JP5474538B2 - Manufacturing method of electronic component firing jig - Google Patents
Manufacturing method of electronic component firing jig Download PDFInfo
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- JP5474538B2 JP5474538B2 JP2009517770A JP2009517770A JP5474538B2 JP 5474538 B2 JP5474538 B2 JP 5474538B2 JP 2009517770 A JP2009517770 A JP 2009517770A JP 2009517770 A JP2009517770 A JP 2009517770A JP 5474538 B2 JP5474538 B2 JP 5474538B2
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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Description
本発明は、誘電体、積層コンデンサ、セラミックコンデンサ、圧電素子、サーミスタ等の電子部品を焼成する際に用いる、セッター、棚板、匣鉢等の電子部品焼成用治具の製造方法に関する。 The present invention relates to a method for manufacturing a jig for firing electronic parts such as setters, shelf boards, and mortars used when firing electronic parts such as dielectrics, multilayer capacitors, ceramic capacitors, piezoelectric elements, and thermistors.
従来の電子部品焼成用治具の製造方法としては、焼成した基材上にジルコニアコーティング材などを付着させて、これを焼成することが一般的であった。
これに対し、焼成することなく乾燥したのみの基材の表面にジルコニアを含有してなるコーティング材を噴霧後、同時焼成により、基材表面にコーティング材を付着させる方法が開示されている(下記特許文献1の[請求項1]等参照)。As a conventional method for manufacturing a jig for firing electronic parts, it has been common to deposit a zirconia coating material or the like on a fired base material and fire it.
On the other hand, after spraying a coating material containing zirconia on the surface of a base material that has only been dried without firing, a method is disclosed in which the coating material is attached to the surface of the base material by simultaneous firing (see below). (Refer to [Claim 1] etc. of patent document 1).
上記製法により製造した電子部品焼成用治具は、基材上にコーティング材などで形成した保護層が形成してあり、焼成時に、基材と保護層は膨張率や収縮率が相違するため、保護層が剥離してしまうことがあった。
本発明者は、この原因を鋭意研究した結果、基材と保護層とを同時に焼成すると保護層が剥離しやすいことを見出した。The electronic component firing jig produced by the above production method has a protective layer formed of a coating material or the like on the base material, and the base material and the protective layer have different expansion rates and shrinkage rates during firing. The protective layer sometimes peeled off.
As a result of intensive studies on this cause, the present inventor has found that the protective layer is easily peeled off when the base material and the protective layer are simultaneously fired.
そこで、本発明の目的は、基材と保護層とが剥離しにくく、また、保護層に亀裂が入りにくい電子部品焼成用治具の製造方法を提供することにある。 Accordingly, an object of the present invention is to provide a method for manufacturing a jig for firing an electronic component in which a base material and a protective layer are hardly peeled off and cracks are not easily formed in the protective layer.
本発明の電子部品焼成用治具の製造方法は、アルミナ系材料、アルミナ−ムライト系材料、ムライト系材料、アルミナ−マグネシア系スピネル材料、アルミナ−ムライト−コーディエライト系材料のいずれかからなる基材上に、アルミナ、ジルコニア、イットリア、シリカ、カルシア、マグネシア、ストロンチア、ムライト及びアルミナ・マグネシアスピネル複合酸化物のいずれか又はこれらの組合せからなる保護層を備えた電子部品焼成用治具の製造方法であって、基材に、バインダーを除去して表面に窪みを形成する予備焼成をし、予備焼成した基材上に保護層を形成した後、基材と保護層とを焼き締める本焼成を、予備焼成の温度より500℃以上高い温度で行う工程を備えたことを特徴とする。 The manufacturing method of the electronic component firing jig of the present invention is a group comprising any one of an alumina material, an alumina-mullite material, a mullite material, an alumina-magnesia spinel material, and an alumina-mullite-cordierite material. Method for manufacturing jig for firing electronic component comprising protective layer made of any one of alumina, zirconia, yttria, silica, calcia, magnesia, strontia, mullite and alumina-magnesia spinel composite oxide or a combination thereof on the material Then, the substrate is pre-baked to remove the binder and form a depression on the surface, and after forming the protective layer on the pre-baked substrate, the main baking is performed to bake the substrate and the protective layer. And a step of performing at a temperature higher by 500 ° C. or more than the pre-baking temperature.
このような工程を備えることにより、基材と保護層とが剥離しにくい電子部品焼成用治具を製造することができる。
これは、従来では、基材を焼成する際、高温で焼成すると、基材が焼き締まり、基材表面が平滑になりやすく、この上に保護層を形成していたため、基材から保護層が剥離しやすくなっていたが、本発明では、基材を予備焼成することにより、基材からバインダーのみが除去され、基材表面上に無数の窪みができ、この窪み内に保護層材料が入り込み焼結されるので、保護層が基材に楔を打ち込んだような形状となり、保護層が基材から剥離しにくくなる。By providing such a process, it is possible to manufacture an electronic component firing jig in which the base material and the protective layer are unlikely to peel off.
Conventionally, when the base material is fired at a high temperature, the base material is baked and the surface of the base material is easily smoothed, and a protective layer is formed thereon. Although it was easy to peel off, in the present invention, by pre-baking the base material, only the binder was removed from the base material, and numerous indentations were formed on the surface of the base material, and the protective layer material entered into the indentations. Since it is sintered, the protective layer has a shape as if a wedge is driven into the substrate, and the protective layer is difficult to peel from the substrate.
また、本発明は、上記製造方法により製造した電子部品焼成用治具も対象とする。 Moreover, this invention also makes the jig | tool for electronic component baking manufactured with the said manufacturing method also object.
なお、本発明でいう「予備焼成」とは、基材のバインダーを除去でき、かつ、基材の強度を保持できるが、本焼成ほど焼き締まらない温度で焼成することをいう。例えば、基材の材質にもよるが、600℃以上1400℃未満で焼成することが予備焼成の好ましい一形態として挙げられる。また、本発明でいう「本焼成」とは、基材が焼き締まる温度で焼成することをいう。例えば、基材の材質にもよるが、1400℃以上2000℃以下で焼成することが本焼成の好ましい一形態として挙げられる。 The “pre-firing” in the present invention refers to firing at a temperature at which the binder of the base material can be removed and the strength of the base material can be maintained, but not as fast as the main firing. For example, although it depends on the material of the base material, firing at 600 ° C. or more and less than 1400 ° C. is a preferred form of preliminary firing. In addition, “main firing” in the present invention means firing at a temperature at which the base material is fired. For example, although it depends on the material of the base material, firing at 1400 ° C. or more and 2000 ° C. or less is a preferable embodiment of the firing.
以下、本発明の一実施形態を説明する。なお、本発明は、この実施形態に限定されるものではない。 Hereinafter, an embodiment of the present invention will be described. Note that the present invention is not limited to this embodiment.
本発明の一実施形態の電子部品焼成用治具の製造方法は、基材を予備焼成した後、その上に保護層を形成して本焼成をする工程を備えたものである。
なお、本実施形態は、一層の保護層としてあるが、本発明は、これに限定するものではなく、二層や三層以上の保護層とすることもできる。The method for manufacturing an electronic component firing jig according to an embodiment of the present invention includes a step of pre-baking a base material, forming a protective layer thereon, and performing main firing.
In addition, although this embodiment is provided as a single protective layer, the present invention is not limited to this, and a protective layer having two layers or three or more layers can also be used.
基材材料としては、従来公知の材料を用いることができ、例えば、アルミナ系材料、アルミナ−ムライト系材料、ムライト系材料、アルミナ−マグネシア系スピネル材料、アルミナ−ムライト−コーディエライト系材料、又はこれらの組み合わせによる材料などを使用することができる。 As the base material, conventionally known materials can be used. For example, alumina-based material, alumina-mullite-based material, mullite-based material, alumina-magnesia-based spinel material, alumina-mullite-cordierite-based material, or A material by a combination of these can be used.
基材材料の平均粒径は、特に限定するものではないが、0.1μm〜5000μm、好ましくは0.2μm〜3000μmとし、また、ランダムな粒径の基材材料で基材を構成してもよい。例えば、平均粒径100μm〜5000μm、好ましくは200μm〜3000μmの粗粒子と平均粒径0.1μm〜100μm、好ましくは0.2μm〜50μmの微粒子を混合したものを、基材材料とすることもできる。 The average particle diameter of the base material is not particularly limited, but may be 0.1 μm to 5000 μm, preferably 0.2 μm to 3000 μm, and the base material may be composed of a base material having a random particle diameter. Good. For example, a material obtained by mixing coarse particles having an average particle size of 100 μm to 5000 μm, preferably 200 μm to 3000 μm, and fine particles having an average particle size of 0.1 μm to 100 μm, preferably 0.2 μm to 50 μm can be used as the base material. .
これら材料に、セルロース系、糖類系、でんぷん系などの結合剤、可塑剤、湿潤剤、離型剤等を混合して結合させ、予備焼成を行い基材を形成することができる。
基材の厚さは、特に限定するものではないが、1mm〜100mm、好ましくは2mm〜50mmに形成することができる。Cellulose-based, saccharide-based, and starch-based binders, plasticizers, wetting agents, mold release agents, and the like can be mixed and bonded to these materials, and pre-baked to form a substrate.
Although the thickness of a base material is not specifically limited, 1 mm-100 mm, Preferably it can form in 2 mm-50 mm.
予備焼成は、基材のバインダーを除去でき、かつ、基材の強度を保持できるが、本焼成ほど焼き締まらない温度で行い、例えば、600℃以上1400℃未満、好ましくは700℃以上1300℃以下で行なうことができ、後述する本焼成の温度より、500℃以上低くするのが好ましい。 The preliminary firing can remove the binder of the base material and can maintain the strength of the base material, but is performed at a temperature that does not shrink as much as the main firing, for example, 600 ° C. or higher and lower than 1400 ° C., preferably 700 ° C. or higher and 1300 ° C. or lower. It is preferable that the temperature is lower by 500 ° C. or more than the temperature of the main firing described later.
この予備焼成した基材上に、保護層の材料をスプレーコートし、100℃で乾燥させて保護層を形成することができる。
この材料としては、従来公知の材料を用いることができ、例えば、酸化アルミニウム(アルミナ)、酸化ジルコニウム(ジルコニア)、酸化イットリウム(イットリア)、二酸化ケイ素(シリカ)、酸化カルシウム(カルシア)、酸化マグネシウム(マグネシア)、酸化ストロンチウム(ストロンチア)、ムライト及びMgAl2O4などのアルミナ・マグネシアスピネル複合酸化物、又はこれらの組み合わせによる材料を使用することができる。The protective layer can be formed by spray-coating the protective layer material on the pre-fired substrate and drying at 100 ° C.
As this material, conventionally known materials can be used. For example, aluminum oxide (alumina), zirconium oxide (zirconia), yttrium oxide (yttria), silicon dioxide (silica), calcium oxide (calcia), magnesium oxide ( Magnesia), strontium oxide (strontia), mullite and alumina-magnesia spinel composite oxides such as MgAl 2 O 4 , or combinations thereof can be used.
この材料の平均粒径は、特に限定するものではないが、0.1μm〜500μm、好ましくは0.2μm〜300μmとし、また、ランダムな粒径の材料で保護層を構成してもよい。例えば、平均粒径20μm〜500μm、好ましくは50μm〜300μmの粗粒子と平均粒径0.1μm〜50μm、好ましくは0.2μm〜30μmの微粒子を混合したものを、材料とすることもできる。
なお、本発明でいう平均粒径は、平均粒径が50μm以上のものについては、振動篩いを用いるロータップ法にて測定し、平均粒径が50μm未満のものについては、レーザー回折法により測定することができる。Although the average particle diameter of this material is not particularly limited, it may be 0.1 μm to 500 μm, preferably 0.2 μm to 300 μm, and the protective layer may be composed of a material having a random particle diameter. For example, a material obtained by mixing coarse particles having an average particle diameter of 20 μm to 500 μm, preferably 50 μm to 300 μm and fine particles having an average particle diameter of 0.1 μm to 50 μm, preferably 0.2 μm to 30 μm can be used.
The average particle diameter as used in the present invention is measured by a low tap method using a vibration sieve for those having an average particle diameter of 50 μm or more, and is measured by a laser diffraction method for those having an average particle diameter of less than 50 μm. be able to.
コートは、例えば、塗布−熱分解法、スプレーコート、ディップコート、結着法等により行なうことができる。
塗布−熱分解法では、上記材料の硝酸塩等の金属塩水溶液を基材上に塗布し、熱分解により変換して保護層を形成することができる。
スプレーコートでは、上記材料を溶媒に懸濁させた溶液を基材上に噴射し、かつ、溶媒を飛散させて基材上に保護層を形成することができる。
ディップコートでは、上記材料を溶解又は懸濁させた溶液に、基材を浸して上記材料を含有する液層を基材表面に形成した後、乾燥して溶媒を除去して保護層を形成することができる。
結着法では、所定の粒径分布を有する上記材料を、バインダーを使用して互いに結合させるとともに基材に結着させて保護層を形成することができる。
保護層の厚さは、特に限定するものではないが、30μm〜500μm、好ましくは50μm〜300μmに形成することができる。The coating can be performed, for example, by a coating-pyrolysis method, spray coating, dip coating, binding method, or the like.
In the coating-pyrolysis method, a metal salt aqueous solution such as nitrate of the above material can be coated on a substrate and converted by thermal decomposition to form a protective layer.
In spray coating, a protective layer can be formed on a substrate by spraying a solution obtained by suspending the material in a solvent onto the substrate and scattering the solvent.
In dip coating, the substrate is immersed in a solution in which the above materials are dissolved or suspended to form a liquid layer containing the above materials on the surface of the substrate, and then dried to remove the solvent and form a protective layer. be able to.
In the binding method, the above materials having a predetermined particle size distribution can be bonded to each other using a binder and bonded to a substrate to form a protective layer.
Although the thickness of a protective layer is not specifically limited, It can form in 30 micrometers-500 micrometers, Preferably it is 50 micrometers-300 micrometers.
このように、基材上に保護層を形成したものを本焼成し、電子部品焼成用治具を製造することができる。
この本焼成は、基材が焼き締まる温度で行い、例えば、1400℃以上2000℃以下、好ましくは1600℃以上1850℃以下で行なうことができる。なお、本焼成は、基材と保護層とが焼き締まる温度で行なうのが好ましい。Thus, the thing which formed the protective layer on the base material can be baked, and the electronic component baking jig | tool can be manufactured.
This main baking is performed at a temperature at which the base material is baked, for example, 1400 ° C. to 2000 ° C., preferably 1600 ° C. to 1850 ° C. In addition, it is preferable to perform this baking at the temperature which a base material and a protective layer bake.
このように製造した電子部品焼成用治具は、基材と保護層とが強固に固着し、熱サイクル環境下でも剥離しにくいものである。
これは、基材を予備焼成したため、基材表面からバインダーのみが除去されて窪みができ、その後、その基材表面上に保護層の材料を塗布することにより、保護層の材料が窪みに入り込み、その状態で本焼成を行なうため、保護層が基材上に楔を打ち込んだような状態になり、基材と保護層とが強固に固着し、剥離しにくくなる。In the electronic component firing jig manufactured in this way, the base material and the protective layer are firmly fixed, and are difficult to peel even in a thermal cycle environment.
This is because the base material was pre-fired, so that only the binder was removed from the surface of the base material to form a recess, and then the protective layer material was applied onto the surface of the base material so that the protective layer material entered the recess. Since the main baking is performed in this state, the protective layer is in a state where a wedge is driven onto the base material, and the base material and the protective layer are firmly fixed and are difficult to peel off.
また、本発明は、二層以上の保護層とすることもでき、例えば、上記保護層上に、さらに、保護層の材料をコートし、乾燥させて二層以上の保護層とすることもできる。
保護層を、二層以上とする場合は、全ての層を形成した後に本焼成を行なうことや、少なくとも一層を形成した後に本焼成を行い、その上に残りの層を形成することができる。In addition, the present invention may be a protective layer having two or more layers. For example, the protective layer material may be further coated on the protective layer and dried to form two or more protective layers. .
When the protective layer has two or more layers, the main baking can be performed after all layers are formed, or the main baking can be performed after forming at least one layer, and the remaining layers can be formed thereon.
以下、本発明の実施例を説明する。但し、本発明は、この実施例に限定されるものではない。 Examples of the present invention will be described below. However, the present invention is not limited to this embodiment.
(実施例1)
実施例1の電子部品焼成用治具は、以下のように形成した。
基材材料は、電融アルミナと電融ムライトとの混合物(平均粒径200μm、重量比率1:1)70重量%と、シリカと仮焼アルミナとの混合物(平均粒径4μm、重量比率1:5)30重量%とを用いた。これら材料を混合した後、水とバインダー(ポリビニルアルコール)を添加して均一になるように、さらに混合してスラリーとし、このスラリーを、油圧成形機を用い、プレスして板状とし、これを1000℃で予備焼成して厚さ5mmのアルミナ−ムライト系基材を形成した。Example 1
The electronic component firing jig of Example 1 was formed as follows.
The base material is composed of 70% by weight of a mixture of fused alumina and fused mullite (average particle size 200 μm, weight ratio 1: 1) and a mixture of silica and calcined alumina (average particle size 4 μm, weight ratio 1: 5) 30% by weight was used. After mixing these materials, water and a binder (polyvinyl alcohol) are added and mixed uniformly to make a slurry, and this slurry is pressed into a plate shape using a hydraulic molding machine. Pre-baking was performed at 1000 ° C. to form an alumina-mullite base material having a thickness of 5 mm.
保護層の材料は、平均粒径150μmのイットリア安定化ジルコニア96重量%と、平均粒径1μmのイットリア安定化ジルコニア4重量%とを用いた。これら材料を混合した後、水とバインダー(ポリビニルアルコール)を添加して均一になるように、さらに混合してスラリーとし、このスラリーを前記第一保護層表面上にスプレーコートし、約100℃で乾燥させて厚さ150μmのイットリア安定化ジルコニア層を形成した。 As the material for the protective layer, 96% by weight of yttria-stabilized zirconia having an average particle diameter of 150 μm and 4% by weight of yttria-stabilized zirconia having an average particle diameter of 1 μm were used. After mixing these materials, water and a binder (polyvinyl alcohol) are added and mixed uniformly to form a slurry, and this slurry is spray-coated on the surface of the first protective layer at about 100 ° C. By drying, a 150 μm thick yttria-stabilized zirconia layer was formed.
このように、基材上に、保護層を形成し、1800℃で本焼成し、実施例1の電子部品焼成用治具を形成した。 Thus, the protective layer was formed on the base material, and the main component was fired at 1800 ° C. to form the electronic component firing jig of Example 1.
(実施例2)
実施例2の電子部品焼成用治具は、基材上に、保護層となるアルミナ層を形成した以外は、実施例1と同様に形成した。
アルミナ層の材料は、平均粒径50μmのアルミナ96重量%と、平均粒径4μmのアルミナ4重量%とを用いた。これら材料を混合した後、水とバインダー(ポリビニルアルコール)を添加して均一になるように、さらに混合してスラリーとし、このスラリーを前記基材表面上にスプレーコートし、約100℃で乾燥させて厚さ100μmのアルミナ層を形成した。(Example 2)
The electronic component firing jig of Example 2 was formed in the same manner as in Example 1 except that an alumina layer serving as a protective layer was formed on the substrate.
As the material for the alumina layer, 96% by weight of alumina having an average particle diameter of 50 μm and 4% by weight of alumina having an average particle diameter of 4 μm were used. After mixing these materials, water and a binder (polyvinyl alcohol) are added and mixed uniformly to form a slurry, which is then spray coated onto the substrate surface and dried at about 100 ° C. An alumina layer having a thickness of 100 μm was formed.
(実施例3)
実施例3の電子部品焼成用治具は、予備焼成温度を700℃とした以外は、実施例2と同様に形成した。(Example 3)
The electronic component firing jig of Example 3 was formed in the same manner as in Example 2 except that the pre-baking temperature was 700 ° C.
(実施例4)
実施例4の電子部品焼成用治具は、予備焼成温度を1300℃とした以外は、実施例2と同様に形成した。Example 4
The electronic component firing jig of Example 4 was formed in the same manner as in Example 2 except that the pre-baking temperature was 1300 ° C.
(実施例5)
実施例5の電子部品焼成用治具は、予備焼成温度を700℃とし、本焼成温度を1600℃とした以外は、実施例2と同様に形成した。(Example 5)
The electronic component firing jig of Example 5 was formed in the same manner as in Example 2 except that the preliminary firing temperature was 700 ° C. and the main firing temperature was 1600 ° C.
(実施例6)
実施例6の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのイットリア70重量%と、平均粒径4μmのイットリア30重量%とし、基材本焼成温度を1850℃とした以外は、実施例1と同様に形成した。(Example 6)
In the electronic component firing jig of Example 6, the protective layer was made of 70% by weight yttria having an average particle size of 50 μm and 30% by weight yttria having an average particle size of 4 μm, and the substrate main firing temperature was 1850 ° C. Except for this, it was formed in the same manner as in Example 1.
(実施例7)
実施例7の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのスピネル(MgAl2O4)65重量%と、平均粒径4μmのスピネル(MgAl2O4)35重量%とし、本焼成温度を1700℃とした以外は、実施例1と同様に形成した。(Example 7)
In the electronic component firing jig of Example 7, the protective layer material was 65% by weight of spinel (MgAl 2 O 4 ) having an average particle diameter of 50 μm and 35% by weight of spinel (MgAl 2 O 4 ) having an average particle diameter of 4 μm. And formed in the same manner as in Example 1 except that the main firing temperature was 1700 ° C.
(実施例8)
実施例8の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとシリカとの混合物30重量%(平均粒径4μm,重量比率4:1)とし、本焼成温度を1850℃とした以外は、実施例1と同様に形成した。(Example 8)
In the electronic part firing jig of Example 8, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and silica (average particle diameter of 4 μm, weight ratio of 4: 1). And was formed in the same manner as in Example 1 except that the main firing temperature was 1850 ° C.
(実施例9)
実施例9の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとジルコニアとの混合物30重量%(平均粒径4μm,重量比率4:1)とした以外は、実施例1と同様に形成した。Example 9
In the jig for firing electronic parts of Example 9, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and zirconia (average particle diameter of 4 μm, weight ratio of 4: 1). Except that, it was formed in the same manner as in Example 1.
(実施例10)
実施例10の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ75重量%と、アルミナとイットリアとの混合物25重量%(平均粒径4μm,重量比率4:1)とし、本焼成温度を1850℃とした以外は、実施例1と同様に形成した。(Example 10)
In the jig for firing electronic parts of Example 10, the protective layer material was 75% by weight of alumina having an average particle diameter of 50 μm and 25% by weight of a mixture of alumina and yttria (average particle diameter of 4 μm, weight ratio of 4: 1). And was formed in the same manner as in Example 1 except that the main firing temperature was 1850 ° C.
(実施例11)
実施例11の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとカルシアとの混合物30重量%(平均粒径4μm,重量比率4:1)とし、本焼成温度を1700℃とした以外は、実施例1と同様に形成した。(Example 11)
In the jig for firing electronic parts of Example 11, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and calcia (average particle diameter of 4 μm, weight ratio of 4: 1). And formed in the same manner as in Example 1 except that the main firing temperature was 1700 ° C.
(実施例12)
実施例12の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとマグネシアとの混合物30重量%(平均粒径4μm,重量比率4:1)とした以外は、実施例1と同様に形成した。(Example 12)
In the electronic part firing jig of Example 12, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and magnesia (average particle diameter of 4 μm, weight ratio of 4: 1). Except that, it was formed in the same manner as in Example 1.
(実施例13)
実施例13の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナと酸化ストロンチウムとの混合物30重量%(平均粒径4μm,重量比率4:1)とした以外は、実施例1と同様に形成した。(Example 13)
In the electronic component firing jig of Example 13, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and strontium oxide (average particle diameter of 4 μm, weight ratio 4: 1). ), Except for the above.
(実施例14)
実施例14の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとスピネル(MgAl2O4)との混合物30重量%(平均粒径4μm,重量比率4:1)とした以外は、実施例1と同様に形成した。(Example 14)
In the electronic component baking jig of Example 14, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina and spinel (MgAl 2 O 4 ) (average particle diameter of 4 μm, It was formed in the same manner as in Example 1 except that the weight ratio was 4: 1).
(実施例15)
実施例15の電子部品焼成用治具は、保護層の材料を、平均粒径150μmのカルシア安定化ジルコニア70重量%と、平均粒径1μmのカルシア安定化ジルコニア30重量%とした以外は、実施例1と同様に形成した。(Example 15)
The electronic component firing jig of Example 15 was carried out except that the protective layer material was 70% by weight of calcia-stabilized zirconia having an average particle diameter of 150 μm and 30% by weight of calcia-stabilized zirconia having an average particle diameter of 1 μm. Formed as in Example 1.
(実施例16)
実施例16の電子部品焼成用治具は、保護層の材料を、平均粒径150μmのマグネシア安定化ジルコニア70重量%と、平均粒径1μmのマグネシア安定化ジルコニア30重量%とした以外は、実施例1と同様に形成した。(Example 16)
The jig for firing electronic parts of Example 16 was implemented except that the protective layer material was 70% by weight of magnesia stabilized zirconia having an average particle size of 150 μm and 30% by weight of magnesia stabilized zirconia having an average particle size of 1 μm. Formed as in Example 1.
(実施例17)
実施例17の電子部品焼成用治具は、本焼成温度を1850℃とした以外は、実施例1と同様に形成した。(Example 17)
The electronic component firing jig of Example 17 was formed in the same manner as in Example 1 except that the main firing temperature was 1850 ° C.
(実施例18)
実施例18の電子部品焼成用治具は、本焼成温度を1850℃とした以外は、実施例1と同様に形成した。(Example 18)
The electronic component firing jig of Example 18 was formed in the same manner as in Example 1 except that the main firing temperature was 1850 ° C.
(実施例19)
実施例19の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとシリカとジルコニアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 19)
In the electronic component firing jig of Example 19, the material of the protective layer was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, silica and zirconia (average particle diameter of 4 μm, weight ratio 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例20)
実施例20の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとシリカとカルシアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 20)
In the electronic component firing jig of Example 20, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm, and 30% by weight of a mixture of alumina, silica and calcia (average particle diameter of 4 μm, weight ratio 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例21)
実施例21の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとシリカとマグネシアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 21)
In the electronic component firing jig of Example 21, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, silica and magnesia (average particle diameter of 4 μm, weight ratio 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例22)
実施例22の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとジルコニアとイットリアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 22)
In the jig for firing electronic parts of Example 22, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, zirconia and yttria (average particle diameter of 4 μm, weight ratio 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例23)
実施例23の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとジルコニアとカルシアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 23)
In the electronic part firing jig of Example 23, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, zirconia and calcia (average particle diameter of 4 μm, weight ratio of 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例24)
実施例24の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとジルコニアとマグネシアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とし、予備焼成温度を800℃とし、本焼成温度を1600℃とした以外は、実施例1と同様に形成した。(Example 24)
In the electronic part firing jig of Example 24, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, zirconia and magnesia (average particle diameter of 4 μm, weight ratio of 8: 1: 1), the pre-baking temperature was 800 ° C., and the main baking temperature was 1600 ° C.
(実施例25)
実施例25の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとジルコニアとスピネル(MgAl2O4)との混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 25)
In the electronic component firing jig of Example 25, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm, and 30% by weight of a mixture of alumina, zirconia and spinel (MgAl 2 O 4 ) (average particle diameter). It was formed in the same manner as in Example 1 except that the thickness was 4 μm and the weight ratio was 8: 1: 1.
(実施例26)
実施例26の電子部品焼成用治具は、保護層の材料を、平均粒径50μmのアルミナ70重量%と、アルミナとイットリアとカルシアとの混合物30重量%(平均粒径4μm,重量比率8:1:1)とした以外は、実施例1と同様に形成した。(Example 26)
In the electronic component firing jig of Example 26, the protective layer material was 70% by weight of alumina having an average particle diameter of 50 μm and 30% by weight of a mixture of alumina, yttria and calcia (average particle diameter of 4 μm, weight ratio of 8: It was formed in the same manner as in Example 1 except that the ratio was 1: 1).
(実施例27)
実施例27の電子部品焼成用治具は、基材の材料を、平均粒径200μmの電融アルミナ70重量%と、粘土と仮焼アルミナとの混合物(平均粒径4μm、重量比率1:5)30重量%とした以外は、実施例2と同様に形成した。(Example 27)
In the electronic component firing jig of Example 27, the base material was made of 70% by weight of fused alumina having an average particle size of 200 μm and a mixture of clay and calcined alumina (average particle size of 4 μm, weight ratio 1: 5). ) It was formed in the same manner as in Example 2 except that it was 30% by weight.
(実施例28)
実施例28の電子部品焼成用治具は、基材の材料を、電融アルミナとスピネル(MgAl2O4)との混合物(平均粒径200μm、重量比率1:1)70重量%と、粘土と仮焼アルミナとの混合物(平均粒径4μm、重量比率1:5)30重量%とした以外は、実施例2と同様に形成した。(Example 28)
In the electronic component firing jig of Example 28, the base material was 70% by weight of a mixture of fused alumina and spinel (MgAl 2 O 4 ) (average particle size 200 μm, weight ratio 1: 1), clay And calcined alumina (average particle size 4 μm, weight ratio 1: 5).
(実施例29)
実施例29の電子部品焼成用治具は、基材の材料を、電融アルミナとコーディエライト(2MgO・2Al2O3・5SiO3)との混合物(平均粒径200μm、重量比率1:1)70重量%と、粘土と仮焼アルミナとの混合物(平均粒径4μm、重量比率1:5)30重量%とし、予備焼成温度を700℃とし、本焼成温度を1600℃とした以外は、実施例2と同様に形成した。(Example 29)
In the electronic component firing jig of Example 29, the base material was a mixture of fused alumina and cordierite (2MgO.2Al 2 O 3 .5SiO 3 ) (average particle size 200 μm, weight ratio 1: 1). ) 70% by weight, a mixture of clay and calcined alumina (average particle size 4 μm, weight ratio 1: 5) 30% by weight, pre-baking temperature 700 ° C., main baking temperature 1600 ° C. It formed similarly to Example 2.
(比較例1)
比較例1の電子部品焼成用治具は、基材及び保護層の材料として実施例2と同様の材料を用い、基材を予備焼成せず、100℃で乾燥させて、その上に保護層を形成し、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 1)
The electronic component firing jig of Comparative Example 1 uses the same material as that of Example 2 as the material of the base material and the protective layer. The base material is not pre-fired and dried at 100 ° C., and the protective layer is formed thereon. The base material and the protective layer were baked at 1800 ° C. and formed.
(比較例2)
比較例2の電子部品焼成用治具は、基材及び保護層の材料として実施例2と同様の材料を用い、基材を予備焼成温度以上の1800℃で焼成し、その上に保護層を形成し、さらに、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 2)
The electronic component firing jig of Comparative Example 2 uses the same material as that of Example 2 as the material for the base material and the protective layer, and the base material is fired at 1800 ° C., which is equal to or higher than the pre-baking temperature. In addition, the substrate and the protective layer were formed by firing at 1800 ° C.
(比較例3)
比較例3の電子部品焼成用治具は、基材及び保護層の材料として実施例1と同様の材料を用い、基材を予備焼成せず、100℃で乾燥させて、その上に保護層を形成し、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 3)
The electronic component firing jig of Comparative Example 3 uses the same material as that of Example 1 as the material of the base material and the protective layer. The base material is not pre-fired and dried at 100 ° C., and the protective layer is formed thereon. The base material and the protective layer were baked at 1800 ° C. and formed.
(比較例4)
比較例4の電子部品焼成用治具は、基材及び保護層の材料として実施例1と同様の材料を用い、基材を予備焼成温度以上の1800℃で焼成し、その上に保護層を形成し、さらに、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 4)
The electronic component firing jig of Comparative Example 4 uses the same material as that of Example 1 as the material of the base material and the protective layer, and the base material is fired at 1800 ° C., which is equal to or higher than the pre-baking temperature. In addition, the substrate and the protective layer were formed by firing at 1800 ° C.
(試験)
上記実施例1〜29及び比較例1〜4の電子部品焼成用治具を用い、以下の評価試験を行なった。
まず、各電子部品焼成用治具を、3時間かけて300℃から1400℃に熱し、次いで、3時間かけて1400℃から300℃に冷やし、このような熱サイクル試験を100回繰り返したものを評価用サンプルとして用いた。
このサンプルを用いて、上記と同様な熱サイクル試験をさらに繰り返し行い、20サイクル毎に剥離の有無及び亀裂の発生を観察した。なお、剥離の有無は、目視により行い、亀裂の発生は、マイクロスコープを用いて行なった。
この試験の結果を、以下の表1に示した。(test)
The following evaluation tests were performed using the electronic component firing jigs of Examples 1 to 29 and Comparative Examples 1 to 4.
First, each electronic component firing jig was heated from 300 ° C. to 1400 ° C. over 3 hours, then cooled from 1400 ° C. to 300 ° C. over 3 hours, and this thermal cycle test was repeated 100 times. Used as an evaluation sample.
Using this sample, the same thermal cycle test as described above was further repeated, and the presence or absence of peeling and the occurrence of cracks were observed every 20 cycles. In addition, the presence or absence of peeling was performed visually, and generation | occurrence | production of the crack was performed using the microscope.
The results of this test are shown in Table 1 below.
(結果)
実施例1〜29の電子部品焼成用治具は、剥離も、亀裂もなく、実使用上全く問題はなかった。
比較例1〜4の電子部品焼成用治具は、熱サイクル100回で亀裂が発生し、120〜140回で剥離が発生した。(result)
The jigs for firing electronic parts of Examples 1 to 29 were free from peeling and cracking and had no problem in actual use.
In the electronic component firing jigs of Comparative Examples 1 to 4, cracks occurred after 100 thermal cycles, and peeling occurred after 120 to 140 times.
また、保護層を二層とした下記実施例30,比較例5,6の電子部品焼成用治具を作成した。 Moreover, the jig | tool for electronic component baking of the following Example 30 and the comparative examples 5 and 6 which made the protective layer into two layers was created.
(実施例30)
実施例30の電子部品焼成用治具は、基材上に、保護層として以下の二層を形成した以外は、実施例1と同様に形成した。
基材の直ぐ上の保護層は、材料として、平均粒径50μmのアルミナ96重量%と、平均粒径4μmのアルミナ4重量%とを用いた。これら材料を混合した後、水とバインダー(ポリビニルアルコール)を添加して均一になるように、さらに混合してスラリーとし、このスラリーを前記基材表面上にスプレーコートし、約100℃で乾燥させて厚さ100μmの一層目の保護層を形成した。(Example 30)
The electronic component firing jig of Example 30 was formed in the same manner as in Example 1 except that the following two layers were formed as protective layers on the substrate.
The protective layer immediately above the base material was made of 96 wt% alumina having an average particle diameter of 50 μm and 4 wt% alumina having an average particle diameter of 4 μm. After mixing these materials, water and a binder (polyvinyl alcohol) are added and mixed uniformly to form a slurry, which is then spray coated onto the substrate surface and dried at about 100 ° C. Thus, a first protective layer having a thickness of 100 μm was formed.
その上の保護層は、材料として、平均粒径150μmのイットリア安定化ジルコニア96重量%と、平均粒径1μmのイットリア安定化ジルコニア4重量%とを用いた。これら材料を混合した後、水とバインダー(ポリビニルアルコール)を添加して均一になるように、さらに混合してスラリーとし、このスラリーを前記第一保護層表面上にスプレーコートし、約100℃で乾燥させて厚さ150μmの二層目の保護層を形成した。
このように、基材上に、二層の保護層を形成し、1800℃で本焼成して、実施例30の電子部品焼成用治具を形成した。The protective layer thereon was made of 96% by weight yttria-stabilized zirconia having an average particle diameter of 150 μm and 4% by weight yttria-stabilized zirconia having an average particle diameter of 1 μm. After mixing these materials, water and a binder (polyvinyl alcohol) are added and mixed uniformly to form a slurry, and this slurry is spray-coated on the surface of the first protective layer at about 100 ° C. A second protective layer having a thickness of 150 μm was formed by drying.
In this way, two protective layers were formed on the base material, followed by main baking at 1800 ° C., thereby forming the electronic component baking jig of Example 30.
(比較例5)
比較例5の電子部品焼成用治具は、基材及び保護層の材料として実施例30と同様の材料を用い、基材を予備焼成せず、100℃で乾燥させて、その上に保護層を形成し、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 5)
The electronic component firing jig of Comparative Example 5 uses the same material as that of Example 30 as the material of the base material and the protective layer. The base material is not pre-fired and dried at 100 ° C., and the protective layer is formed thereon. The base material and the protective layer were baked at 1800 ° C. and formed.
(比較例6)
比較例6の電子部品焼成用治具は、基材及び保護層の材料として実施例30と同様の材料を用い、基材を予備焼成温度以上の1800℃で焼成し、その上に保護層を形成し、さらに、この基材及び保護層を1800℃で焼成して形成した。(Comparative Example 6)
The electronic component firing jig of Comparative Example 6 uses the same material as that of Example 30 as the material of the base material and the protective layer, and the base material is fired at 1800 ° C., which is equal to or higher than the pre-baking temperature. In addition, the substrate and the protective layer were formed by firing at 1800 ° C.
(結果)
実施例30及び比較例5,6の電子部品焼成用治具を用い、上記と同様に評価試験を行ない、熱サイクル後の剥離の有無、亀裂の発生を観察した。
実施例30の電子部品焼成用治具は、剥離も、亀裂もなく、実使用上全く問題はなかった。
比較例5の電子部品焼成用治具は、熱サイクル100回で亀裂が発生し、140回で剥離が発生し、比較例6の電子部品焼成用治具は、熱サイクル100回で亀裂が発生し、120回で剥離が発生した。(result)
Using the electronic component firing jigs of Example 30 and Comparative Examples 5 and 6, an evaluation test was performed in the same manner as described above, and the presence or absence of peeling after thermal cycling and the occurrence of cracks were observed.
The electronic component firing jig of Example 30 was free from peeling and cracking, and had no problem in actual use.
The jig for firing electronic parts of Comparative Example 5 cracked after 100 heat cycles and peeled after 140 times. The jig for firing electronic parts of Comparative Example 6 cracked after 100 heat cycles. Then, peeling occurred at 120 times.
Claims (2)
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| JP2009517770A JP5474538B2 (en) | 2007-06-04 | 2008-05-19 | Manufacturing method of electronic component firing jig |
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| JP2007148465 | 2007-06-04 | ||
| JP2007148465 | 2007-06-04 | ||
| JP2009517770A JP5474538B2 (en) | 2007-06-04 | 2008-05-19 | Manufacturing method of electronic component firing jig |
| PCT/JP2008/059114 WO2008149656A1 (en) | 2007-06-04 | 2008-05-19 | Method for manufacturing electronic component baking jig |
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| JPWO2008149656A1 JPWO2008149656A1 (en) | 2010-08-26 |
| JP5474538B2 true JP5474538B2 (en) | 2014-04-16 |
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| JP5758084B2 (en) * | 2010-03-31 | 2015-08-05 | 一般財団法人電力中央研究所 | A crucible for solid cathode treatment of metal fuel reprocessing. |
| WO2026083711A1 (en) * | 2024-10-18 | 2026-04-23 | 三井金属株式会社 | Ceramic sheet sintered compact and method for producing same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10275746A (en) * | 1997-03-28 | 1998-10-13 | Hitachi Aic Inc | Manufacture of solid-state electrolytic capacitor |
| JP2000103689A (en) * | 1998-09-28 | 2000-04-11 | Kyocera Corp | Alumina sintered body, method for producing the same, and plasma-resistant member |
| JP2002114578A (en) * | 2000-09-29 | 2002-04-16 | Mitsui Mining & Smelting Co Ltd | Jig for firing electronic components |
| JP2002362986A (en) * | 2001-06-04 | 2002-12-18 | Yotai Refractories Co Ltd | Method for producing tool material for firing electronic ceramics |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004137114A (en) * | 2002-10-18 | 2004-05-13 | Mitsui Mining & Smelting Co Ltd | Jig for firing electronic components |
| JP4549091B2 (en) * | 2004-03-31 | 2010-09-22 | 三井金属鉱業株式会社 | Electronic component firing jig |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10275746A (en) * | 1997-03-28 | 1998-10-13 | Hitachi Aic Inc | Manufacture of solid-state electrolytic capacitor |
| JP2000103689A (en) * | 1998-09-28 | 2000-04-11 | Kyocera Corp | Alumina sintered body, method for producing the same, and plasma-resistant member |
| JP2002114578A (en) * | 2000-09-29 | 2002-04-16 | Mitsui Mining & Smelting Co Ltd | Jig for firing electronic components |
| JP2002362986A (en) * | 2001-06-04 | 2002-12-18 | Yotai Refractories Co Ltd | Method for producing tool material for firing electronic ceramics |
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| JPWO2008149656A1 (en) | 2010-08-26 |
| WO2008149656A1 (en) | 2008-12-11 |
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