JP2941495B2 - Molded body for thermal history detection - Google Patents

Molded body for thermal history detection

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Publication number
JP2941495B2
JP2941495B2 JP3154893A JP15489391A JP2941495B2 JP 2941495 B2 JP2941495 B2 JP 2941495B2 JP 3154893 A JP3154893 A JP 3154893A JP 15489391 A JP15489391 A JP 15489391A JP 2941495 B2 JP2941495 B2 JP 2941495B2
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JP
Japan
Prior art keywords
molded body
firing
temperature
weight
present
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
Application number
JP3154893A
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Japanese (ja)
Other versions
JPH051955A (en
Inventor
憲一 清水
潤一郎 川野
幸一 馬込
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kyocera Corp
Original Assignee
Kyocera Corp
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Filing date
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Priority to JP3154893A priority Critical patent/JP2941495B2/en
Publication of JPH051955A publication Critical patent/JPH051955A/en
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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、セラミックスなどの焼
成工程における熱履歴を検知するためのものであり、特
にガラスセラミック、陶器、ステアタイト、釉薬焼き付
け等の、800〜1300℃の温度域の焼成における熱
履歴検知用成形体に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is for detecting a heat history in a firing process for ceramics or the like, and particularly for a temperature range of 800 to 1300 DEG C., such as glass ceramics, pottery, steatite, and glaze baking. The present invention relates to a molded body for detecting heat history in firing.

【0002】[0002]

【従来の技術】セラミックスの焼成工程において、温度
プロファイル、焼成炉の種類、炉内のセッティング等に
よって被焼成体の受ける熱履歴は変化する。即ち、焼成
温度が同じでも他の条件が異なれば熱履歴は異なること
となり、この熱履歴を正しく検知する必要があった。
2. Description of the Related Art In the process of firing ceramics, the thermal history of the object to be fired changes depending on the temperature profile, the type of firing furnace, the settings in the furnace, and the like. That is, even if the firing temperature is the same, if other conditions are different, the thermal history will be different, and it is necessary to correctly detect the thermal history.

【0003】例えば、実開昭56−29441号公報な
どに示されているゼーゲルコーンを用いて被焼成体の熱
履歴を検知することが行われていた。ゼーゲルコーンと
は、溶倒温度の異なる複数の三角錐状体を支持台上に備
えたものであり、このゼーゲルコーンを被焼成体と共に
焼成した後、各三角錐状体の倒れ方によって、熱履歴を
検知するようになっていた。しかし、これでは正確な検
知ができないことから、現在では使用されることが少な
くなっている。
For example, the thermal history of a body to be fired has been detected using a Zegel cone disclosed in Japanese Utility Model Application Laid-Open No. 56-29441. A Zegel cone is one in which a plurality of triangular pyramids having different melting temperatures are provided on a support base.After firing this Zegel cone together with the object to be calcined, the thermal history is determined by the manner in which each triangular pyramid falls. Was to be detected. However, since accurate detection is not possible with this, it is rarely used at present.

【0004】そこで、例えば特開平1−184388号
公報等に示されているように、セラミックスの未焼成成
形体を用いて、この成形体を被焼成体と共に焼成した
後、収縮による寸法変化を測定することによって、熱履
歴を検知することが行われていた。例えば、図3に示す
ようなリング状の成形体20、あるいは図4に示すよう
なシート状の成形体30が用いられていた。
Therefore, as shown in, for example, Japanese Patent Application Laid-Open No. 1-184388, a green compact of ceramics is used, and the green compact is fired together with a body to be fired. By doing so, the thermal history has been detected. For example, a ring-shaped molded body 20 as shown in FIG. 3 or a sheet-shaped molded body 30 as shown in FIG. 4 has been used.

【0005】なお、このような焼成収縮による寸法変化
を測定する場合、寸法変化は便宜的に温度に変換される
が、この温度は実温を測定したものではなく、熱履歴を
表すものであって、本発明では指示温度と呼ぶこととす
る。
When such a dimensional change due to firing shrinkage is measured, the dimensional change is conveniently converted to a temperature. However, this temperature is not a measurement of the actual temperature, but a thermal history. Therefore, in the present invention, it is referred to as an indicated temperature.

【0006】[0006]

【発明が解決しようとする課題】ところが、上記の熱履
歴検知用セラミックス成形体は、Al2 3 −Si
2 、またはSiO2 −MgO系を主成分とし、多量の
不純物を含む天然原料からなるものであったため、焼成
収縮率にバラツキがあり、検知された指示温度の精度が
悪かった。また、1100℃以下の比較的低温の焼成で
は、収縮しないために利用できないという問題点があっ
た。
However, the above ceramic molded body for detecting thermal history is made of Al 2 O 3 —Si.
Since it was made of a natural raw material containing O 2 or SiO 2 —MgO as a main component and containing a large amount of impurities, the firing shrinkage ratio varied, and the accuracy of the detected indicated temperature was poor. In addition, there is a problem that firing at a relatively low temperature of 1100 ° C. or less cannot be used because it does not shrink.

【0007】さらに、図2に示すリング状のものでは、
面積が大きいため、焼成炉内で広いスペースを必要と
し、図3に示すシート状のものでは、ソリが発生して正
しく寸法を測定できないなどの問題点があった。
Further, in the ring-shaped one shown in FIG.
Since the area is large, a large space is required in the firing furnace, and the sheet-shaped one shown in FIG. 3 has a problem that warpage occurs and dimensions cannot be measured correctly.

【0008】[0008]

【課題を解決するための手段】そこで本発明は、SiO
2 −MgO−CaOの三成分組成図におけるSiO2
0〜65重量%、MgO0〜25重量%、CaO10〜
60重量%の範囲内の組成をもったセラミックス未焼成
成形体を熱履歴検知用成形体としたものである。
SUMMARY OF THE INVENTION Accordingly, the present invention provides a method of forming
SiO 2 4 in the ternary composition diagram of 2- MgO—CaO
0 to 65% by weight, MgO 0 to 25% by weight, CaO 10
The unfired ceramic compact having a composition within the range of 60% by weight was used as a thermal history detecting compact.

【0009】本発明において、SiO2 を40〜65重
量%としたのは、SiO2 が65重量%より多いか、4
0重量%より少ない場合は1300℃でほとんど収縮し
ないためである。また、MgOを0〜25重量%とした
のは、MgOが25重量%より多いと1300℃でほと
んど収縮しないためである。なお、本発明においてMg
Oは必須成分ではないが、好ましくは5〜25重量%の
範囲で含んでいた方がよい。そして、残部が10〜60
重量%のCaOからなっているが、この他の成分を微量
に含んでいてもよい。また、上記SiO2 、MgO、C
aOは、酸化物だけでなく、水酸化物、炭酸塩などの化
合物の形でもよい。
[0009] In the present invention, to that of SiO 2 and 40 to 65 wt%, or SiO 2 is more than 65 wt%, 4
If the amount is less than 0% by weight, it hardly shrinks at 1300 ° C. The reason why MgO is set to 0 to 25% by weight is that if MgO is more than 25% by weight, it hardly shrinks at 1300 ° C. In the present invention, Mg
O is not an essential component, but is preferably contained in the range of 5 to 25% by weight. And the rest is 10-60
Although it is composed of CaO by weight%, other components may be contained in trace amounts. In addition, the above SiO 2 , MgO, C
aO may be in the form of compounds such as hydroxides and carbonates as well as oxides.

【0010】[0010]

【実施例】以下本発明の実施例を説明する。Embodiments of the present invention will be described below.

【0011】図1(a)(b)に示すように、本発明の
熱履歴検知用成形体10は、円板体に平行な弦部12、
12を形成したものであり、残された円弧部は優れた真
円度の測定面11、11としてある。また、表裏を区別
するためのドットあるいはアルファベットなどの刻印に
よる凹部13が片面に形成され、上下面の角部には面取
り14が施されている。
As shown in FIGS. 1 (a) and 1 (b), a heat history detecting molded body 10 of the present invention has a chord portion 12 parallel to a disk body.
12 are formed, and the remaining arc portions are measurement surfaces 11 and 11 having excellent roundness. In addition, a concave portion 13 is formed on one side by engraving such as a dot or an alphabet for distinguishing the front and back sides, and a chamfer 14 is formed on the corners of the upper and lower surfaces.

【0012】さらに、この成形体10は、図2のSiO
2 −MgO−CaO三成分組成図に示すように、SiO
2 40〜65重量%、MgO0〜25重量%、CaO1
0〜60重量%の範囲内の組成からなっており、原料粉
末の粒系、成形体の生密度などを極めて厳密に管理し、
プレス成形してなる、未焼成成形体である。そして、後
述するように、ある条件の下で焼成温度を変化させて、
この成形体10の焼成後の寸法を測定し、寸法と焼成温
度の関係を換算表として用意しておく。その後、異なる
条件で焼成を行う際に、被焼成体と共にこの成形体10
を焼成し、焼成後の寸法変化を測定することによって、
上記換算表より指示温度を求めることができる。
Further, the molded body 10 is made of SiO 2 shown in FIG.
As shown in the 2- MgO-CaO ternary composition diagram, SiO 2
2 40-65 wt%, MgO0-25 wt%, CaO1
It has a composition within the range of 0 to 60% by weight, and controls the grain system of the raw material powder, the green density of the molded body, etc. very strictly,
It is a green compact formed by press molding. And, as described later, by changing the firing temperature under certain conditions,
The dimensions of the molded body 10 after firing are measured, and the relationship between the dimensions and the firing temperature is prepared as a conversion table. Thereafter, when firing is performed under different conditions, the molded body 10 is fired together with the fired body.
By firing and measuring the dimensional change after firing,
The indicated temperature can be obtained from the above conversion table.

【0013】なお、前記したように、この指示温度と
は、実際の温度ではなく、熱履歴を便宜的に表したもの
である。即ち、本発明の熱履歴検知用成形体を用いれ
ば、焼成条件が異なる場合でも、指示温度を求めること
によって、熱履歴自体を管理することが可能となる。
As described above, the indicated temperature is not an actual temperature but a heat history for convenience. That is, by using the heat history detecting molded body of the present invention, even when firing conditions are different, it is possible to manage the heat history itself by obtaining the indicated temperature.

【0014】また、本発明の成形体は、さまざまな焼成
雰囲気の下で使用できるが、被酸化性雰囲気で使用する
場合は、仮焼して脱バインダーを行った方がよい。
Although the molded article of the present invention can be used in various firing atmospheres, when it is used in an oxidizing atmosphere, it is better to calcine and remove the binder.

【0015】さらに、本発明の成形体10は、弦部1
2、12をもっていることから、図2に示した従来例に
比べて面積が小さく、焼成炉内で大きなスペースを必要
としない。なお、この弦部12、12は互いに平行でな
くてもよく、一ヶ所のみに形成してもよい。さらに、本
発明の成形体10は、3〜10mm程度の肉厚をもった
プレス成形品であるからソリなどが生じることはなく、
また寸法測定時には図1(a)に示すように、円弧をし
た測定面11、11間を低定圧マイクロメータで測定す
ればよく、測定位置がずれても同じ直径Dを正確に測定
できる。
Further, the molded body 10 of the present invention has the chord 1
2 and 12, the area is smaller than that of the conventional example shown in FIG. 2, and a large space is not required in the firing furnace. Note that the chords 12 and 12 need not be parallel to each other, and may be formed only at one location. Furthermore, since the molded body 10 of the present invention is a press-molded article having a thickness of about 3 to 10 mm, no warpage or the like occurs,
Further, at the time of dimension measurement, as shown in FIG. 1 (a), it is only necessary to measure between the arc-shaped measurement surfaces 11, 11 with a low constant-pressure micrometer, and the same diameter D can be accurately measured even if the measurement position is shifted.

【0016】また、本発明の成形体10の形状について
は、密度が均一となるような単純な形状であれば、さま
ざまなものとすることができる。
The shape of the molded body 10 of the present invention can be various as long as it is a simple shape having a uniform density.

【0017】実施例1 精製したSiO2 、MgO、CaO原料を使用して表1
および図2に示す組成とし、アルミナボールにより湿式
粉砕し、レーザー光散乱法による粒度分析を行って、平
均粒径2.0±0.1μmの範囲とする。この原料粉末
に6重量%のワックス系バインダーを添加混合し、噴霧
乾燥することによって、流動性の良い顆粒を得る。この
顆粒を、空調された成形室にて、図1(a)(b)に示
す形状にプレス成形するが、このとき成形体の生密度を
1.900±0.005g/cm3 の範囲内として、本
発明の熱履歴検知用成形体を得た。
Example 1 Using purified SiO 2 , MgO and CaO raw materials, Table 1
The composition shown in FIG. 2 is wet-pulverized with an alumina ball, and subjected to particle size analysis by a laser light scattering method, so that the average particle diameter is in a range of 2.0 ± 0.1 μm. A 6% by weight wax-based binder is added to the raw material powder, mixed and spray-dried to obtain granules having good fluidity. The granules are press-molded in an air-conditioned molding chamber into the shape shown in FIGS. 1 (a) and 1 (b). At this time, the green density of the compact is within the range of 1.900 ± 0.005 g / cm 3 . As a result, a molded article for detecting heat history of the present invention was obtained.

【0018】これらの成形体を、800℃で2時間、1
000℃で2時間、1300℃で2時間の3種類の条件
で焼成した。結果は表2に示す通りである。
These compacts are treated at 800 ° C. for 2 hours,
Firing was performed under three conditions of 2 hours at 000 ° C. and 2 hours at 1300 ° C. The results are as shown in Table 2.

【0019】[0019]

【表1】 [Table 1]

【0020】[0020]

【表2】 [Table 2]

【0021】表1、表2より明らかに、SiO2 が65
重量%を超えたNo.7、40重量%未満のNo.9、
MgOが25重量%を超えたNo.8は、1000℃で
はほとんど収縮せず、1300℃でもわずかに収縮する
程度であるため、目的とする温度範囲での使用には適さ
なかった。
As is clear from Tables 1 and 2, SiO 2 is 65
No. exceeding 10% by weight. 7, No. less than 40% by weight. 9,
In the case of No. 2 containing MgO exceeding 25% by weight. Sample No. 8 hardly shrinks at 1000 ° C. and shrinks slightly even at 1300 ° C., and thus was not suitable for use in a target temperature range.

【0022】これに対し、No.1〜6の本発明実施例
では、その収縮過程が800〜1300℃の範囲内にあ
ることがわかった。例えば、No.1は800〜100
0℃、No.4は900〜1150℃の温度範囲におい
て適している。
On the other hand, no. In Examples 1 to 6 of the present invention, it was found that the shrinkage process was in the range of 800 to 1300 ° C. For example, no. 1 is 800-100
0 ° C., No. 4 is suitable in the temperature range of 900 to 1150 ° C.

【0023】実験例2 実験例1と全く同様にして、表1中No.4の組成で、
直径Dが22.300mmの熱履歴検知用成形体10を
用意した。この成形体10を厳密に管理校正された焼成
炉を用いて、酸化雰囲気にて、昇温速度200℃/時、
最高焼成温度で2時間保持、降温速度300℃/時とし
て焼成し、350℃で1時間脱脂した。焼成後の成形体
10の寸法を、20℃にて低定圧マイクロメータで測定
した。
Experimental Example 2 In the same manner as in Experimental Example 1, Table 1 With the composition of 4,
A heat history detecting molded body 10 having a diameter D of 22.300 mm was prepared. The molded body 10 was heated in an oxidizing atmosphere at a rate of 200 ° C./hour in a sintering furnace strictly controlled and calibrated.
It was held at the highest firing temperature for 2 hours, fired at a temperature lowering rate of 300 ° C./hour, and degreased at 350 ° C. for 1 hour. The dimensions of the molded body 10 after firing were measured at 20 ° C. with a low constant pressure micrometer.

【0024】焼成温度(指示温度)をさまざまに変化さ
せて、それぞれ20個の成形体10の焼成の焼成を3回
繰り返して行った。この結果は、表3および図5に示す
通りである。
The firing temperature (indicated temperature) was changed variously, and firing of the 20 compacts 10 was repeated three times. The results are as shown in Table 3 and FIG.

【0025】また、各温度における、寸法のばらつき
(3σ)と、その温度での1℃当たりの寸法変化量(接
線の傾き)から、指示温度の検知精度=±寸法のばらつ
き/1℃当たりの寸法変化量により、指示温度の検知精
度(3σ)を算出した。結果は、表3に示す通り、90
0〜1150℃の範囲内で、指示温度の検知精度を±2
℃以内とすることができた。
Further, from the dimensional variation (3σ) at each temperature and the dimensional change per 1 ° C. (tangential slope) at that temperature, the detection accuracy of the indicated temperature = ± the dimensional variation / per 1 ° C. The detection accuracy (3σ) of the indicated temperature was calculated from the dimensional change amount. The results are as shown in Table 3, 90
Within the range of 0 to 1150 ° C, the detection accuracy of the indicated temperature is ± 2.
It could be within ° C.

【0026】さらに、表3では指示温度50℃ごとの成
形体の寸法を示しているが、もっと細かな指示温度ごと
の寸法を測定しておくことによって、成形体の寸法と指
示温度の換算表とすることができる。
Further, Table 3 shows the dimensions of the compact at each indicated temperature of 50 ° C. By measuring the dimensions at each designated temperature more finely, a conversion table of the dimensions of the compact and the designated temperature is obtained. It can be.

【0027】[0027]

【表3】 [Table 3]

【0028】また、上記実施例では、熱履歴検知用成形
体10を得るために、原料の粒径2.0±0.1μm、
成形体の生密度1.900±0.005g/cm3 とし
たが、いずれもこの値に限定されるものではなく、さま
ざまに変化させることができる。通常、粒径については
±0.2μmで管理し、生密度については±0.01g
/cm3 の範囲内にバラツキを押さえれば、指示温度の
検知精度を±2℃とすることが可能であった。
In the above embodiment, in order to obtain the heat history detecting molded body 10, the raw material has a particle size of 2.0 ± 0.1 μm.
Although the green density of the molded body was 1.900 ± 0.005 g / cm 3 , none of these values is limited to this value, and various changes can be made. Usually, the particle size is controlled at ± 0.2 μm, and the green density is ± 0.01 g
/ Cm 3 , the detection accuracy of the indicated temperature could be made ± 2 ° C.

【0029】[0029]

【発明の効果】このように本発明によれば、SiO2
MgO−CaOの三成分組成図におけるSiO2 40〜
65重量%、MgO0〜25重量%、CaO10〜60
重量%の範囲内の組成をもったセラミックス未焼成成形
体を熱履歴検知用成形体としたことによって、指示温度
の測定精度を±2℃以内と極めて高精度にできることか
ら、焼成条件が変わっても焼成工程を厳密に管理するこ
とができ、優れた焼結体を得ることが可能となる。ま
た、特に1100℃以下の比較的低温での焼成管理を可
能とすることができる。
As described above, according to the present invention, SiO 2-
SiO 2 40 to the ternary composition diagram of the MgO-CaO
65% by weight, MgO 0 to 25% by weight, CaO 10 to 60
By changing the unfired ceramic molded body having a composition within the range of weight% to a thermal history detection molded body, the measurement accuracy of the indicated temperature can be made extremely high within ± 2 ° C. Also, the firing step can be strictly controlled, and an excellent sintered body can be obtained. In addition, it is possible to control the firing at a relatively low temperature of 1100 ° C. or less.

【図面の簡単な説明】[Brief description of the drawings]

【図1】(a)は本発明実施例の熱履歴検知用成形体を
示す平面図、(b)は同図(a)中のX−X線断面図で
ある。
FIG. 1A is a plan view showing a heat history detecting molded body according to an embodiment of the present invention, and FIG. 1B is a cross-sectional view taken along line XX in FIG. 1A.

【図2】本発明の熱履歴検知用成形体の組成範囲を示す
三成分組成図である。
FIG. 2 is a three-component composition diagram showing a composition range of a molded article for heat history detection of the present invention.

【図3】従来の熱履歴検知用成形体を示す斜視図であ
る。
FIG. 3 is a perspective view showing a conventional heat history detecting molded body.

【図4】従来の熱履歴検知用成形体を示す斜視図であ
る。
FIG. 4 is a perspective view showing a conventional heat history detecting molded body.

【図5】本発明の熱履歴検知用成形体における、焼成収
縮率と指示温度の関係を示すグラフである。
FIG. 5 is a graph showing the relationship between the firing shrinkage and the indicated temperature in the molded article for heat history detection of the present invention.

【符号の説明】[Explanation of symbols]

10・・・熱履歴検知用成形体 11・・・測定面 12・・・弦部 13・・・凹部 14・・・面取り DESCRIPTION OF SYMBOLS 10 ... Heat history detection molded body 11 ... Measurement surface 12 ... String part 13 ... Depression 14 ... Chamfer

───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平1−184388(JP,A) 特開 昭58−118928(JP,A) 特開 昭63−217240(JP,A) 特開 平4−110738(JP,A) 特開 平4−65369(JP,A) 実開 昭56−29441(JP,U) 実開 昭62−30131(JP,U) (58)調査した分野(Int.Cl.6,DB名) G01K 11/00 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-1-184388 (JP, A) JP-A-58-118928 (JP, A) JP-A-63-217240 (JP, A) JP-A-4- 110738 (JP, A) JP-A-4-65369 (JP, A) JP-A-56-29441 (JP, U) JP-A-62-30131 (JP, U) (58) Fields investigated (Int. 6 , DB name) G01K 11/00

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】SiO2 −MgO−CaOの三成分組成図
におけるSiO2 40〜65重量%、MgO0〜25重
量%、CaO10〜60重量%の範囲内の組成をもった
セラミックス未焼成成形体からなることを特徴とする熱
履歴検知用成形体。
1. A ceramic green compact having a composition in the range of 40 to 65% by weight of SiO 2 , 0 to 25% by weight of MgO and 10 to 60% by weight of CaO in a three-component composition diagram of SiO 2 —MgO—CaO. A molded article for detecting heat history, comprising:
JP3154893A 1991-06-26 1991-06-26 Molded body for thermal history detection Expired - Lifetime JP2941495B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3154893A JP2941495B2 (en) 1991-06-26 1991-06-26 Molded body for thermal history detection

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3154893A JP2941495B2 (en) 1991-06-26 1991-06-26 Molded body for thermal history detection

Publications (2)

Publication Number Publication Date
JPH051955A JPH051955A (en) 1993-01-08
JP2941495B2 true JP2941495B2 (en) 1999-08-25

Family

ID=15594261

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3154893A Expired - Lifetime JP2941495B2 (en) 1991-06-26 1991-06-26 Molded body for thermal history detection

Country Status (1)

Country Link
JP (1) JP2941495B2 (en)

Also Published As

Publication number Publication date
JPH051955A (en) 1993-01-08

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