JPH01195685A - Manufacture of ceramic heater - Google Patents
Manufacture of ceramic heaterInfo
- Publication number
- JPH01195685A JPH01195685A JP63019085A JP1908588A JPH01195685A JP H01195685 A JPH01195685 A JP H01195685A JP 63019085 A JP63019085 A JP 63019085A JP 1908588 A JP1908588 A JP 1908588A JP H01195685 A JPH01195685 A JP H01195685A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- sintered
- ceramic heater
- sintering
- group
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 150000004767 nitrides Chemical class 0.000 abstract description 4
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 7
- 230000002706 hydrostatic effect Effects 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 239000004020 conductor Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
Landscapes
- Combustion Methods Of Internal-Combustion Engines (AREA)
- Resistance Heating (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明はセラミックヒータの製造方法に関する。[Detailed description of the invention] (Industrial application field) The present invention relates to a method of manufacturing a ceramic heater.
（従来技術）
セラミックヒータの製造方法には、特公昭６２− ＋
９０３４号公報に示すように、一対のセラミック成形体
でタングステン薄板よりなる発熱抵抗体を挟持し、それ
をホットプレス法により焼結するものが知られている。(Prior art) The method for manufacturing ceramic heaters includes
As shown in Japanese Patent No. 9034, it is known that a heating resistor made of a thin tungsten plate is sandwiched between a pair of ceramic molded bodies and then sintered by a hot pressing method.
この製造方法によれば、焼結時に、ホットプレス法を用
いていることから、セラミック成形体とタングステン薄
板との収縮差に基づくクラックが抑えられることになる
と共に密度が高められることになる。According to this manufacturing method, since a hot press method is used during sintering, cracks due to shrinkage differences between the ceramic molded body and the tungsten thin plate are suppressed, and the density is increased.
（発明が解決しようとする問題点）
しかし、上記製造方法においては、ホットプレス法を用
いることから、セラミック成形体が金型の圧縮力を受け
ることになり、複雑形状のセラミック成形体の場合には
、圧縮力が部分的に異なって作用して、一対のセラミッ
ク成形体が相１にずれ、該一対のセラミック成形体間の
発熱抵抗体が切断される虞れがあった。このため、」１
記セラミックヒータの製造方法におＣづるホットプレス
法においては、一対のセラミック成形体が相互にずれな
いようにするため、（）１純形状のセラミック成形体し
か用いることができず、この結果、−１＋７ｅ方法では
、完成品としてのセラミックヒータは単純形状のものだ
けが対象となっていた。(Problems to be Solved by the Invention) However, in the above manufacturing method, since a hot press method is used, the ceramic molded body is subjected to compressive force from the mold, and in the case of a ceramic molded body with a complicated shape, In this case, there is a possibility that the compressive force acts differently in some parts, causing the pair of ceramic molded bodies to shift to phase 1, and the heating resistor between the pair of ceramic molded bodies to be cut. For this reason, ``1
In the hot press method described in C in the manufacturing method of the ceramic heater, in order to prevent the pair of ceramic molded bodies from shifting from each other, only a ceramic molded body with a pure shape can be used.As a result, In the -1+7e method, only ceramic heaters with simple shapes were targeted as finished products.
本発明はＥ記実情に鑑みてなされたもので、その目的は
、複雑形状のセラミックヒータをも得ることができるセ
ラミックヒータの製造方法を提供することにある。The present invention has been made in view of the actual situation described in E. An object of the present invention is to provide a method for manufacturing a ceramic heater that can also produce a ceramic heater with a complicated shape.
（問題点を解決するための手段、作用）かかる目的を達
成するために本発明にあっては、一対の金属Ｓｉ圧粉成
形体で該一対の金属Ｓｉ圧粉成形体間に金属ＩＶ Ａ若
しくは■Δ族粉ペーストを埋設した被焼結体を、Ｎ２雰
囲気下で焼結して、焼結体に形成し、
前記焼結体に熱間静水圧処理を施す、
ことを特徴とするセラミックヒータの製造方法。(Means and effects for solving the problem) In order to achieve the above object, the present invention provides a pair of metal Si powder compacts, and a metal IV A or ■ A ceramic heater characterized in that a sintered body in which a Δ group powder paste is embedded is sintered in an N2 atmosphere to form a sintered body, and the sintered body is subjected to hot isostatic pressure treatment. manufacturing method.
とした構成としである。This is the configuration.
北述の構成により、焼結時、金属ＩＶ Ａ族若しくはＶ
Ａ族粉ペーストはＮ２と反応して導電性窒化物が生成さ
れる一方、金属Ｓｉ圧粉成形体は、Ｎ２により窒化され
、窒化珪素（ＳｉｆｆＮ＊）系セラミックスが反応焼結
によって得られることになる。このため、手記方法にお
いては、常圧焼結とすることができることになり、ホッ
トプレス法の場合のように、焼結体が単純形状となる制
約を受けることがなくなる。Due to the configuration described above, during sintering, metal IV group A or V
Group A powder paste reacts with N2 to generate conductive nitrides, while metal Si powder compacts are nitrided with N2, and silicon nitride (SiffN*)-based ceramics are obtained by reactive sintering. Become. Therefore, in the manual method, pressureless sintering can be performed, and unlike the hot press method, the sintered body is not restricted to a simple shape.
そして、焼結体は、次の熱間静水圧処理（以下、！＋
Ｉ Ｐ処理）により、焼結体の形状にかかわりなく密度
が上げられることになり、所定性能のセラミックヒータ
とされることになる。この結果、所定性能を維持しつつ
複雑形状のセラミックヒータ夕をも、製造することがで
きることになる。。Then, the sintered body is subjected to the following hot isostatic pressure treatment (hereinafter referred to as !+
IP treatment) increases the density regardless of the shape of the sintered body, resulting in a ceramic heater with a predetermined performance. As a result, it is possible to manufacture a ceramic heater plate having a complicated shape while maintaining a predetermined performance. .
また、Ｎｔを利用した反応焼結とすることができること
から、セラミック成形体ではなくＳｉ成形体を用いるこ
とができることになり、加工度の低く１価なＳｉ粉末原
料を用いることができることになる。Furthermore, since reaction sintering can be performed using Nt, a Si molded body can be used instead of a ceramic molded body, and a monovalent Si powder raw material with a low degree of processing can be used.
（実施例）
以下、本発明の実施例を、第１図、第２図に示すような
円環状のセラミックヒータｌを製造する場合について説
明する。(Example) Hereinafter, an example of the present invention will be described with reference to a case where an annular ceramic heater l as shown in FIGS. 1 and 2 is manufactured.
先ず、第３図、第４図に示すように、円環状の金属Ｓｉ
圧粉成形体（以下、Ｓｉ成形体）２を成形する。このＳ
ｉ成形体２は、例えば、プレス１′Ｅ９００ｋｇ／ｃｍ
２の金属プレス等により形成される。First, as shown in FIGS. 3 and 4, a circular metal Si
A powder compact (hereinafter referred to as a Si compact) 2 is molded. This S
i The molded body 2 is, for example, press 1'E900kg/cm
2. It is formed by a metal press or the like.
次に、金属Ｔｉ粉ペースト３を、第５図、第６図に示す
ようにＳｉ成形体２表面に数度にわたり塗布する。金属
′「ｉ粉ペースト３は。平均粒径５μｍ以ドの金属］゛
ｉｉ粉末チルセルロースを加えて作られたものが用いら
れる。上記金属Ｔｉ粉ペースト３の塗布の厚さβは、例
えばｆｌ、＝１５０μｍとされる。Next, a metal Ti powder paste 3 is applied to the surface of the Si molded body 2 several times as shown in FIGS. 5 and 6. The metal Ti powder paste 3 is made by adding powdered chillulose (metal with an average particle size of 5 μm or less).The coating thickness β of the metal Ti powder paste 3 is, for example, fl , = 150 μm.
次いで、Ｓｉ成形体２に対して別のＳｉ成形体２′を重
ね、再度プレスして第一段目の焼結を行なう。」二記別
のＳｉ成形体２′は金属１゛ｉ粉ペースト：３が収まる
溝部（図示略）を有しており、このＳｉ成形体２′と１
１」記Ｓｉ成形体２と金属Ｔｉ粉ペースト３とが被焼結
体を構成する。焼結は、Ｎ、雰囲気中、例えば１４００
℃、１５０ｈｒの条件の下で行なわれる。これにより、
Ｓｉ成形体２．２′は、Ｎ２によって窒化され、焼結体
として５ｉｚＮａが反応焼結によって得られ、同時に金
属Ｔｉ粉ペースト３のＴｉ扮末もＴｉＮとなってＴｉＮ
導電体層（導電性窒化物）となることになる。また、ペ
ースト成分であるセルロースも一部、カーボンＣとなっ
て残留している。この段階では、焼結層は、気孔率が約
２０％となっており、ＴｉＮが空気中の０２と反応して
酸化され、強度も低くなっている。Next, another Si molded body 2' is stacked on the Si molded body 2 and pressed again to perform the first stage of sintering. The other Si molded body 2' has a groove (not shown) in which the metal 1 powder paste 3 is accommodated, and this Si molded body 2' and 1
1'' The Si molded body 2 and the metal Ti powder paste 3 constitute a body to be sintered. Sintering is carried out in an atmosphere of N, e.g. 1400
C. for 150 hours. This results in
The Si molded body 2.2' is nitrided with N2, and 5izNa is obtained as a sintered body by reaction sintering, and at the same time, the Ti powder of the metal Ti powder paste 3 also turns into TiN.
This will become a conductive layer (conductive nitride). In addition, a portion of cellulose, which is a paste component, remains as carbon C. At this stage, the sintered layer has a porosity of about 20%, TiN reacts with 02 in the air and is oxidized, and its strength is also low.
このため、上記内容を解決するために第二段［］の焼結
としてＨＩ Ｐ処理を行なう。この場合、ガラスカプセ
ル法によって外周面を封じる必要がある。ＨＩ Ｐ処理
は、例えば１６５０℃でｌｈｒ、Ｎ２ガス圧２０００気
圧下で行われる。Therefore, in order to solve the above problem, HIP treatment is performed as the second stage [] of sintering. In this case, it is necessary to seal the outer peripheral surface using a glass capsule method. The HIP process is performed, for example, at 1650° C. for 1 hr under N2 gas pressure of 2000 atm.
この結果、緻密なＳｉ：＋Ｎａの焼結体４が得られると
同時に、ＴｉＮ導電体層５も緻密化され、良好な発熱抵
抗体となった。As a result, a dense Si:+Na sintered body 4 was obtained, and at the same time, the TiN conductor layer 5 was also made dense, resulting in a good heating resistor.
次に、ゴｉＮの端部６を露出させるように切断して抵抗
値を測定した。結果はＲ（２５℃）＝８０ｍΩであった
。なお、ＴｉＮ導電体層５の断面形状は厚さ１００μｍ
、幅４ｍｍで、発熱抵抗体としての長さはＸ線透過にて
約８ｃｍである事を確認した。Next, the GoiN was cut to expose the end portion 6, and the resistance value was measured. The result was R (25°C) = 80 mΩ. Note that the cross-sectional shape of the TiN conductor layer 5 has a thickness of 100 μm.
It was confirmed by X-ray transmission that the width was 4 mm, and the length as a heating resistor was about 8 cm.
次に、このようにして得られたセラミックヒータ１の１
，７温特性を調べた。電源は１２Ｖバツテリを用いた。Next, 1 of the ceramic heater 1 obtained in this way
, 7-temperature characteristics were investigated. A 12V battery was used as the power source.
その結果は第７図に示すように所望のものとなった。The results were as desired as shown in FIG.
以」二天施例について説明したが本発明にあっては、次
のようなものを包含する。Although two embodiments have been described above, the present invention includes the following.
■１”ｉに代えて、■、Ｉ−１ｆ、Ｚ「等ＩＶ Ａ ｌ
疾、ＶＡ族の金属を用いて扮ペーストを作ること。これ
らは、窒化物として導電性を有し、反応焼結時の温度に
て融解しないからである。■Instead of 1”i, ■, I-1f, Z” etc.IV A l
To make a paste using metals from the VA group. This is because these have conductivity as nitrides and do not melt at the temperature during reaction sintering.
■本発明に係るＩｙＪ造方法により、第８図、第９図に
示すように、ディーゼルエンジンにおける渦流室噴［１
部７を形成すること。その場合、Ｓｉ成形体は：３分割
で作り、発熱体層は２層形成することになる。その池、
自動ｉＮエンジンにおける吸気ヒータ、グロープラグ簿
を製造すること。■By the IyJ manufacturing method according to the present invention, as shown in FIGS. 8 and 9, swirl chamber jet [1
Forming part 7. In that case, the Si molded body will be made by dividing into three parts, and two heating element layers will be formed. That pond,
To manufacture intake heaters and glow plugs for automatic iN engines.
（発明の効果）
本発明は以に述へたように、所定性能を維持し、１１１
つつ複雑形状のセラミックヒータをも製造することがで
きる。(Effects of the Invention) As described below, the present invention can maintain a predetermined performance and manufacture ceramic heaters with complex shapes.
またセラミック成形体ではなくＳｉ成形体を用いること
ができることになり、加工度の低く廉価なＳｉ粉末原料
を用いることができる。Moreover, it is possible to use a Si molded body instead of a ceramic molded body, and it is possible to use an inexpensive Si powder raw material with a low degree of processing.
第１図は円環状セラミックヒータを示す手面図、
第２図は第１図の正面図、
第３図は円環状Ｓｉ成形体を示す９Ｉｔ−面図、第４図
は第３図の正面図、
第５図はＳｉ成形体表面に金属Ｔｉ粉ペーストを塗布し
た状態を示す′Ｔｔｌｒｉｉ図、第６図は第５図の正面
図、
第７図はセラミックヒータの表＋ｎｉ温度−通電時間、
電流−通電時間の関係を示す特性線図、第８図は本発明
に係る方法を用いて形成された渦流室噴口部を示すｆ面
図、
第９図は第８図の縦断面図である。
Ｉ：セラミックヒータ
２．２′ ：成形体
３：金属Ｔｉ粉ペースト
特許出廓人マツダ株式会社
第１図 第３図
第２図 第４図Fig. 1 is a hand view showing the annular ceramic heater, Fig. 2 is a front view of Fig. 1, Fig. 3 is a 9It-plane view showing an annular Si molded body, and Fig. 4 is a front view of Fig. 3. Figure 5 is a 'Ttlrii diagram showing a state in which metal Ti powder paste is applied to the surface of a Si molded body, Figure 6 is a front view of Figure 5, Figure 7 is a table of ceramic heater + ni temperature - energizing time,
A characteristic diagram showing the relationship between current and energization time; FIG. 8 is a f-plane view showing the vortex chamber nozzle formed using the method according to the present invention; FIG. 9 is a longitudinal cross-sectional view of FIG. 8. . I: Ceramic heater 2.2': Molded body 3: Metal Ti powder paste Patent distributor Mazda Motor Corporation Figure 1 Figure 3 Figure 2 Figure 4
Claims (1)
粉成形体間に金属VIＡ若しくはＶＡ族粉ペーストを埋設
した被焼結体を、Ｎ＿２雰囲気下で焼結して、焼結体に
形成し、 前記焼結体に熱間静水圧処理を施す、 ことを特徴とするセラミックヒータの製造方法。(1) Sintering a pair of metal Si compacted bodies with metal VIA or VA group powder paste embedded between the pair of metal Si compacted bodies is sintered in an N_2 atmosphere. 1. A method for manufacturing a ceramic heater, comprising: forming a ceramic heater into a ceramic heater body, and subjecting the sintered body to hot isostatic pressure treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63019085A JPH01195685A (en) | 1988-01-29 | 1988-01-29 | Manufacture of ceramic heater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63019085A JPH01195685A (en) | 1988-01-29 | 1988-01-29 | Manufacture of ceramic heater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01195685A true JPH01195685A (en) | 1989-08-07 |
Family
ID=11989613
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63019085A Pending JPH01195685A (en) | 1988-01-29 | 1988-01-29 | Manufacture of ceramic heater |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01195685A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01226767A (en) * | 1988-03-07 | 1989-09-11 | Hitachi Ltd | Electrically conductive material and production thereof |
-
1988
- 1988-01-29 JP JP63019085A patent/JPH01195685A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01226767A (en) * | 1988-03-07 | 1989-09-11 | Hitachi Ltd | Electrically conductive material and production thereof |
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