JPS6161687B2 - - Google Patents
Info
- Publication number
- JPS6161687B2 JPS6161687B2 JP55179492A JP17949280A JPS6161687B2 JP S6161687 B2 JPS6161687 B2 JP S6161687B2 JP 55179492 A JP55179492 A JP 55179492A JP 17949280 A JP17949280 A JP 17949280A JP S6161687 B2 JPS6161687 B2 JP S6161687B2
- Authority
- JP
- Japan
- Prior art keywords
- resistor
- firing
- firing container
- insulating film
- gas
- 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
Links
- 238000010304 firing Methods 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 12
- 238000003746 solid phase reaction Methods 0.000 claims description 8
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 7
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 10
- 238000009413 insulation Methods 0.000 description 6
- 239000004593 Epoxy Substances 0.000 description 5
- 229940126214 compound 3 Drugs 0.000 description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 4
- 239000011368 organic material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 2
- -1 Co 2 O 3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Landscapes
- Thermistors And Varistors (AREA)
Description
【発明の詳細な説明】
本発明は電圧非直線抵抗体素子の製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method of manufacturing a voltage nonlinear resistor element.
従来、Znoを主成分とする電圧非直線抵抗体
（以下抵抗体と略する。）の側面絶縁方法は、焼成
後抵抗体側面にエポキシ系有機物を塗布して絶縁
するか、あるいは抵抗体（圧縮成形体）の焼成前
に種々の無機化合物を抵抗体側面に塗布後焼成
し、ガラス質又は結晶質の絶縁被膜を形成させて
絶縁していた。 Conventionally, the side insulation methods for voltage nonlinear resistors (hereinafter abbreviated as resistors) whose main component is ZNO are to coat the sides of the resistor with an epoxy-based organic material after firing, or to insulate the resistor (compressed Before firing the molded body, various inorganic compounds were coated on the side surfaces of the resistor and fired to form a glassy or crystalline insulating film for insulation.
しかし、前者の方法においては、塗布するエポ
キシ系有機物と抵抗体との密着性が悪いため抵抗
体に水分が吸着され、特性劣化が大きく短波尾耐
量も弱くなる欠点がある。又、抵抗体とエポキシ
系有機物との間に熱膨張の差があるため熱衝撃で
エポキシ系有機物にクラツクが入り劣化の原因と
なる欠点がある。又、後者の方法においては、焼
成時に抵抗体と側面絶縁剤との収縮率を一致させ
る必要があり、このため仮焼成してある程度抵抗
体を収縮させた後に側面絶縁剤を塗布して本焼成
し、側面絶縁被膜を形成させている。従つてこの
場合には、焼成を２回に分けて行うこととなり、
燃料（電力を含む。）費が上昇するとともに焼成
装置を２回使用するので製造コストが上昇する欠
点がある。又、両者の方法とも側面絶縁被膜を必
要厚に均一にするためには相当の技術と装置を要
する欠点がある。 However, the former method has the disadvantage that moisture is adsorbed to the resistor due to poor adhesion between the applied epoxy-based organic substance and the resistor, resulting in significant deterioration of characteristics and weakening of short-wave tail resistance. Furthermore, since there is a difference in thermal expansion between the resistor and the epoxy organic material, there is a drawback that the epoxy organic material cracks due to thermal shock, causing deterioration. In addition, in the latter method, it is necessary to match the shrinkage rates of the resistor and the side insulating material during firing, so after pre-firing the resistor to a certain extent, the side insulating material is applied and the main firing is performed. Then, an insulating coating is formed on the side surfaces. Therefore, in this case, the firing will be done in two parts.
This method has disadvantages of increased fuel (including electric power) costs and increased production costs since the firing device is used twice. Furthermore, both methods have the disadvantage that considerable skill and equipment are required to make the side insulating coating uniform to the required thickness.
このため、抵抗体の焼成時に焼成用容器内にア
ンチモン酸化物（Sb2o3等）を配置し、焼成と同
時に気−固相反応により側面絶縁被膜を形成する
方法が提案されており、この方法ではアンチモン
酸化物の蒸気と抵抗体との気−固相反応を利用し
ているため抵抗体と絶縁被膜との密着性が良く、
電流放電耐量、耐コロナ性および耐アーク性等の
電気的諸特性がエポキシ系有機物を塗布した場合
に比べて改善されるとともに、無機化合物を塗布
焼成した場合に比べると収縮率を考慮する必要が
少くなつた。 For this reason, a method has been proposed in which antimony oxide (Sb 2 o 3, etc.) is placed in the firing container during firing of the resistor, and a side insulating film is formed through a gas-solid phase reaction at the same time as the firing. The method utilizes a gas-solid phase reaction between antimony oxide vapor and the resistor, so it has good adhesion between the resistor and the insulating film.
Electrical properties such as current discharge withstand, corona resistance, and arc resistance are improved compared to when epoxy-based organic materials are applied, and shrinkage rate needs to be taken into consideration compared to when inorganic compounds are applied and fired. It has become less.
しかるに焼成容器は気密質材料で形成されてほ
ぼ密閉状態である。一方圧縮成形された抵抗体は
水分や結合剤を含んであるため焼成過程において
これらの有機物が分解してCO2や水蒸気などのガ
スを放出するが、密閉した焼成容器内にあること
によりガスの放出が抑制されるとともに側面絶縁
皮膜の形成により抵抗体内に残留ガスが生じ、抵
抗体の異常膨張により抵抗体の変形や割れ、クラ
ツクの発生、抵抗体と側面絶縁皮膜の密着性の悪
化などを生じる。その一例を第１図ａ，ｂに示
す。又、第２図ａ〜ｉは他の例を示し、この場合
は900℃まで80℃／時間の昇温速度で加熱し、900
℃に３時間保持した後、1200℃まで80℃／時間で
加熱し、1200℃に数時間保持した場合を示す。 However, the firing container is made of an airtight material and is almost sealed. On the other hand, since compression-molded resistors contain moisture and binders, these organic substances decompose during the firing process and release gases such as CO 2 and water vapor. In addition to suppressing emissions, residual gas is generated inside the resistor due to the formation of the side insulating film, and abnormal expansion of the resistor causes deformation, cracking, and deterioration of the adhesion between the resistor and the side insulating film. arise. An example is shown in FIGS. 1a and 1b. In addition, Fig. 2 a to i shows another example, in which heating is performed at a heating rate of 80°C/hour to 900°C.
The case is shown in which the sample was kept at 1200°C for 3 hours, then heated at 80°C/hour to 1200°C, and then kept at 1200°C for several hours.
ａ図は900℃に1.5時間保持した状態、ｂ図は
900℃に３時間保持した状態、ｃ図は950℃の状
態、ｄ図は1000℃、ｅ図は1050℃、ｆ図は1100
℃、ｇ図は1150℃、ｈ図は1200℃の各状態を示
す。又、１図は1200℃に数時間保持した焼成の最
終状態を示し、抵抗体と側面絶縁皮膜がはく離し
ていることが判明する。ことは保持温度を600℃
３時間あるいは800℃３時間に変えても同様であ
つた。このため、気−固相反応により側面絶縁皮
膜を形成する方法においてもやはり抵抗体はあら
かじめ仮焼成してガスの放出を行うことが必要と
なり、二回の焼成によりコストアツプとなつた。 Figure a shows the state held at 900℃ for 1.5 hours, figure b shows the state
After being held at 900℃ for 3 hours, figure c is 950℃, figure d is 1000℃, figure e is 1050℃, figure f is 1100℃.
℃, the g diagram shows the conditions at 1150°C, and the h diagram shows the conditions at 1200°C. Furthermore, Figure 1 shows the final state after firing at 1200°C for several hours, and it is clear that the resistor and the side insulation film have peeled off. The holding temperature is 600℃
The same result was obtained even if the temperature was changed to 3 hours or 800°C for 3 hours. For this reason, even in the method of forming a side insulating film by a gas-solid phase reaction, it is still necessary to pre-fire the resistor to release the gas, and the cost increases due to two firings.
本発明は上記の欠点を除去して、電圧非直線抵
抗体の側面絶縁皮膜をアンチモン酸化物と該抵抗
体との気−固相反応により密着性良くかつ該抵抗
体に変形や割れを生じずに形成することができる
電圧非直線抵抗体の製造方法を提供することを目
的とする。 The present invention eliminates the above-mentioned drawbacks, and forms a side insulating film of a voltage nonlinear resistor with good adhesion through a gas-solid phase reaction between antimony oxide and the resistor, and without causing deformation or cracking of the resistor. It is an object of the present invention to provide a method for manufacturing a voltage nonlinear resistor that can be formed as follows.
以下本発明の実施例を図面とともに説明する。
第３図は焼成装置を示し、抵抗体１はZno91mol
％にSb2o3、Bi2O3、Co2O3、MnO2、Cr2O3、SiO2
などを9mol％加え、さらに水や結合剤を加え、
充分混合した後圧縮成形して適当な形状例えば円
柱状の圧縮成形体とする。２は気密質から成る焼
成容器本体、２ａは焼成容器本体２を密閉する蓋
で、蓋２ａは焼成温度領域で熱的、機械的に安定
でかつ焼成中抵抗体１、化合物３およびこれらの
蒸気と反応しない多孔質により形成する。焼成容
器本体２と蓋２ａにより焼成容器を形成するが、
焼成容器本体２も蓋２ａと同じ多孔質としても良
く、又焼成容器本体２のみ多孔質とし蓋２ａを気
密質としても良い。焼成容器の通気性は本実施例
で２〜３％としたが0.5〜20％（閉気孔も含めた
気孔率５〜40％）でも良い。３は少くともアンモ
チン酸化物（Sb2O3等）を含む化合物で、化合物
３は水を加えてスラリーとし、焼成容器本体２の
内周壁に塗布する。化合物３としてはSb2O3系、
Sb2O3−Bi2O3系、Sb2O3−Bi2O3−SiO2系、
Sb2O3−Bi2O3−SiO2−ZnO系などを用いる。化
合物２は乾燥粉として焼成容器内に収納するだけ
でも良い。４は台座、５は台座４と抵抗体１との
溶着を防ぐための敷粉、６，７は抵抗体１の両端
に設けたしやへい板である。このように抵抗体１
および化合物３を焼成容器本体２内に配置し蓋２
ａで密閉した状態で、1000〜1400℃に加熱する
と、抵抗体１はCO2や水蒸気などのガスを放出す
るとともに800〜1000℃で内部で種々の反応をし
体積比で約40％収縮する。一方、化合物３中のア
ンチモン酸化物は900℃付近で昇華しはじめ1000
℃以上では昇華が非常に活発となる。このため焼
成容器内はアンチモン酸化物の蒸気で満たされ、
該蒸気と抵抗体１内のZnOなどとが気一固相反応
する。この結果、第４図に示すように抵抗体１が
焼成されるとともに抵抗体１の側面に高抵抗の側
面絶縁皮膜８が形成される。側面絶縁皮膜８をＸ
線回折により調べると第５図に示すようになり、
Zn2.33Sb0.67O4（スピネル）が主成分であること
が判明した。Ｘ線マイクロアナライザにより調べ
ても同様であつた。 Embodiments of the present invention will be described below with reference to the drawings.
Figure 3 shows the firing device, and resistor 1 is Zno91mol
% Sb 2 O 3 , Bi 2 O 3 , Co 2 O 3 , MnO 2 , Cr 2 O 3 , SiO 2
Add 9 mol% of etc., further add water and binder,
After thorough mixing, compression molding is performed to obtain a compression molded body having an appropriate shape, for example, a cylindrical shape. 2 is an airtight firing container body; 2a is a lid that seals the firing container body 2; the lid 2a is thermally and mechanically stable in the firing temperature range, and holds the resistor 1, compound 3, and their vapors during firing. It is formed by a porous material that does not react with A firing container is formed by the firing container body 2 and the lid 2a,
The firing container main body 2 may also be porous like the lid 2a, or only the firing container main body 2 may be porous and the lid 2a may be airtight. Although the air permeability of the firing container was set to 2 to 3% in this example, it may be 0.5 to 20% (porosity including closed pores of 5 to 40%). 3 is a compound containing at least ammothine oxide (Sb 2 O 3 etc.), compound 3 is made into a slurry by adding water, and is applied to the inner circumferential wall of the firing container body 2. Compound 3 is Sb 2 O 3 type,
Sb 2 O 3 −Bi 2 O 3 system, Sb 2 O 3 −Bi 2 O 3 −SiO 2 system,
A Sb 2 O 3 −Bi 2 O 3 −SiO 2 −ZnO system or the like is used. Compound 2 may simply be stored in the firing container as a dry powder. 4 is a pedestal, 5 is a pad for preventing welding between the pedestal 4 and the resistor 1, and 6 and 7 are shield plates provided at both ends of the resistor 1. In this way, resistor 1
and Compound 3 are placed inside the firing container body 2, and the lid 2 is placed inside the firing container body 2.
When heated to 1000 to 1400℃ in a sealed state, resistor 1 releases gases such as CO 2 and water vapor, and undergoes various internal reactions at 800 to 1000℃, shrinking by about 40% by volume. . On the other hand, antimony oxide in compound 3 begins to sublimate at around 900℃.
Sublimation becomes very active at temperatures above ℃. For this reason, the inside of the firing container is filled with antimony oxide vapor,
The vapor and ZnO in the resistor 1 undergo a gas-solid phase reaction. As a result, as shown in FIG. 4, the resistor 1 is fired and a high-resistance side insulation film 8 is formed on the side surface of the resistor 1. Side insulation film 8
When examined by line diffraction, it is shown in Figure 5,
It was found that Zn 2 . 33 Sb 0 . 67 O 4 (spinel) was the main component. The same result was obtained when examined using an X-ray microanalyzer.
上記実施例においては、焼成容器の蓋２ａを多
孔質材により形成しており、蓋２ａは多少の通気
性を有している。このため、焼成中の抵抗体１か
らのガスの放出が良好となり、抵抗体１中の残留
ガスにより抵抗体１が異常膨張により変形や割れ
を生じたり、クラツクを生じたりすることがな
く、又抵抗体１と側面絶縁皮膜８のはくりなども
生じない。第６図は焼成最終状態における抵抗体
１を示し、何ら異常はない。尚、蒸発物質が多孔
質から成る蓋２ａの気孔に付着しても次回の焼成
時に再び蒸発するので気孔を塞いでガスの放出を
妨げるようなことはない。 In the above embodiment, the lid 2a of the firing container is formed of a porous material, and the lid 2a has some degree of air permeability. For this reason, gas can be released from the resistor 1 during firing, and the resistor 1 will not be deformed, cracked, or cracked due to abnormal expansion due to residual gas in the resistor 1. Peeling of the resistor 1 and the side insulating film 8 does not occur. FIG. 6 shows the resistor 1 in the final state of firing, and there is no abnormality. Incidentally, even if the evaporated substance adheres to the pores of the porous lid 2a, it will evaporate again during the next firing, so it will not block the pores and prevent gas release.
以上のように本発明においては、電圧非直線抵
抗体の焼成時に焼成容器内を抵抗体と少くともア
ンチモン酸化物を含む化合物を収納し、気−固相
反応により抵抗体の側面に絶縁皮膜を形成してお
り、しかも焼成容器の少くとも一部を多孔質材に
より形成している。従つて、焼成容器は多少の通
気性を有しており、焼成時抵抗体内に生じるガス
は良好に放出される。このため、抵抗体は残留ガ
スにより異常膨張して変形や割れを生じたり、ク
ラツクを生じたりすることがなく、又抵抗体と側
面絶縁皮膜の密着性も良好となる。従つて、抵抗
体はあらかじめガスを放出するための仮焼成を必
要とせず（仮焼成すれば密着性をさらに高めるこ
とができるが）、製作が容易となりコストダウン
となる。又、抵抗体と側面絶縁皮膜との密着性が
良好となるために電流放電耐量、耐コロナ性、耐
アーク性などの電気的諸特性が改善される。 As described above, in the present invention, when firing a voltage nonlinear resistor, the resistor and a compound containing at least antimony oxide are stored in the firing container, and an insulating film is formed on the side surface of the resistor by a gas-solid reaction. Moreover, at least a portion of the firing container is formed of a porous material. Therefore, the firing container has some degree of air permeability, and the gas generated inside the resistor during firing can be efficiently released. Therefore, the resistor will not be deformed, cracked, or cracked due to abnormal expansion due to residual gas, and the adhesion between the resistor and the side insulation coating will be good. Therefore, the resistor does not require pre-firing to release gas (although pre-firing can further improve adhesion), making it easier to manufacture and reducing costs. Further, since the adhesion between the resistor and the side insulating film is improved, various electrical properties such as current discharge withstand capacity, corona resistance, and arc resistance are improved.
第１図ａ，ｂは夫々気密質の焼成容器内で気−
固相反応により側面絶縁皮膜を形成した素子の平
面図および正面図、第２図ａ〜ｈは夫々気密質の
焼成容器内で気−固相反応により側面絶縁皮膜を
形成した素子の各昇温過程における正面図、第２
図ｉは同平面図、第３〜６図は本発明に係るもの
で、第３図は焼成装置の断面図、第４図は素子の
断面図、第５図は側面絶縁皮膜のＸ線回折図、第
６図は焼成最終状態における素子の平面図。
１……電圧非直線抵抗体、２……焼成容器本
体、２ａ……蓋、３……化合物、８……側面絶縁
皮膜。
Figures 1a and b are air-filled in an airtight firing container.
A plan view and a front view of an element with a side insulating film formed by a solid phase reaction, and Figures 2a to 2h show respective temperature rises of an element with a side insulating film formed by a gas-solid phase reaction in an airtight firing container. Front view in process, 2nd
Figure i is a plan view of the same, Figures 3 to 6 are related to the present invention, Figure 3 is a cross-sectional view of the firing device, Figure 4 is a cross-sectional view of the element, and Figure 5 is an X-ray diffraction diagram of the side insulating film. FIG. 6 is a plan view of the element in the final state of firing. DESCRIPTION OF SYMBOLS 1... Voltage nonlinear resistor, 2... Baking container main body, 2a... Lid, 3... Compound, 8... Side insulating film.
Claims (1)
焼成容器内に入れて焼成する際に、焼成容器内に
少くともアンチモン酸化物を含む化合物を配置す
るとともに焼成容器の少くとも一部は焼成温度領
域で熱的、機械的に安定で電圧非直線抵抗体、前
記化合物およびこれらの蒸気と反応しない多孔質
物質により形成し、前記焼成と同時に気−固相反
応により電圧非直線抵抗体の側面絶縁被膜を形成
することを特徴とする電圧非直線抵抗体素子の製
造方法。1. When a voltage nonlinear resistor containing zinc oxide as a main component is placed in a firing container and fired, a compound containing at least antimony oxide is placed in the firing container, and at least a portion of the firing container is fired. A voltage non-linear resistor that is thermally and mechanically stable in a temperature range, formed from a porous material that does not react with the above-mentioned compounds and their vapors, and formed by a gas-solid phase reaction at the same time as the above-mentioned firing. A method for manufacturing a voltage nonlinear resistor element, comprising forming an insulating film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55179492A JPS57103301A (en) | 1980-12-18 | 1980-12-18 | Method of producing voltage non-linear resistor element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55179492A JPS57103301A (en) | 1980-12-18 | 1980-12-18 | Method of producing voltage non-linear resistor element |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57103301A JPS57103301A (en) | 1982-06-26 |
| JPS6161687B2 true JPS6161687B2 (en) | 1986-12-26 |
Family
ID=16066765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP55179492A Granted JPS57103301A (en) | 1980-12-18 | 1980-12-18 | Method of producing voltage non-linear resistor element |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57103301A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2543744Y2 (en) * | 1991-03-01 | 1997-08-13 | 東レ株式会社 | Floor material |
| JP5049578B2 (en) * | 2006-12-15 | 2012-10-17 | 株式会社東芝 | Steam turbine |
-
1980
- 1980-12-18 JP JP55179492A patent/JPS57103301A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57103301A (en) | 1982-06-26 |
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