JPH03218965A - Production of barium titanate-based semiconductor porcelain - Google Patents
Production of barium titanate-based semiconductor porcelainInfo
- Publication number
- JPH03218965A JPH03218965A JP2012156A JP1215690A JPH03218965A JP H03218965 A JPH03218965 A JP H03218965A JP 2012156 A JP2012156 A JP 2012156A JP 1215690 A JP1215690 A JP 1215690A JP H03218965 A JPH03218965 A JP H03218965A
- Authority
- JP
- Japan
- Prior art keywords
- semiconductor porcelain
- atmosphere
- barium titanate
- temp
- based semiconductor
- 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
- 239000004065 semiconductor Substances 0.000 title claims abstract description 44
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 32
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000010304 firing Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 description 2
- 239000010956 nickel silver Substances 0.000 description 2
- -1 oxygen ions Chemical class 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910000807 Ga alloy Inorganic materials 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QTJOIXXDCCFVFV-UHFFFAOYSA-N [Li].[O] Chemical compound [Li].[O] QTJOIXXDCCFVFV-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Apparatuses And Processes For Manufacturing Resistors (AREA)
- Thermistors And Varistors (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はチタン酸バリウム系半導体磁器の製造方法に関
する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for manufacturing barium titanate-based semiconductor ceramics.
（従来の技術）
一般に、チタン酸ノ＼リウム系半導体磁器を製造する場
合、チタン酸バリウム系半導体磁器用の原料粉末を所定
形状に成形し、これを所定の条件下で焼成することが行
われているが、任意の比抵抗をもつ焼結体を得ようとす
る場合、焼成時の昇温速度、焼成温度、保持時間、降温
速度、雰囲気等の種々の条件を目的に応じて設定して焼
成することが行われている。(Prior art) Generally, when manufacturing norium titanate-based semiconductor porcelain, raw material powder for barium titanate-based semiconductor porcelain is formed into a predetermined shape, and then fired under predetermined conditions. However, when trying to obtain a sintered body with a desired resistivity, various conditions such as heating rate during firing, firing temperature, holding time, cooling rate, atmosphere, etc. must be set according to the purpose. Baking is being done.
（発明が解決しようとする課題）
しかしながら、チタン酸バリウム系半導体磁器を大量生
産する場合、目的とする比抵抗が異なるロフト毎に、焼
成時の前記諸条件を設定しなおさなければならず、生産
性が低下するという問題があった。また、比抵抗を調整
する手段として、焼成諷度や保持時間等を変えることが
行われてはいるが、この方法では任意の比抵抗をもつ半
導体磁器は得られても、異常粒成長等を生じ、耐破壊電
圧、負荷試験等のレベルの低下を招いているのが現状で
ある。(Problem to be Solved by the Invention) However, when mass producing barium titanate-based semiconductor porcelain, the above-mentioned conditions during firing must be reset for each loft with a different target resistivity. There was a problem of decreased sex. In addition, as a means of adjusting resistivity, changing the firing degree, holding time, etc. has been used, but although this method can produce semiconductor porcelain with a desired resistivity, it may cause abnormal grain growth, etc. The current situation is that this has resulted in a decline in the breakdown voltage, load test, etc.
これらの問題を解決する手段としては、半導体磁器の組
成変更や粉砕度合の変更等を採用し得るが、原料ロフト
が増加し、結局、生産性が低下するという問題かあった
。As a means to solve these problems, it is possible to adopt changes in the composition of the semiconductor porcelain, changes in the degree of grinding, etc., but this increases the raw material loft, resulting in a decrease in productivity.
従って、本発明は、任意の比抵抗を有するチタン酸バリ
ウム系半導体磁器を容易に、かつ、効率良く生産できる
ようにすることを技術的課題とするものである。Therefore, the technical object of the present invention is to enable easy and efficient production of barium titanate-based semiconductor ceramics having any specific resistance.
（課題を解決するための手段）
本発明は、これらの課題を解決するため、予め自然雰囲
気中で焼成して低抵抗の半導体磁器を調製しておき、こ
れを前記自然雰囲気よりも酸素分圧が大きい酸素リッチ
ガス雰囲気中その焼成時の温度またはそれより低い温度
で短時間熱処理し、比抵抗をコントロールするようにし
たものである。(Means for Solving the Problems) In order to solve these problems, the present invention prepares a low-resistance semiconductor porcelain by firing it in a natural atmosphere in advance, and then bakes it in an oxygen partial pressure lower than that in the natural atmosphere. The resistivity is controlled by heat treatment for a short time at the firing temperature or a lower temperature in an oxygen-rich gas atmosphere with a large oxygen content.
即ち、本発明の要旨は、チタン酸バリウム系半導体磁器
用の原料粉末を所定形状に成形し、これを自然雰囲気中
で焼成して低比抵抗の半導体磁器素体と成し、次いで、
前記自然雰囲気よりも酸素分圧が大きい酸素リッチガス
雰囲気中、１１００゜Ｃ前記焼成時の温度以下の温度で
熱処理することを特徴とするチタン酸バリウム系半導体
磁器の製造方法にある。That is, the gist of the present invention is to form raw material powder for barium titanate-based semiconductor porcelain into a predetermined shape, sinter it in a natural atmosphere to form a semiconductor porcelain body with low resistivity, and then:
A method for manufacturing barium titanate-based semiconductor porcelain, characterized in that heat treatment is carried out at a temperature of 1100°C, which is lower than the firing temperature, in an oxygen-rich gas atmosphere having a higher oxygen partial pressure than the natural atmosphere.
低比抵抗の半導体磁器素体を形成する第一段階での焼成
は、チタン酸バリウム系半導体磁器が焼結する温度、通
常、空気中、１２００〜１４００゜Ｃの温度で１〜５時
間行われる。Firing in the first stage to form a low resistivity semiconductor porcelain body is carried out for 1 to 5 hours at a temperature at which barium titanate semiconductor porcelain is sintered, usually in the air at a temperature of 1200 to 1400°C. .
前記半導体磁器を形成するための第二段階としての熱処
理は、酸素’Ｊ ノチガス雰囲気、即ち、酸素分圧が２
０〜１００ｖｏｌ％の範囲内のガス雰囲気で行なわれる
が、その温度はＩＩ００℃以上で第１段階の焼成温度以
下の温度で行われる。The heat treatment as the second step for forming the semiconductor porcelain is carried out in an oxygen gas atmosphere, that is, an oxygen partial pressure is 2.
It is carried out in a gas atmosphere within the range of 0 to 100 vol %, and the temperature is above II00° C. and below the firing temperature of the first stage.
第２段階の熱処理において、雰囲気の酸素分圧を２０〜
１ ０ ０ ｖｏｌ％の範囲としたのは、第１段階の焼
成時の雰囲気が自然雰囲気で酸素分圧が２０ｖｏｌ％程
度であり、これ以下の酸素分圧の雰囲気中で熱処理を行
なうと、チタン酸バリウム系半導体磁器の比抵抗がさが
るだけではなく、抵抗温度特性まで著し《劣化してしま
うからである。In the second stage of heat treatment, the oxygen partial pressure of the atmosphere is set to 20~
The range of 100 vol% was chosen because the atmosphere during the first step of firing was a natural atmosphere with an oxygen partial pressure of about 20 vol%, and if heat treatment was performed in an atmosphere with an oxygen partial pressure lower than this, titanium This is because not only the resistivity of barium oxide semiconductor ceramics decreases, but also the resistance temperature characteristics deteriorate significantly.
また、第２段階の熱処理の温度を１１００℃以上て第１
段階の焼成温度以下としたのは、１１００゜Ｃ末満て熱
処理を行なうとチタン酸バリウム系半導体磁器の比抵抗
が変化せず、第１段階の焼成温度を越える温度で熱処理
を行なうと異常粒成長が起こり耐破壊電圧特性が劣化す
るからである。In addition, the temperature of the second stage heat treatment was set to 1100°C or higher, and the first stage
The reason for setting the firing temperature below the first stage is that the resistivity of the barium titanate semiconductor porcelain does not change if the heat treatment is performed at a temperature below 1100°C, and abnormal grains may occur if the heat treatment is performed at a temperature exceeding the first stage firing temperature. This is because growth occurs and breakdown voltage characteristics deteriorate.
（作用）
自然雰囲気中で焼成して低比抵抗の半導体磁器素体を作
成した後、■１００°Ｃ以上でその焼成温度以下の温度
で前記自然雰囲気よりも酸素分圧が大きい酸素リッチガ
ス雰囲気中で熱処理すると、焼結体中に酸素イオンが拡
散して酸素イオン欠陥が除去され、粒成長させることな
く半導体磁器の比抵抗をコントロールすることができ、
また、その電気的特性を安定化させる。(Function) After firing in a natural atmosphere to create a low resistivity semiconductor porcelain body, ■ in an oxygen-rich gas atmosphere with a higher oxygen partial pressure than the natural atmosphere at a temperature of 100°C or higher and lower than the firing temperature. When heat treated with , oxygen ions diffuse into the sintered body, oxygen ion defects are removed, and the resistivity of semiconductor porcelain can be controlled without causing grain growth.
It also stabilizes its electrical characteristics.
以下、本発明の実施例について説明する。Examples of the present invention will be described below.
（実施例）
出発原料としてＢａＣＯ．，ＴｉＯ，，ＳｒＣＯｓ，Ｙ
ｔＯｓ，ＣａＣＯｓ．ＭｎＣＯ＠を用い、これらの原料
粉末をそれぞれＢａＯ，ＴｉＯ＊，ＳｒＯ，ＹＯ．ｔ，
ＣａＯ，ＭｎＯに換算して、モル比で０．８９３：１．
０１： ０．０５ ： ０．００３５ ： ０．０５
： ０．００ １２になるように混合し、１１３０℃で
仮焼した後、粉砕し、２０＃のサランメッシュを通して
仮焼粉末を得た。この仮焼粉末に適当な有機パイングー
を加えて混合した後、直径１０＋＋ｍ，厚さ３．６ｎ＋
ｍの円板状の成形体を成形した。(Example) BaCO. , TiO, , SrCOs, Y
tOs, CaCOs. Using MnCO@, these raw material powders were converted to BaO, TiO*, SrO, YO. t,
In terms of CaO and MnO, the molar ratio is 0.893:1.
01: 0.05: 0.0035: 0.05
: 0.00 12, calcined at 1130°C, pulverized, and passed through a 20# Saran mesh to obtain calcined powder. After adding and mixing a suitable organic pine goo to this calcined powder, the powder was made into a powder with a diameter of 10++m and a thickness of 3.6n+.
A disk-shaped molded body of m was molded.
得られた成形体を自然雰囲気中で１２７０’Ｃ〜１３６
０゜Ｃの範囲の温度で１，５時間焼成して、低抵抗の半
導体磁器素体を得た。この半導体磁器素体の抵抗値とそ
のバラッキを調べるため、各素体の両表面にＩｎ−Ｇａ
合金を塗布、乾燥させて電極とし、２０個の試料につい
て抵抗値を測定した結果、平均値Ｒ０−２。８３Ω．３
ＣＶ＝８．６％であった。また、半導体磁器素体と電極
は、完全にオーミック接触していた。The obtained molded body was heated at 1270'C to 136°C in a natural atmosphere.
A low-resistance semiconductor porcelain body was obtained by firing at a temperature in the range of 0°C for 1.5 hours. In order to investigate the resistance value and its dispersion of this semiconductor ceramic element, In-Ga was added to both surfaces of each element.
The alloy was coated and dried to form electrodes, and the resistance values of 20 samples were measured, and the average value was R0-2.83Ω. 3
CV=8.6%. Furthermore, the semiconductor ceramic body and the electrode were in perfect ohmic contact.
次に、この半導体磁器素体を、第１表に示す条件下で、
前記自然雰囲気よりも酸素分圧が大きい酸素リソチガス
雰囲気中で熱処理してチタン酸バリウム系半導体磁器を
得た。なお、表中、＊を付した試料は本発明の範囲外で
あることを示す。Next, this semiconductor ceramic body was processed under the conditions shown in Table 1.
A barium titanate-based semiconductor ceramic was obtained by heat treatment in an oxygen-lithium gas atmosphere having a higher oxygen partial pressure than the natural atmosphere. In addition, in the table, samples marked with * indicate that they are outside the scope of the present invention.
（以 下 余 白）
得られたチタン酸バリウム系半導体磁器の抵抗値とその
バラッキを調べるためため、素体の場合と同様にしてＩ
ｎ−Ｇａ合金電極を形成し、２０個の試料について２５
℃における抵抗値を測定した。その平均値（Ｒ１）とバ
ラッキ３ｃｖを第２表に示す。(Left below) In order to investigate the resistance value and its dispersion of the obtained barium titanate semiconductor porcelain, I
n-Ga alloy electrodes were formed and 25
The resistance value at ℃ was measured. The average value (R1) and variation 3cv are shown in Table 2.
第２表
第２表に示す結果から明らかなように、本発明によれば
、熱処理条件を変えることによって、チタン酸バリウム
系半導体磁器の抵抗を任意にコントロールでき、また、
そのときのバラッキは元の半導体磁器素体よりも低く抑
えることができる。As is clear from the results shown in Table 2, according to the present invention, by changing the heat treatment conditions, the resistance of barium titanate-based semiconductor ceramics can be controlled arbitrarily.
At that time, the variation can be kept lower than that of the original semiconductor porcelain body.
また、この再現性を確認するため、前記半導体磁器素体
を用いて前記の場合と同条件下で熱処理したところ、抵
抗値Ｒ．とそのバラッキの再現性は非常に高いことが確
認された。In order to confirm this reproducibility, the semiconductor ceramic body was heat-treated under the same conditions as in the above case, and the resistance value R. It was confirmed that the reproducibility of the variation was very high.
次に、前記試料番号２，４．６のチタン酸バリウム系半
導体磁器に無電解メッキ法により゛ニッケルメノ牛を形
成し、その上に銀ペイントを塗布したのち６００゜Ｃの
温度で焼き付けてニッケルー銀電極を形成し、負荷寿命
試験、耐電圧試験を行った。それらの結果を第３表に示
す。Next, a nickel plate was formed on the barium titanate semiconductor porcelain of Sample Nos. 2 and 4.6 by electroless plating, and silver paint was applied thereon and baked at a temperature of 600°C to form a nickel-silver plate. Electrodes were formed and subjected to load life tests and withstand voltage tests. The results are shown in Table 3.
なお、低温および高温負荷寿命試験は、それぞれ温度２
５℃，８５゜Ｃ、印加電圧１２５ＶＤ，Ｃ，、試験時間
１０００時間の条件で行い、測定値は試料数１０個につ
いての平均値である。また、耐電圧は、チタン酸バリウ
ム系半導体磁器の両端に直流電圧を印加した場合に絶縁
破壊を起こした値である。Note that the low-temperature and high-temperature load life tests were performed at a temperature of 2.
The test was carried out under the following conditions: 5° C., 85° C., an applied voltage of 125 VD, C, and a test time of 1000 hours, and the measured values are the average values for 10 samples. Further, the withstand voltage is the value at which dielectric breakdown occurs when a DC voltage is applied across the barium titanate semiconductor ceramic.
なお、第３表中、試料番号１０，１１．１２は、仮焼粉
末を成形して得た円板状の成形体をそれぞれ、空気中、
１３００℃で１時間、１３３０℃で１．５時間．１３６
０℃で１．５時間の条件下で焼成してチタン酸バリウム
系半導体磁器を得、これにニッケルー銀電極を同様にし
て形成したものである。In Table 3, sample numbers 10, 11.12 are disk-shaped compacts obtained by compacting calcined powder, respectively, in air.
1 hour at 1300℃, 1.5 hours at 1330℃. 136
Barium titanate-based semiconductor porcelain was obtained by firing at 0° C. for 1.5 hours, and nickel-silver electrodes were formed thereon in the same manner.
（以 下 余 白）
第３表から明らかなように、本発明方法により製造され
たチタン酸バリウム系半導体磁器は、比抵抗が同じでも
従来法により製造されたチタン酸バリウム系半導体磁器
に比べて、耐電圧特性及び負荷寿命が２倍以上と著しく
向上していることが判る。(Left below) As is clear from Table 3, barium titanate-based semiconductor porcelain manufactured by the method of the present invention has a higher resistivity than barium titanate-based semiconductor porcelain manufactured by the conventional method, even if the resistivity is the same. It can be seen that the withstand voltage characteristics and load life are significantly improved by more than double.
（発明の効果）
以上の説明から明らかなように、本発明によれば、半導
体磁器の比抵抗を容易にコントロールできるだけでな《
、その耐破壊電圧、負荷寿命など諸特性を著しく向上さ
せることができる。また、熱処理を焼成温度以下の温度
で短時間で行えるので、工業的利用価値が大きいなど、
優れた効果が得られる。(Effects of the Invention) As is clear from the above explanation, according to the present invention, not only can the resistivity of semiconductor ceramics be easily controlled, but also the specific resistance of semiconductor ceramics can be easily controlled.
, its breakdown voltage, load life, and other characteristics can be significantly improved. In addition, heat treatment can be performed in a short time at a temperature below the firing temperature, so it has great industrial utility value.
Excellent effects can be obtained.
Claims (1)
所定形状に成形し、これを自然雰囲気中で焼成して低比
抵抗の半導体磁器素体と成し、次いで、前記自然雰囲気
よりも酸素分圧が大きい酸素リッチガス雰囲気中、１１
００℃以上前記焼成時の温度以下の温度で熱処理するこ
とを特徴とするチタン酸バリウム系半導体磁器の製造方
法。(1) Raw material powder for barium titanate-based semiconductor porcelain is molded into a predetermined shape and fired in a natural atmosphere to form a semiconductor porcelain body with low resistivity. In a high pressure oxygen rich gas atmosphere, 11
A method for manufacturing barium titanate-based semiconductor porcelain, characterized in that heat treatment is performed at a temperature of 00° C. or higher and lower than the firing temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012156A JP2662740B2 (en) | 1990-01-22 | 1990-01-22 | Method for producing barium titanate-based semiconductor porcelain |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012156A JP2662740B2 (en) | 1990-01-22 | 1990-01-22 | Method for producing barium titanate-based semiconductor porcelain |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03218965A true JPH03218965A (en) | 1991-09-26 |
| JP2662740B2 JP2662740B2 (en) | 1997-10-15 |
Family
ID=11797600
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2012156A Expired - Lifetime JP2662740B2 (en) | 1990-01-22 | 1990-01-22 | Method for producing barium titanate-based semiconductor porcelain |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2662740B2 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4890308A (en) * | 1972-03-06 | 1973-11-26 | ||
| JPS6186467A (en) * | 1984-10-02 | 1986-05-01 | 科学技術庁無機材質研究所長 | Manufacturing method of high performance barium titanate posister |
-
1990
- 1990-01-22 JP JP2012156A patent/JP2662740B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4890308A (en) * | 1972-03-06 | 1973-11-26 | ||
| JPS6186467A (en) * | 1984-10-02 | 1986-05-01 | 科学技術庁無機材質研究所長 | Manufacturing method of high performance barium titanate posister |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2662740B2 (en) | 1997-10-15 |
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