JP4069637B2 - Electronic component firing jig - Google Patents
Electronic component firing jig Download PDFInfo
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- JP4069637B2 JP4069637B2 JP2002027938A JP2002027938A JP4069637B2 JP 4069637 B2 JP4069637 B2 JP 4069637B2 JP 2002027938 A JP2002027938 A JP 2002027938A JP 2002027938 A JP2002027938 A JP 2002027938A JP 4069637 B2 JP4069637 B2 JP 4069637B2
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- Prior art keywords
- jig
- zirconia
- electronic component
- firing
- reaction
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Description
【０００１】
【発明の属する技術分野】
本発明はセラミック誘電体、圧電素子、フェライトなどの電子部品を焼成する際に使用する匣鉢、セッターなどの治具に関するものである。
【０００２】
【従来の技術】
セッター等の電子部品焼成用治具は使用条件に応じた耐熱性と機械的強度を具備していなければならないが、その他に重要な特性として焼成するセラミック電子部品と反応しないこと、電子部品の電気特性に影響を及ぼさないことが要求される。即ち、電子部品が焼成用治具と接触部分において反応を生じると変色や融着を起こし、電子部品が不良品となったり、治具が使用不能となるなどの事態を招く。また、治具に反応痕がなくても電子部品の電気特性が低下する不都合を生じる場合もある。
【０００３】
通常、これらの治具の基材には耐熱衝撃性に優れるアルミナ・シリカ質材料が使用される。そして被焼成物との反応を防止する目的で、基材表面に難反応性のジルコニア質のコーティング層を形成した治具が使用されている。この際に使用されるジルコニアはカルシア、イットリア、マグネシア等の安定化剤を含む安定化または部分安定化ジルコニアが一般的である。
【０００４】
ジルコニア質のコーティング層を形成すると、被焼成物との反応防止に有効であるが、繰り返し使用している内に、安定化剤であるカルシアやマグネシアが次第に脱固溶し、ジルコニアの安定化度が低下し、熱間におけるジルコニア特有の膨張、収縮挙動によりコーティング層に亀裂が生じ、ついには基材から剥離するという問題があった。安定化剤のうち、イットリアは脱固溶されにくく安定化度は保持されやすいのであるが、イットリアが非常に高価であり、治具のコストアップを招くため使用しづらい問題がある。
【０００５】
本発明者らは、上述した従来技術の欠点を解消する手法として、基材表面に完全安定化量以上のカルシアを含有するジルコニア質のコーティング層を形成させた治具を開示している。（特開平１０−１３９５７２号公報）
【０００６】
特開平１０−１３９５７２号公報に記載の治具は、コランダム・ムライト質基材の表面に、カルシアを１０〜３３重量％含有するジルコニアのコーティング層を形成させたものである。カルシア含有量が１０〜３３重量％の範囲にある場合、カルシアはジルコン酸カルシウムの形態で存在し、安定化ジルコニアとは異なり、カルシアが脱固溶することなく安定に存在するため、コーティング層の剥離もなく、治具の耐用向上に寄与するものであった。また、この治具は被焼成物との反応抑制効果も非常に優れているものである。
【０００７】
【発明が解決しようとする課題】
上述のように、特開平１０−１３９５７２号公報に記載の治具は被焼成物との反応防止及び耐用性に優れたものであるが、焼成する電子部品によっては、治具に反応の形跡はないが電子部品の電気特性が低下する事態が生じる場合があった。
【０００８】
【課題を解決するための手段】
本発明者等は、ジルコン酸カルシウムの溶射層を形成した治具に関し、種々検討を重ねた結果、ジルコン酸カルシウム、イットリア安定化ジルコニアからなる溶射層を形成することで、前述の問題点を解消するにいたり、本発明を完成させたものである。
【０００９】
即ち、本発明はアルミナ・シリカ質基材の表面にジルコニアを主体とする溶射層を有する電子部品焼成用治具において、該溶射層がジルコン酸カルシウムとイットリア安定化ジルコニアからなることを特徴とする電子部品焼成用治具である。
【００１０】
さらに本発明はアルミナ・シリカ質基材の表面にジルコニアを主体とする溶射層を有する電子部品焼成用治具において、該溶射層がジルコン酸カルシウム、イットリア安定化ジルコニア及び未安定ジルコニアからなることを特徴とする電子部品焼成用治具である。
【００１１】
本発明の電子部品焼成用治具によれば、完全安定化量以上のＣａＯ量を含有するジルコン酸カルシウムの溶射層により焼成する部品と治具との反応を抑制し、少量のイットリア安定化ジルコニアを使用することにより部品の電気特性低下を防止する効果が得られる。
【００１２】
【発明の実施の形態】
治具の基材となるアルミナ・シリカ質材料は、通常の耐火れんがや匣鉢等に使用されるものであり、Ａｌ２Ｏ３含有量が７２重量％以上のものが好ましい。Ａｌ２Ｏ３含有量が７２重量％未満の場合は、必然的にシリカ量が増え、基材中に遊離のシリカ成分が存在するようになり、ジルコニアのコーティング層中に移動拡散することにより、電子部品の特性への悪影響や反応性が増すようになり好ましくない。シリカ量が減少すると耐熱衝撃性が低下するので、基材の組成は治具の使用条件を考慮して設定すればよい。
【００１３】
基材表面にはジルコン酸カルシウムとイットリア安定化ジルコニアからなる溶射層を形成する。溶射は通常のプラズマ溶射が好ましい。溶射層の厚さは０．０１ｍｍ以上が好ましく、０．０５ｍｍ以上がより好ましい。溶射層厚さが０．０１ｍｍ未満では基材中のＡｌ２Ｏ３、ＳｉＯ２成分と電子部品との反応防止効果が不十分となる。
【００１４】
ジルコン酸カルシウムとイットリア安定化ジルコニアからなる溶射層はそれらの混合粉末を溶射すればよい。混合割合は、溶射層中のイットリアの含有量が０．０５重量％以上になることが好ましい。溶射層中のイットリアの含有量が０．０５重量％未満であると、焼成する電子部品に所望の電気特性が得られない場合が生じるため好ましくない。イットリアの含有量の上限は特に規定されるものではなく、コスト設計において適正な量を決定すればよい。
【００１５】
本発明においては、ジルコン酸カルシウムの溶射層により優れた電子部品との反応防止効果が得られ、イットリア安定化ジルコニアを含有させることで、特殊な電子部品の焼成においても反応痕を生じることなく、また電子部品の電気特性低下も抑制される。ジルコン酸カルシウムの組成は理論上カルシアが３１重量％であるが、遊離のカルシアの存在を避けるために通常はカルシア含有量が２０〜２９重量％程度に設定されている。
【００１６】
電子部品によっては、溶射層中にカルシア量が多すぎるとイットリア安定化ジルコニアを含有させても、電気特性の低下が生じてしまう場合がある。本発明においてはこのような電子部品焼成用として、ジルコン酸カルシウムに未安定のジルコニアを混合させることにより、溶射層中のカルシア含有量を任意に設定することが可能である。ジルコン酸カルシウムと未安定ジルコニアの混合比は特に限定されるものではないが、未安定ジルコニアの割合が多いと、熱間での膨張・収縮挙動の影響が大きく、溶射層の剥離の危険性が増し、また電子部品との反応の危険性が増すため、未安定ジルコニアが重量比でジルコン酸カルシウムと同量以下であることが好ましく、ジルコン酸カルシウムの１／２以下の量であることがさらに好ましい。
【００１７】
本発明においては、基材表面にジルコン酸カルシウムとイットリア安定化ジルコニアからなる溶射層を形成するが、該溶射層の形成に先立ち、基材表面にアルミナ溶射層を形成することにより、溶射層の接着性を大幅に向上させることができる。
【００１８】
【実施例】
本発明を実施例により説明する。表１に示す仕様の溶射層を形成した治具を作成した。治具に使用した基材はＡｌ２Ｏ３ ８５重量％、ＳｉＯ２ １５重量％のアルミナ−シリカ質である。溶射層はいずれも１５０μｍ厚さに形成した。表１に示した比較例の治具も同様に作成した。ジルコニアを主体とする溶射層の化学組成を表１に示した。
【００１９】
【表１】
作製した治具を用いてチタン酸バリウムを主成分とする電子部品の焼成を行った。この部品はイットリア安定化ジルコニアの溶射層を形成した治具による焼成では治具との反応が激しく生じ、特開平１０−１３９５７２号公報記載のジルコン酸カルシウムの溶射層を形成した治具による焼成では部品の電気特性低下が生じていずれも所望の焼成結果が得られないものであった。焼成後に治具と電子部品の反応性、焼成した電子部品の電気特性を調査した。調査結果を表１に示した。表中、部品との反応性について、○；反応痕跡なし、△；反応による黒点あり、×；反応による突起、あるいは溶射層の剥離ありの３段階に評価した。また、焼成した部品の電気特性については、○；所望の特性が得られたもの、△；若干の特性低下が見られたもの、×；特性が大幅に低下したものの３段階に評価した。
【００２１】
表１に示すように本発明による治具を使用した焼成では、いずれも部品との反応は見られず、部品の電気特性も所望の結果が得られた。それに対し、比較例に示した治具を使用した焼成では、部品との反応が激しいもの、あるいは電気特性の低下が激しいものが見られる結果となった。
【００２２】
【発明の効果】
本発明の治具によれば、従来、焼成時の反応や電気特性の低下を抑制できなかった電子部品の焼成に使用した場合、部品との反応もなく、また所望の電気特性を有する部品の焼成が可能となる。従って、電子部品の生産性、治具の耐用性両面において、良好な結果が得られる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to jigs such as mortars and setters used when firing electronic parts such as ceramic dielectrics, piezoelectric elements, and ferrite.
[0002]
[Prior art]
Electronic parts firing jigs such as setters must have heat resistance and mechanical strength according to the conditions of use, but other important characteristics are that they do not react with the fired ceramic electronic parts, It is required not to affect the characteristics. That is, when the electronic component reacts at the contact portion with the firing jig, discoloration or fusion occurs, leading to a situation in which the electronic component becomes defective or the jig becomes unusable. Moreover, even if there is no reaction mark on the jig, there may be a disadvantage that the electrical characteristics of the electronic component are deteriorated.
[0003]
Usually, an alumina / silica material having excellent thermal shock resistance is used for the base material of these jigs. And the jig | tool which formed the hardly reactive zirconia coating layer on the base-material surface is used in order to prevent reaction with to-be-fired material. The zirconia used in this case is generally stabilized or partially stabilized zirconia containing a stabilizer such as calcia, yttria, magnesia and the like.
[0004]
Forming a coating layer of zirconia is effective in preventing reaction with the object to be fired, but while repeatedly used, the stabilizers calcia and magnesia gradually desolidify, and the degree of stabilization of zirconia There was a problem that the coating layer cracked due to the expansion and contraction behavior peculiar to zirconia in the hot state and finally peeled off from the substrate. Among the stabilizers, yttria is difficult to be dissolved and easily maintained in stability, but yttria is very expensive and has a problem that it is difficult to use because it increases the cost of the jig.
[0005]
The present inventors have disclosed a jig in which a zirconia-based coating layer containing a calcia containing a fully stabilized amount or more is formed on the surface of the substrate as a technique for solving the above-described drawbacks of the conventional technology. (Japanese Patent Laid-Open No. 10-139572)
[0006]
The jig described in JP-A-10-139572 is obtained by forming a coating layer of zirconia containing 10 to 33% by weight of calcia on the surface of a corundum / mullite base material. When the calcia content is in the range of 10 to 33% by weight, the calcia exists in the form of calcium zirconate, and unlike the stabilized zirconia, the calcia exists stably without desolvation, so the coating layer There was no peeling and it contributed to the improvement of the durability of the jig. Further, this jig is very excellent in the effect of suppressing the reaction with the object to be fired.
[0007]
[Problems to be solved by the invention]
As described above, the jig described in JP-A-10-139572 is excellent in preventing reaction and durability with the object to be fired, but depending on the electronic parts to be fired, there is no evidence of reaction on the jig. In some cases, however, the electrical characteristics of the electronic component may deteriorate.
[0008]
[Means for Solving the Problems]
The inventors of the present invention have made various studies on a jig formed with a sprayed layer of calcium zirconate, and as a result, formed the sprayed layer of calcium zirconate and yttria-stabilized zirconia, thereby solving the above-mentioned problems. In other words, the present invention has been completed.
[0009]
That is, the present invention is an electronic component firing jig having a thermal spray layer mainly composed of zirconia on the surface of an alumina / silica substrate, wherein the thermal spray layer is composed of calcium zirconate and yttria stabilized zirconia. This is an electronic component firing jig.
[0010]
Furthermore, the present invention relates to an electronic component firing jig having a thermal spray layer mainly composed of zirconia on the surface of an alumina / silica substrate, wherein the thermal spray layer is composed of calcium zirconate, yttria stabilized zirconia and unstable zirconia. The electronic component firing jig is characterized.
[0011]
According to the electronic component firing jig of the present invention, the reaction between the fired component and the jig is suppressed by the sprayed layer of calcium zirconate containing a CaO amount that is not less than the fully stabilized amount, and a small amount of yttria-stabilized zirconia is achieved. The effect of preventing the deterioration of the electrical characteristics of the parts can be obtained.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
The alumina / siliceous material used as the base material of the jig is used for ordinary refractory bricks and mortars, and preferably has an Al2O3 content of 72% by weight or more. When the content of Al2O3 is less than 72% by weight, the amount of silica is inevitably increased, and a free silica component is present in the base material. By moving and diffusing into the coating layer of zirconia, The adverse effect on the characteristics and the reactivity increase, which is not preferable. Since the thermal shock resistance decreases when the amount of silica decreases, the composition of the substrate may be set in consideration of the use conditions of the jig.
[0013]
A sprayed layer composed of calcium zirconate and yttria-stabilized zirconia is formed on the substrate surface. Thermal spraying is preferably normal plasma spraying. The thickness of the sprayed layer is preferably 0.01 mm or more, and more preferably 0.05 mm or more. When the sprayed layer thickness is less than 0.01 mm, the effect of preventing the reaction between the Al2O3 and SiO2 components in the substrate and the electronic component becomes insufficient.
[0014]
The thermal spray layer composed of calcium zirconate and yttria stabilized zirconia may be sprayed with a mixed powder thereof. The mixing ratio is preferably such that the yttria content in the sprayed layer is 0.05% by weight or more. If the yttria content in the sprayed layer is less than 0.05% by weight, it may not be possible to obtain desired electrical characteristics for the electronic component to be fired. The upper limit of the yttria content is not particularly defined, and an appropriate amount may be determined in cost design.
[0015]
In the present invention, an excellent effect of preventing reaction with an electronic component is obtained by the sprayed layer of calcium zirconate, and by containing yttria-stabilized zirconia, reaction marks are not generated even in the firing of special electronic components, Moreover, the electrical characteristic fall of an electronic component is also suppressed. The composition of calcium zirconate is theoretically 31% by weight of calcia, but in order to avoid the presence of free calcia, the content of calcia is usually set to about 20 to 29% by weight.
[0016]
Depending on the electronic component, if the amount of calcia is too large in the sprayed layer, even if yttria-stabilized zirconia is contained, the electrical characteristics may be deteriorated. In the present invention, the calcia content in the sprayed layer can be arbitrarily set by mixing unstable zirconia with calcium zirconate for such electronic component firing. The mixing ratio of calcium zirconate and unstable zirconia is not particularly limited, but if the ratio of unstable zirconia is large, the effect of hot expansion and contraction is large, and the risk of peeling of the sprayed layer is high. In addition, since the risk of reaction with electronic components increases, it is preferable that the unstable zirconia is less than or equal to the amount of calcium zirconate by weight, and more preferably ½ or less of calcium zirconate. preferable.
[0017]
In the present invention, a sprayed layer composed of calcium zirconate and yttria-stabilized zirconia is formed on the surface of the substrate. Prior to the formation of the sprayed layer, an alumina sprayed layer is formed on the surface of the substrate, Adhesiveness can be greatly improved.
[0018]
【Example】
The present invention is illustrated by examples. A jig having a sprayed layer having the specifications shown in Table 1 was prepared. The base material used for the jig is an alumina-silica material of 85% by weight of Al2O3 and 15% by weight of SiO2. Each sprayed layer was formed to a thickness of 150 μm. The jig of the comparative example shown in Table 1 was also prepared in the same manner. Table 1 shows the chemical composition of the sprayed layer mainly composed of zirconia.
[0019]
[Table 1]
An electronic component mainly composed of barium titanate was fired using the produced jig. When firing with a jig with a yttria-stabilized zirconia sprayed layer, this part reacts violently with the jig, and with a jig with a calcium zirconate sprayed layer described in JP-A-10-139572, The electrical characteristics of the parts deteriorated, and any desired firing results could not be obtained. After firing, the reactivity of the jig and electronic parts and the electrical properties of the fired electronic parts were investigated. The survey results are shown in Table 1. In the table, the reactivity with the components was evaluated in three stages: ○: no reaction trace, Δ: black spot due to reaction, x: protrusion due to reaction, or peeling of sprayed layer. In addition, the electrical characteristics of the fired parts were evaluated in three stages: ◯: a desired characteristic was obtained, Δ: a slight characteristic decrease was observed, and X: a characteristic was significantly decreased.
[0021]
As shown in Table 1, in the firing using the jig according to the present invention, no reaction with the parts was observed, and the electrical characteristics of the parts had the desired results. On the other hand, in the firing using the jig shown in the comparative example, there was a result that the reaction with the part was severe or the electrical property was severely deteriorated.
[0022]
【The invention's effect】
According to the jig of the present invention, when used for firing an electronic component that could not suppress a reaction during firing and a decrease in electrical characteristics, there is no reaction with the component and a component having desired electrical characteristics. Firing is possible. Therefore, good results can be obtained in both the productivity of electronic parts and the durability of jigs.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002027938A JP4069637B2 (en) | 2002-02-05 | 2002-02-05 | Electronic component firing jig |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002027938A JP4069637B2 (en) | 2002-02-05 | 2002-02-05 | Electronic component firing jig |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003226586A JP2003226586A (en) | 2003-08-12 |
| JP4069637B2 true JP4069637B2 (en) | 2008-04-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002027938A Expired - Fee Related JP4069637B2 (en) | 2002-02-05 | 2002-02-05 | Electronic component firing jig |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4069637B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228362B (en) * | 2005-10-27 | 2012-01-18 | 日本精工株式会社 | Insulating rolling bearing for use in prevention of electric corrosion, method for manufacture thereof, and bearing device |
| JP5100726B2 (en) * | 2009-09-11 | 2012-12-19 | 日本碍子株式会社 | Setter |
| CN113185326A (en) * | 2021-04-02 | 2021-07-30 | 武汉科技大学 | Kiln furniture spray coating for roasting lithium battery anode material and preparation method thereof |
| US20230046855A1 (en) * | 2021-08-02 | 2023-02-16 | Taiyo Yuden Co., Ltd. | Ceramic electronic device, dielectric material, and manufacturing method of ceramic electronic device |
-
2002
- 2002-02-05 JP JP2002027938A patent/JP4069637B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2003226586A (en) | 2003-08-12 |
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