-07 JP JP14933090A patent/JPH0443586A/en active Pending
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