JP4457056B2 - Method of manufacturing ceramic member for bonding, ceramic member for bonding, bonded body, vacuum switch, and vacuum container - Google Patents

Method of manufacturing ceramic member for bonding, ceramic member for bonding, bonded body, vacuum switch, and vacuum container Download PDF

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JP4457056B2
JP4457056B2 JP2005236642A JP2005236642A JP4457056B2 JP 4457056 B2 JP4457056 B2 JP 4457056B2 JP 2005236642 A JP2005236642 A JP 2005236642A JP 2005236642 A JP2005236642 A JP 2005236642A JP 4457056 B2 JP4457056 B2 JP 4457056B2
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nickel
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ceramic member
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JP2005336055A (en
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友亮 牧野
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NGK Spark Plug Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H33/00—High-tension or heavy-current switches with arc-extinguishing or arc-preventing means
    • H01H33/60—Switches wherein the means for extinguishing or preventing the arc do not include separate means for obtaining or increasing flow of arc-extinguishing fluid
    • H01H33/66—Vacuum switches
    • H01H33/662—Housings or protective screens
    • H01H33/66207—Specific housing details, e.g. sealing, soldering or brazing
    • H01H2033/66215—Details relating to the soldering or brazing of vacuum switch housings

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Description

本発明は、例えば金属とセラミックを接合する場合のように、接合強度、気密性等が要求される部材などに関し、接合用セラミック部材の製造方法、接合用セラミック部材、接合体、真空スイッチ、及び真空容器に関するものである。   The present invention relates to a member that requires bonding strength, airtightness, and the like, for example, when a metal and ceramic are bonded, a method for manufacturing a bonding ceramic member, a bonding ceramic member, a bonded body, a vacuum switch, and the like It relates to a vacuum vessel.

従来より、セラミック基材の表面にメタライズを施す方法として、モリブデン−マンガン法（Ｍｏ−Ｍｎ法；テレフンケン法）が知られている。
このＭｏ−Ｍｎ法は、ＷやＭｏ等の高融点金属の粉末に、Ｍｎ粉末、Ｔｉ粉末、ガラス成分（ＳｉＯ2）等の接合助剤を添加し、有機バインダと混合してペーストとしたメタライズインクを、セラミック基材上に塗布し焼き付ける方法（焼成方法）である。 Conventionally, a molybdenum-manganese method (Mo-Mn method; Telefunken method) is known as a method for metallizing the surface of a ceramic substrate.
This Mo-Mn method is a metallized paste in which a bonding aid such as Mn powder, Ti powder, glass component (SiO 2 ), etc. is added to a powder of a high melting point metal such as W or Mo and mixed with an organic binder. This is a method (firing method) in which ink is applied onto a ceramic substrate and baked.

上述したＭｏ−Ｍｎ法による従来技術では、メタライズの焼き付け温度は、１３００〜１５００℃の高温であり、炉の構造、光熱費、耐熱消耗材等、焼成費用が大きくかかるという問題があった。   In the prior art based on the Mo-Mn method described above, the baking temperature of the metallization is a high temperature of 1300 to 1500 ° C., and there is a problem that the firing cost such as the furnace structure, the heat and heat consumption, and the heat-consuming consumables is high.

また、高温の焼き付けにより、セラミック自体の変形も生じ、寸法精度を満足しない製品が発生するという問題もあった。
この対策として、従来の組成のメタライズインクを、１３００℃未満の低温で焼き付けることが考えられるが、この場合は、十分な接合強度が得られないという問題があった。 Further, there is a problem that the ceramic itself is deformed by baking at a high temperature, resulting in a product that does not satisfy the dimensional accuracy.
As a countermeasure, it is conceivable to bake a metallized ink having a conventional composition at a low temperature of less than 1300 ° C. However, in this case, there is a problem that sufficient bonding strength cannot be obtained.

また、Ｍｏ−Ｍｎ法で形成したメタライズ層に、他の金属部材等をロー付け接合する場合には、良好な接合を得るために、ロー材の濡れ性を向上させる必要があり、Ｎｉメッキ及びその後のシンター（焼成）等の後処理が不可欠となっているが、この後処理によって、製造工程が複雑になるという問題もあった。   In addition, when brazing and joining other metal members or the like to the metallized layer formed by the Mo-Mn method, it is necessary to improve the wettability of the brazing material in order to obtain good joining, and Ni plating and Subsequent post-treatment such as sintering (firing) is indispensable, but this post-treatment has a problem that the manufacturing process becomes complicated.

本発明は前記課題を解決するためになされたものであり、その目的は、低温での焼成でも十分なメタライズの接合強度が得られ、しかもその製造工程を簡易化できる接合用セラミック部材の製造方法、接合用セラミック部材、接合体、真空スイッチ、及び真空容器を提供することにある。   The present invention has been made to solve the above-mentioned problems, and the object thereof is to provide a method for producing a ceramic member for joining which can obtain sufficient metallized joining strength even by firing at a low temperature and can simplify the production process. It is to provide a ceramic member for bonding, a bonded body, a vacuum switch, and a vacuum vessel.

（１）前記目的を達成するための請求項１の発明は、
モリブデン粉末及びニッケル粉末を含有する第１混合物と、有機バインダとを混合した第１ペーストを、セラミック焼成体であるセラミック基材に塗布し乾燥して第１層を形成する第１工程と、ニッケル粉末又は酸化ニッケル粉末と、銅粉末、酸化銅粉末、マンガン粉末、及び酸化マンガン粉末のうち少なくとも１種と、を含有する第２混合物、あるいは、ニッケル−銅の合金粉末又はニッケル−マンガンの合金粉末を含有する第２混合物と、有機バインダとを混合した第２ペーストを、前記第１層上に塗布し乾燥して第２層を形成する第２工程と、前記第１層及び第２層を加熱して焼き付ける第３工程と、を備え、前記第２混合物として、前記ニッケル成分を３５〜７５重量％と、銅成分又はマンガン成分を２５〜６５重量％と、を含有する混合物を用いることを特徴とする接合用セラミック部材の製造方法を要旨とする。 (1) The invention of claim 1 for achieving the object is as follows:
A first mixture comprising molybdenum powder, and nickel powder, a first step of forming a first paste obtained by mixing an organic binder, the first layer was applied to the ceramic substrate is a ceramic fired body dry, nickel Second mixture containing powder or nickel oxide powder and at least one of copper powder, copper oxide powder, manganese powder, and manganese oxide powder, or nickel-copper alloy powder or nickel-manganese alloy powder a second mixture containing a second paste prepared by mixing an organic binder, and a second step of forming a second layer was applied and dried on the first layer, said first and second layers e Bei a third step of baking heat to, the, as the second mixture, to contain and 35 to 75 wt% of the nickel component, and 25 to 65 wt% of copper component or a manganese component, Mixture summarized as method for producing a bonded ceramic component, which comprises using a.

尚、ここでは、第２混合物として、ニッケル粉末又は酸化ニッケル粉末と、銅粉末、酸化銅粉末、マンガン粉末、及び酸化マンガン粉末のうち少なくとも１種と、を含有する第２混合物か、あるいは、ニッケル−銅の合金粉末又はニッケル−マンガンの合金粉末を含有する第２混合物を用いる。   Here, the second mixture is a second mixture containing nickel powder or nickel oxide powder and at least one of copper powder, copper oxide powder, manganese powder, and manganese oxide powder, or nickel. A second mixture containing copper alloy powder or nickel-manganese alloy powder is used.

本発明では、第１ペースト中に、Ｎｉを含むので、Ｎｉが高融点金属のＭｏと反応し、メタライズ層における焼結を促進する。これにより、例えば１０８０〜１１８０℃の低温でも十分に焼結が可能である。   In the present invention, since the first paste contains Ni, Ni reacts with Mo, which is a refractory metal, and promotes sintering in the metallized layer. Thereby, for example, sintering can be sufficiently performed even at a low temperature of 1080 to 1180 ° C.

その結果、従来と比べて、炉の構造、光熱費、耐熱消耗材等に関する焼成費用を少なくすることができる。また、低温での焼き付けにより、セラミック自体の変形も生じにくく、高い寸法精度が得られる。更に、低温でも十分に焼結ができるので、高い接合強度を確保できる。   As a result, it is possible to reduce the firing cost related to the furnace structure, the utility cost, the heat-resistant consumables, and the like as compared with the conventional case. In addition, the ceramic itself is not easily deformed by baking at a low temperature, and high dimensional accuracy is obtained. Furthermore, since sufficient sintering can be performed even at a low temperature, a high bonding strength can be ensured.

特に、本発明では、第２ペースト中に、Ｎｉに加え、ＣｕやＭｎを添加しているので、融点が下がり、（メタライズ層の上に）緻密な合金層が形成できる。このため、従来の焼き付け後のＮｉメッキ等の手間のかかる後処理がなくとも、良好なロー付けができる。つまり、大幅な製造工程の簡略化が可能であるという顕著な効果を奏する。   In particular, in the present invention, since Cu and Mn are added in addition to Ni in the second paste, the melting point is lowered, and a dense alloy layer (on the metallized layer) can be formed. For this reason, it is possible to perform good brazing without a conventional post-baking process such as Ni plating. That is, there is a remarkable effect that the manufacturing process can be greatly simplified.

また、第２層は合金化するため、Ｍｏを含む第１層へのＮｉの過度の拡散が減少し、Ｍｏの過焼結による強度低下を防止できる。
尚、第３工程における焼き付けは、加湿還元雰囲気にて、特に前記１０８０〜１１８０℃の温度範囲にて行うと、製品の接合強度や気密性が高く好適である。
特に本発明では、前記第２混合物として、前記（ニッケル粉末又は酸化ニッケル粉末、あるいは、ニッケル−銅の合金粉末又はニッケル−マンガンの合金粉末における）ニッケル成分を３５〜７５重量％と、（銅粉末、酸化銅粉末、又はニッケル−銅の合金粉末における）銅成分又は（マンガン粉末、酸化マンガン粉末、又はニッケル−マンガンの合金粉末における）マンガン成分を２５〜６５重量％と、を含有する混合物を用いる。
本発明では、第２混合物中に、Ｎｉ分を３５〜７５重量％含むので、メタライズ層との接合強度及び気密性が高い。
また、Ｃｕ分又はＭｎ分は、２５重量％以上であるので、ロー付け性に優れ、且つ高い強度が得られる。更に、Ｃｕ分又はＭｎ分は、６５重量％以下であるので、メタライズ層への浸透を抑制でき、よって、セラミック基材とメタライズ層との間の接合強度を確保することができる。
尚、第２混合物中に、酸化ニッケルや酸化銅等の酸化金属を含む場合には、更に、ＳｉＯ 2 を加えると、一層気密性が向上するので好適である。 Moreover, since the second layer is alloyed, excessive diffusion of Ni into the first layer containing Mo is reduced, and strength reduction due to over-sintering of Mo can be prevented.
Note that baking in the third step is preferably performed in a humidified and reduced atmosphere, particularly in the temperature range of 1080 to 1180 ° C. because of high bonding strength and airtightness of the product.
Particularly, in the present invention, as the second mixture, the nickel component (in nickel powder or nickel oxide powder, or nickel-copper alloy powder or nickel-manganese alloy powder) is contained in an amount of 35 to 75% by weight (copper powder). 25 to 65 wt% of a copper component (in a copper oxide powder or a nickel-copper alloy powder) or a manganese component (in a manganese powder, a manganese oxide powder or a nickel-manganese alloy powder) .
In the present invention, since the Ni content is 35 to 75% by weight in the second mixture, the bonding strength and the airtightness with the metallized layer are high.
Moreover, since Cu content or Mn content is 25 weight% or more, it is excellent in brazing property and high intensity | strength is obtained. Furthermore, since the Cu content or the Mn content is 65% by weight or less, the penetration into the metallized layer can be suppressed, and thus the bonding strength between the ceramic substrate and the metallized layer can be ensured.
When the second mixture contains a metal oxide such as nickel oxide or copper oxide, it is preferable to add SiO 2 since the airtightness is further improved.

・なお、前記第１混合物として、前記モリブデン成分を７０〜９４重量％と、前記ニッケル成分を１〜１０重量％と、を含有する混合物を用いてもよい。 In addition, as the first mixture, a mixture containing 70 to 94% by weight of the molybdenum component and 1 to 10% by weight of the nickel component may be used.

この場合には、第１混合物中のＮｉが１重量％以上であるので、Ｎｉが高融点金属のＭｏと反応し、メタライズ層における焼結を促進する。これにより、上述した低温でも十分に焼結が可能である。また、Ｎｉは１０重量％以下であるので、Ｍｏの過焼結を防止でき、よって、セラミック基材とメタライズ層との間の接合強度の不足を防止できる。 In this case, since Ni in the first mixture is 1% by weight or more, Ni reacts with Mo, which is a refractory metal, and promotes sintering in the metallized layer. Thereby, it can sinter enough even at the low temperature mentioned above. Moreover, since Ni is 10 weight% or less, oversintering of Mo can be prevented, and hence insufficient bonding strength between the ceramic substrate and the metallized layer can be prevented.

また、第１混合物中に、Ｍｏを７０〜９４重量％含むので、強固なメタライズ層を形成することができる。
・また、前記第１混合物中に、更に、（例えば酸化珪素粉末として）酸化珪素成分を２〜２３重量％含んでもよい。 Moreover, since 70 to 94 weight% of Mo is contained in the first mixture, a strong metallized layer can be formed.
· In addition, in the first mixture, further, (e.g., as silicon oxide powder), a silicon oxide component may also 2 to 23% by weight containing I.

この場合には、第１混合物中に酸化珪素（ＳｉＯ2）成分を２〜２３重量％含むので、セラミック基材とメタライズ層との接合性に一層優れている。 In this case, since the silicon oxide in the first mixture comprising the (SiO 2) component 2 to 23 wt%, that has more excellent bonding between the ceramic substrate and the metallization layer.

（２）請求項２の発明は、
セラミック焼成体であるセラミック基材表面に、モリブデン及びニッケルを含有する下層であるメタライズ層を備えるとともに、前記メタライズ層の表面側に、ニッケルと、銅又はマンガンと、を含有する上層である合金層を備え、前記合金層は、前記ニッケルを３６〜６１．３重量％と、銅を３３〜６０重量％又はマンガンを２〜３０重量％と、を含むことを特徴とする接合用セラミック部材を要旨とする。 ( 2 ) The invention of claim 2
The ceramic substrate surface is a ceramic fired body provided with a metallized layer is a lower layer containing molybdenum and nickel, on the surface side of the metallization layer, a layer containing a nickel, copper or manganese, an alloy e Bei layer, the alloy layer, and 36 to 61.3% by weight of said nickel, bonding ceramic member characterized by comprising, a 2-30 wt% 33 to 60% by weight or manganese copper Is the gist.

本発明では、下層であるメタライズ層中にＮｉを含むので、焼き付けの際の焼結を促進し、低温でも十分に焼結が可能である。   In the present invention, since the lower metallization layer contains Ni, sintering during baking is promoted and sufficient sintering is possible even at low temperatures.

その結果、従来と比べて、炉の構造、光熱費、耐熱消耗材等に関する焼成費用を少なくすることができる。また、低温での焼き付けにより、高い寸法精度が得られる。更に、低温でも十分に焼結ができるので、高い接合強度を確保できる。
特に、本発明では、上層である合金層中に、Ｎｉに加えＣｕやＭｎを含んでいるので、焼き付けの際に、融点が下がり、緻密な合金層が形成できる。このため、従来の焼き付け後のＮｉメッキ等の後処理がなくとも、良好なロー付けができる。つまり、製造工程が大幅に簡略化できる。 As a result, it is possible to reduce the firing cost related to the furnace structure, the utility cost, the heat-resistant consumables, and the like as compared with the conventional case. Further, high dimensional accuracy can be obtained by baking at a low temperature. Furthermore, since sufficient sintering can be performed even at a low temperature, a high bonding strength can be ensured.
In particular, in the present invention, since the upper alloy layer contains Cu and Mn in addition to Ni, the melting point decreases during baking, and a dense alloy layer can be formed. For this reason, it is possible to perform good brazing without the post-treatment such as Ni plating after baking. That is, the manufacturing process can be greatly simplified.

特に本発明では、前記合金層は、前記ニッケルを３６〜６１．３重量％と、銅を３３〜６０重量％又はマンガンを２〜３０重量％と、を含む。Particularly in the present invention, the alloy layer contains 36 to 61.3% by weight of nickel, 33 to 60% by weight of copper, or 2 to 30% by weight of manganese.
本発明では、合金層中に、Ｎｉ分を３６〜６１．３重量％含むので、合金層のメタライズ層との接合強度及び気密性が高い。  In the present invention, since 36 to 61.3% by weight of Ni is contained in the alloy layer, the bonding strength and hermeticity of the alloy layer with the metallized layer are high.
また、Ｃｕ分は、３３重量％以上であるので、合金層のロー付け性に優れ、且つ高い強度が得られる。しかも、Ｃｕ分は、６０重量％以下であるので、セラミック基材とメタライズ層との間の接合強度の向上に寄与する。  Moreover, since Cu content is 33 weight% or more, it is excellent in the brazing property of an alloy layer, and high intensity | strength is obtained. And since Cu content is 60 weight% or less, it contributes to the improvement of the joint strength between a ceramic base material and a metallizing layer.
一方、Ｍｎ分は、２重量％以上であるので、合金層のロー付け性に優れ、且つ高い強度が得られる。しかも、Ｍｎ分は、３０重量％以下であるので、セラミック基材とメタライズ層との間の接合強度の向上に寄与する。  On the other hand, since the Mn content is 2% by weight or more, the brazing property of the alloy layer is excellent and high strength is obtained. And since Mn content is 30 weight% or less, it contributes to the improvement of the joint strength between a ceramic base material and a metallization layer.

・なお、前記メタライズ層は、モリブデンを７１〜８８重量％と、ニッケルを０．７〜５．５重量％と、を含んでもよい。 - In addition, the metallized layer has a 71 to 88 wt% molybdenum, and 0.7 to 5.5 wt% of nickel, may also including I a.

この場合は、メタライズ層中のＮｉが０.７重量％以上であるので、低温でも十分に焼結が可能である。また、Ｎｉは５.５重量％以下であるので、Ｍｏの過焼結を防止でき、セラミック基材とメタライズ層との間の接合強度の不足を防止できる。 In this case, since Ni in the metallized layer is 0.7% by weight or more, sufficient sintering is possible even at a low temperature. Moreover, since Ni is 5.5 weight% or less, oversintering of Mo can be prevented, and insufficient bonding strength between the ceramic substrate and the metallized layer can be prevented.

また、メタライズ層中に、Ｍｏを７１〜８８重量％含むので、強固なメタライズ層となる。
・また、前記メタライズ層に、更に、酸化物換算した酸化珪素成分を３．０〜１８．０重量％含んでもよい。 Further, since 71 to 88% by weight of Mo is contained in the metallized layer, it becomes a strong metallized layer.
- Also, the metallization layer, further, the oxide-converted silicon oxide component may also containing I 3.0 to 18.0 wt%.

この場合は、メタライズ層中に酸化珪素（ＳｉＯ2）成分を３．０〜１８．０重量％含むので、セラミック部材とメタライズ層との接合性が極めて高い。 In this case, because they contain silicon oxide metallization layer in (SiO 2) component 3.0 to 18.0 wt%, bonding strength between the ceramic member and the metallizing layer is not very high.

（３）請求項３の発明は、
前記請求項２に記載の接合用セラミック部材に、少なくとも前記メタライズ層及び前記合金層を介して金属部材を接合したことを特徴とする接合体を要旨とする。 ( 3 ) The invention of claim 3
The gist of the present invention is a joined body in which a metal member is joined to the joining ceramic member according to claim 2 through at least the metallized layer and the alloy layer.

本発明は、接合用セラミック部材と金属部材とを、上述したメタライズ層及び合金層を介して接合したものである。つまり、セラミック基材の表面にメタライズ層を形成し、更にその上に合金層を形成した接合用セラミック部材に対して、その合金層と金属部材を例えばロー材により接合したものである。 In the present invention, a joining ceramic member and a metal member are joined through the metallized layer and the alloy layer described above. That is, forming a metallized layer on the surface of the ceramic base material, further the bonding ceramic member formed with an alloy layer thereon, Ru der those joining the alloy layer and the metal member by, for example, brazing material.

従って、従来の様な（メタライズ層の表面の）ニッケルメッキ及びその後のシンター処理が不要であり、合金層に直接に金属部材をロー付けすることができる。よって、その製造工程が少なく、製造コストが低い。また、この接合体は、高い接合強度及び高い寸法精度を有する。   Therefore, the conventional nickel plating (on the surface of the metallized layer) and subsequent sintering treatment are unnecessary, and the metal member can be brazed directly to the alloy layer. Therefore, the manufacturing process is few and the manufacturing cost is low. Moreover, this joined body has high joint strength and high dimensional accuracy.

（４）請求項４の発明は、
前記請求項２に記載の接合用セラミック部材に、少なくとも前記メタライズ層及び前記合金層を介して他の接合用セラミック部材を接合したことを特徴とする接合体を要旨とする。 ( 4 ) The invention of claim 4
The gist of the present invention is a joined body in which another joining ceramic member is joined to the joining ceramic member according to claim 2 via at least the metallized layer and the alloy layer.

本発明は、接合用セラミック部材と他の接合用セラミック部材とを、上述したメタライズ層及び合金層を介して接合したものである。 The present invention, a bonding ceramic member and the other joining ceramic component, Ru der those bonded via the metallized layer and the alloy layer described above.

例えばメタライズ層及び合金層を形成した２つの接合用セラミック部材を用い、両合金層同士をロー材を用いて接合した接合体が挙げられる。
従って、前記請求項３と同様に、従来の様なニッケルメッキ及びその後のシンター処理が不要であり、合金層に直接に金属部材をロー付けすることができる。よって、製造コストが低い。また、この接合体は、高い接合強度及び高い寸法精度を有する。 For example, there may be mentioned a joined body in which two ceramic members for joining on which a metallized layer and an alloy layer are formed are joined together using a brazing material.
Therefore, similarly to the third aspect , the conventional nickel plating and the subsequent sintering treatment are unnecessary, and the metal member can be brazed directly to the alloy layer. Therefore, the manufacturing cost is low. Moreover, this joined body has high joint strength and high dimensional accuracy.

（５）請求項５の発明は、
前記請求項３又は４の接合体を備えたことを特徴とする真空スイッチを要旨とする。 ( 5 ) The invention of claim 5
The gist of the present invention is a vacuum switch comprising the joined body according to claim 3 or 4 .

本発明は、上述した接合体を用いた真空スイッチである。この真空スイッチとは、例えばセラミック製の絶縁バルブを用いた電気回路開閉器であり、特に高電圧、大電流の開閉に好適なものである。   The present invention is a vacuum switch using the above-described joined body. The vacuum switch is an electric circuit switch using an insulating valve made of ceramic, for example, and is particularly suitable for high voltage and large current switching.

（６）請求項６の発明は、
前記請求項３又は４の接合体を備えたことを特徴とする真空容器を要旨とする。
本発明は、上述した真空スイッチなどに用いられる真空容器（例えば絶縁バルブ）であり、この真空容器内に電極などを配置することにより、真空スイッチ（電気回路開閉器）を形成することができる。 ( 6 ) The invention of claim 6
A gist is a vacuum vessel provided with the joined body according to claim 3 or 4 .
The present invention is a vacuum vessel (for example, an insulating valve) used for the above-described vacuum switch, and a vacuum switch (electric circuit switch) can be formed by disposing an electrode or the like in the vacuum vessel.

以上詳述した様に、請求項１の発明の接合用セラミック部材の製造方法により、メタライズの低温での十分な焼結が可能であるので、製造コストを低減できる。また、高い寸法精度及び高い接合強度を実現できる。しかも、従来のメッキ処理等が不要であるので、その点からも、製造工程等を簡易化できる。   As described in detail above, since the metallizing can be sufficiently sintered at a low temperature by the method for manufacturing a ceramic member for bonding according to the first aspect of the present invention, the manufacturing cost can be reduced. Moreover, high dimensional accuracy and high bonding strength can be realized. In addition, since the conventional plating process or the like is unnecessary, the manufacturing process and the like can be simplified from this point.

また、請求項２の発明の接合用セラミック部材は、低温でも十分に焼結が進んだメタライズ層を有するので、前記請求項１と同様に、焼成費用を低減でき、高い寸法精度及び高い接合強度を有する。しかも、従来のメッキ処理等が不要であるので、その点からも、製造工程等を簡易化できる。 In addition, since the ceramic member for bonding according to the second aspect of the present invention has a metallized layer that has been sufficiently sintered even at a low temperature, as in the case of the first aspect, the firing cost can be reduced, and high dimensional accuracy and high bonding strength. Have In addition, since the conventional plating process or the like is unnecessary, the manufacturing process and the like can be simplified from this point.

更に、請求項３及び請求項４の接合体は、上述した接合用セラミック部材を有するので、前記と同様に、コストの低減や高い接合強度及び高い寸法精度という利点がある。
その上、請求項５の発明の真空スイッチ及び請求項６の発明の真空容器は、上述した接合用セラミック部材を備えた接合体を有するので、前記と同様に、コストの低減や高い接合強度及び高い寸法精度という利点がある。 Furthermore, since the joined body of claim 3 and claim 4 has the joining ceramic member described above, there are advantages such as cost reduction, high joining strength, and high dimensional accuracy, as described above.
In addition, since the vacuum switch of the invention of claim 5 and the vacuum container of the invention of claim 6 have the joined body provided with the above-described joining ceramic member, the cost reduction, high joining strength and There is an advantage of high dimensional accuracy.

以下、本発明の、接合用セラミック部材の製造方法、接合用セラミック部材、接合体、真空スイッチ、及び真空容器の実施の形態の例（実施例）を、図面を参照して説明する。
（実施例１）
ここでは、接合用セラミック部材と金属部材の接合体を例に挙げる。 Hereinafter, an example (example) of an embodiment of a manufacturing method of a joining ceramic member, a joining ceramic member, a joined object, a vacuum switch, and a vacuum vessel of the present invention is explained with reference to drawings.
Example 1
Here, a joined body of a joining ceramic member and a metal member is taken as an example.

ａ）図１に模式的に示す様に、本実施例では、接合用セラミック部材１と金属部材３とがロー材５により接合されて接合体７が形成されている。
詳しくは、接合用セラミック部材１は、セラミック基材９上にメタライズ層（下層）１１が形成され、このメタライズ層１１上に合金層（上層）１３が形成され、合金層１３と金属部材３とがロー材５により接合され、これにより接合用セラミック部材１と金属部材３とが接合一体化されている。 a) As schematically shown in FIG. 1, in this embodiment, a joining ceramic member 1 and a metal member 3 are joined together by a brazing material 5 to form a joined body 7.
Specifically, in the bonding ceramic member 1, a metallized layer (lower layer) 11 is formed on a ceramic substrate 9, an alloy layer (upper layer) 13 is formed on the metallized layer 11, and the alloy layer 13, the metal member 3, Are joined by the brazing material 5, whereby the joining ceramic member 1 and the metal member 3 are joined and integrated.

特に、本実施例では、メタライズ層１１中に、Ｍｏを７１〜８８重量％と、Ｎｉを０．７〜５．５重量％と、酸化物換算したＳｉＯ2を３〜１８重量％含んでおり、合金層１３中に、Ｎｉを３６〜６１．３重量％と、Ｃｕを３３〜６０重量％（又はＭｎを２〜３０重量％）とを含んでいる。 In particular, in this example, the metallized layer 11 contains 71 to 88% by weight of Mo, 0.7 to 5.5% by weight of Ni, and 3 to 18% by weight of SiO 2 in terms of oxide. The alloy layer 13 contains 36 to 61.3% by weight of Ni and 33 to 60% by weight of Cu (or 2 to 30% by weight of Mn).

従って、本実施例の接合体７は、後の実験例からも明らかな様に、セラミック基材９とメタライズ層１１との接合強度が高く気密性にも優れている。
また、従来の様に、メッキ処理等を施さなくとも、合金層１３にて金属部材３とのロー付けが可能であるので、製造工程を大幅に簡易化できる。 Therefore, the bonded body 7 of the present embodiment has a high bonding strength between the ceramic base material 9 and the metallized layer 11 and is excellent in airtightness, as is apparent from the later experimental examples.
Further, as in the prior art, it is possible to braze the metal member 3 with the alloy layer 13 without performing plating or the like, so that the manufacturing process can be greatly simplified.

ｂ）次に、この接合体７の１例として円形のテストピースの製造方法を、接合用セラミック部材１の製造方法とともに説明する。
1)まず、下記表１に示す様に、Ｍｏ粉末、Ｎｉ粉末、ＳｉＯ2粉末を用いて、第１混合物を作成し、この第１混合物の粉末（例えば８７重量％）を、粉砕混合し、エトセル等の有機バインダ（例えば１３重量％）と混合して第１ペースト（第１メタライズインク）を製造した。 b) Next, a method for producing a circular test piece as an example of the joined body 7 will be described together with a method for producing the joining ceramic member 1.
1) First, as shown in Table 1 below, a first mixture is prepared using Mo powder, Ni powder, and SiO 2 powder, and the powder (for example, 87% by weight) of the first mixture is pulverized and mixed. A first paste (first metallized ink) was produced by mixing with an organic binder such as etosel (for example, 13% by weight).

2)また、同様に、下記表１に示す様に、Ｎｉ粉末、Ｃｕ粉末、Ｍｎ粉末、Ｍｏ粉末、Ｎｉ−Ｃｕ合金粉末、Ｎｉ−Ｍｎ合金粉末の中から選択して、第２混合物を作成し、この第２混合物の粉末（例えば８７重量％）を、粉砕混合し、エトセル等の有機バインダ（例えば１３重量％）と混合して第２ペースト（第２メタライズインク）を製造した。   2) Similarly, as shown in Table 1 below, a second mixture is prepared by selecting from Ni powder, Cu powder, Mn powder, Mo powder, Ni-Cu alloy powder, and Ni-Mn alloy powder. Then, the powder (for example, 87% by weight) of the second mixture was pulverized and mixed and mixed with an organic binder (for example, 13% by weight) such as etose to produce a second paste (second metallized ink).

3)次に、前記第１ペーストを、セラミック焼成体であるアルミナ製（例えばアルミナ９２重量％）のセラミック基材９（例えば厚み５ｍｍ×外径φ３０ｍｍ×内径φ８．５ｍｍの円筒形のテストピース）の表面に、厚み１０〜２０μｍ程度塗布し、乾燥して（後にメタライズ層１１となる）第１層を形成した。   3) Next, the first paste is applied to a ceramic substrate 9 made of alumina (for example, 92% by weight of alumina) (for example, a cylindrical test piece having a thickness of 5 mm, an outer diameter of 30 mm, and an inner diameter of 8.5 mm). The first layer was coated on the surface of the film with a thickness of about 10 to 20 μm and dried (to be later referred to as the metallized layer 11).

4)次に、前記第２ペーストを、前記第１層の表面に対して、その表面全体を覆うように、厚み１０〜２０μｍ程度塗布し、乾燥して（後に合金層１３となる）第２層を形成した。   4) Next, the second paste is applied to the surface of the first layer so as to cover the entire surface, and is dried (afterwards, becomes the alloy layer 13). A layer was formed.

5)次に、前記第１層及び第２層を形成したセラミック基材９を炉中に入れ、ウエッター温度５０℃のＨ2／Ｎ2（１：１）のフォーミングガス雰囲気にて、下記表３に示す様に、１０５０〜１２００℃の温度範囲の温度にて焼成した。これにより、セラミック基材９の表面にメタライズ層１１及び合金層１３を備えた接合用セラミック部材１が得られた。 5) Next, the ceramic substrate 9 on which the first layer and the second layer are formed is put in a furnace, and the following table is formed in a forming gas atmosphere of H 2 / N 2 (1: 1) with a wetter temperature of 50 ° C. As shown in FIG. 3, it was baked at a temperature in the temperature range of 1050 to 1200 ° C. Thereby, the joining ceramic member 1 provided with the metallized layer 11 and the alloy layer 13 on the surface of the ceramic base material 9 was obtained.

6)次に、接合用セラミック部材１とコバール製（Ｆｅ−Ｎｉ−Ｃｏ）の金属部材３をロー付けした。
具体的には、合金層１３と金属部材３（例えば厚み１ｍｍ×外径φ１６ｍｍのコバール円板）との間に、銀ロー材（ＢＡｇ−８）５の箔を配置して、所定のロー付け温度にて加熱して冷却することにより、接合用セラミック部材１と金属部材３とをロー付け接合して接合体７を完成した。 6) Next, the joining ceramic member 1 and the metal member 3 made of Kovar (Fe—Ni—Co) were brazed.
Specifically, a foil of silver brazing material (BAg-8) 5 is disposed between the alloy layer 13 and the metal member 3 (for example, Kovar disk having a thickness of 1 mm × outer diameter φ16 mm), and predetermined brazing is performed. By heating and cooling at a temperature, the joining ceramic member 1 and the metal member 3 were brazed and joined to complete the joined body 7.

つまり、上述した1)〜6)の製造工程によって、下記表１に示す様に、第１及び第２ペーストの成分を違えて、図２に示す様に、実験に供する接合体７として、Ｎo.１〜１０、１５〜２０の円形のテストピース（試料）を作成した。
尚、前記試料のうち、試料No.２〜４、７〜９、１５〜２０の試料が、本発明の範囲内の試料であり、試料No.１、５、６、１０の試料は、本発明の範囲外の参考例の試料である（以下、表１、表２、表３において同様）。 That is, as shown in FIG. 2, the manufacturing processes of 1) to 6) described above differed in the components of the first and second pastes, and as shown in FIG. Circular test pieces (samples) of 0.1 to 10 and 15 to 20 were prepared.
Of the samples, samples Nos. 2 to 4, 7 to 9, and 15 to 20 are samples within the scope of the present invention, and samples Nos. 1, 5, 6, and 10 are It is a sample of a reference example outside the scope of the invention (hereinafter the same as in Table 1, Table 2, and Table 3).

尚、ペースト組成を違えた比較例の試料Ｎo.１１〜１４も作成した。   In addition, comparative samples No. 11 to 14 having different paste compositions were also prepared.

Figure 0004457056
Figure 0004457056

また、製造された接合用セラミック部材１の断面を研磨し、メタライズ層１１及び合金層１３の成分の定量分析を行った。詳しくは、電子プローブマイクロアナライザー（加速電圧；２０ｋＶ、スポット径；５μｍ）により定量分析を行った。その結果を、下記表２に記す。   Moreover, the cross section of the manufactured ceramic member 1 for joining was grind | polished, and the quantitative analysis of the component of the metallization layer 11 and the alloy layer 13 was performed. Specifically, quantitative analysis was performed using an electron probe microanalyzer (acceleration voltage: 20 kV, spot diameter: 5 μm). The results are shown in Table 2 below.

尚、分析は、偏析の影響を少なくするために、各試料とも５箇所行い、その平均値を求めた。また、Ｓｉの重量％は、酸化物換算した値である。更に、各層の残部は、セラミック基材からの拡散によるＡｌ2Ｏ3、ＭｇＯ、ＣａＯ等のガラス成分が占めている。 In addition, in order to reduce the influence of segregation, the analysis was performed at five locations for each sample, and the average value was obtained. Moreover, the weight% of Si is a value in terms of oxide. Furthermore, the remainder of each layer is occupied by glass components such as Al 2 O 3 , MgO, CaO due to diffusion from the ceramic substrate.

Figure 0004457056
Figure 0004457056

ｃ）次に、前記の製造方法にて製造した接合体７の各試料の接合強度を調べた。
具体的には、図３に示す様に、接合体７を金属部材３を下向きにして配置するとともに、セラミック基材９の外周の下端を円筒形の鉄製の受け台２１で支える。この状態で、セラミック基台９の中央の貫通孔２３に、上方より円柱形のステンレス製の打ち抜き棒２５を配置し、打ち抜き棒２５を荷重速度０．５ｍｍ／ｍｉｎで図の下方に移動させる。 c) Next, the bonding strength of each sample of the bonded body 7 manufactured by the above manufacturing method was examined.
Specifically, as shown in FIG. 3, the joined body 7 is arranged with the metal member 3 facing downward, and the lower end of the outer periphery of the ceramic base 9 is supported by a cylindrical iron cradle 21. In this state, a cylindrical stainless steel punching rod 25 is disposed in the central through hole 23 of the ceramic base 9 from above, and the punching rod 25 is moved downward in the figure at a load speed of 0.5 mm / min.

そして、この際の金属部材３が剥がれる時の強度（破壊強度）を、打ち抜き棒２５の上方に配置した荷重計（図示せず）によって測定し、これをロー付け強度とした。このロー付け強度（接合強度）の評価を、各試料の焼成温度別に、下記表３に記す。   Then, the strength (breaking strength) when the metal member 3 peeled at this time was measured by a load meter (not shown) arranged above the punching rod 25, and this was used as brazing strength. The evaluation of this brazing strength (bonding strength) is shown in Table 3 below for each firing temperature of each sample.

尚、前記表３の評価は、１０５０〜１２００℃において、○は１７ＭＰａを上回ることを示し、△は１１〜１７ＭＰａを示し、×は１１ＭＰａ未満を示している。   In the evaluation of Table 3, at 1050 to 1200 ° C., ◯ indicates that it exceeds 17 MPa, Δ indicates 11 to 17 MPa, and × indicates less than 11 MPa.

Figure 0004457056
Figure 0004457056

この表３から明らかな様に、本発明の試料Ｎo.２〜４、７〜９、１５〜２０は、低温での焼成にもかかわらず、メタライズ層は十分に焼結するので、高いロー付け強度が得られ好適である。また、低温での焼結が可能であるので、焼結のためのコストが少なくて済むという利点がある。更に、低温での十分な焼結が可能であるので、高温での焼結に比べて、接合用セラミック部材の寸法精度が高いという効果がある。 As is apparent from Table 3, the samples No. 2 to 4 , 7 to 9 , and 15 to 20 of the present invention are sufficiently brazed because the metallized layer is sufficiently sintered despite firing at a low temperature. Strength is obtained and suitable. Further, since sintering at a low temperature is possible, there is an advantage that the cost for sintering can be reduced. Furthermore, since sufficient sintering at a low temperature is possible, there is an effect that the dimensional accuracy of the ceramic member for bonding is higher than that at high temperature.

特に、本発明の試料Ｎo.２〜４、７〜９、１６、１７、２０のもの（即ち前記表３にて、焼成温度の２カ所以上で「○」がついた試料）は、その接合強度が高く、一層好適である。 In particular, those of specimen No.2~4,7~9,16,17,20 of the present invention (i.e. in Table 3, "○" is attached at two or more places in the firing temperature sample), the The bonding strength is high, which is more preferable.

これに対して、比較例の試料Ｎo.１１〜１４は、ロー付け強度が低く、好ましくない。
ｄ）次に、前記の製造方法にて製造した接合体７の各試料の気密性を調べた。
具体的には、図３に示す接合体７の一方の側を真空にし（１×１０-8Torr以下）、他方の側にヘリウムを充填して、ヘリウムが漏出があるか否かを調べた。 On the other hand, the samples No. 11 to 14 of the comparative example are not preferable because the brazing strength is low.
d) Next, the airtightness of each sample of the joined body 7 manufactured by the above manufacturing method was examined.
Specifically, one side of the joined body 7 shown in FIG. 3 was evacuated (1 × 10 −8 Torr or less), and the other side was filled with helium to examine whether helium leaked or not. .

その結果を、前記表３にて「k」の記号で示した。
この表３から明らかな様に、特に本発明の試料Ｎo.２〜５、７〜９、１５〜２０のものは、気密性に優れていることが分かる。
（実施例２）
次に、実施例２について説明するが、前記実施例１と同様な箇所の説明は省略する。 The result is indicated by the symbol “k” in Table 3 above.
As apparent from Table 3, it can be seen that the samples No. 2 to 5, 7 to 9, and 15 to 20 of the present invention are excellent in airtightness.
(Example 2)
Next, the second embodiment will be described, but the description of the same parts as the first embodiment will be omitted.

ここでは、接合用セラミック部材同士を接合した接合体を例に挙げる。
ａ）図４に模式的に示す様に、本実施例では、アルミナ製の第１接合用セラミック部材３１と同様なアルミナ製の第２接合用セラミック部材３３とがロー材３５により接合されて接合体３７が形成されている。 Here, a bonded body obtained by bonding ceramic members for bonding to each other will be described as an example.
a) As schematically shown in FIG. 4, in this embodiment, the first bonding ceramic member 31 made of alumina and the second bonding ceramic member 33 made of alumina are bonded by a brazing material 35 and bonded. A body 37 is formed.

詳しくは、第１接合用セラミック部材３１は、第１セラミック基材３９上に第１メタライズ層４１が形成されたものであり、この第１メタライズ層４１上には第１合金層４３が形成されている。一方、第２接合用セラミック部材３３は、第２セラミック基材４５上に第２メタライズ層４７が形成されたものであり、この第２メタライズ層４７上には第２合金層４９が形成されている。   Specifically, the first bonding ceramic member 31 is a member in which a first metallized layer 41 is formed on a first ceramic substrate 39, and a first alloy layer 43 is formed on the first metallized layer 41. ing. On the other hand, the second bonding ceramic member 33 is obtained by forming the second metallized layer 47 on the second ceramic substrate 45, and the second alloy layer 49 is formed on the second metallized layer 47. Yes.

そして、第１合金層４３と第２合金層４９とがロー材３５により接合されることにより、第１接合用セラミック部材３１と第２接合用セラミック部材３３とが接合されて一体となっている。   Then, the first alloy layer 43 and the second alloy layer 49 are joined together by the brazing material 35, so that the first joining ceramic member 31 and the second joining ceramic member 33 are joined together. .

ｂ）次に、この接合体３７の製造方法を、第１、第２接合用セラミック部材３１、３３の製造方法とともに説明する。
1)前記実施例１にて説明した様に（以下省略した内容は前記実施例１と同様である）、前記表１に示す第１、第２ペーストの成分の粉末を使用して、各試料の第１、第２ペーストを製造した。 b) Next, a manufacturing method of the joined body 37 will be described together with manufacturing methods of the first and second joining ceramic members 31 and 33.
1) As explained in Example 1 (the contents omitted below are the same as in Example 1), each sample was prepared using the powders of the first and second paste components shown in Table 1 above. The first and second pastes were produced.

2)次に、第１ペーストを、第１、第２セラミック基材３９、４５のそれぞれの表面に塗布し、乾燥してそれぞれ第１層を形成した。
3)次に、第２ペーストを、第１、第２セラミック基材３９、４５のそれぞれの第１層の表面に塗布し、乾燥してそれぞれ第２層を形成した。 2) Next, the first paste was applied to the surfaces of the first and second ceramic substrates 39 and 45 and dried to form the first layers.
3) Next, the second paste was applied to the surfaces of the first layers of the first and second ceramic substrates 39 and 45, and dried to form second layers.

4)次に、前記第１層及び第２層を形成した第１、２セラミック基材３９、４５を、それぞれ炉中に入れ、１０５０〜１２００℃の温度にて焼成した。これにより、第１メタライズ層４１上に第１合金層４３が積層された第１接合用セラミック部材３１と、第２メタライズ層４７上に第２合金層４９が積層された第２接合用セラミック部材３３を得た。   4) Next, the first and second ceramic base materials 39 and 45 on which the first layer and the second layer were formed were respectively placed in a furnace and fired at a temperature of 1050 to 1200 ° C. Accordingly, the first bonding ceramic member 31 in which the first alloy layer 43 is stacked on the first metallized layer 41 and the second bonding ceramic member in which the second alloy layer 49 is stacked on the second metallized layer 47. 33 was obtained.

5)次に、両合金層４３、４９の間に、銀ロー材３５を配置してロー付け接合し、両接合用セラミック部材３１、３３を接合して一体化して接合体３７を完成した。
本実施例の接合体３７は、前記実施例１と同様に、接合強度が高く気密性にも優れている。
（実施例３）
次に、実施例３について説明するが、前記実施例１、２と同様な箇所の説明は省略する。 5) Next, the silver brazing material 35 was placed between the alloy layers 43 and 49 and brazed and joined, and the joined ceramic members 31 and 33 were joined and integrated to complete the joined body 37.
The joined body 37 of this example has high joining strength and excellent airtightness, as in Example 1.
(Example 3)
Next, the third embodiment will be described, but the description of the same parts as the first and second embodiments will be omitted.

本実施例は、前記実施例１のような接合用セラミック部材と金属部材からなる接合体を真空スイッチに用いた例である。
即ち、本実施例の真空スイッチは、真空容器内に電極等を内蔵し、高電圧、大電流の開閉に適した高負荷開閉器である。 The present embodiment is an example in which a joined body made of a joining ceramic member and a metal member as in the first embodiment is used for a vacuum switch.
That is, the vacuum switch according to the present embodiment is a high load switch that incorporates an electrode or the like in a vacuum vessel and is suitable for switching a high voltage and a large current.

詳しくは、図５に示す様に、真空負荷開閉器１００は、絶縁バルブ１０１と、絶縁バルブ１０１の端部を塞いで取り付けられた第１及び第２の端蓋１０２、１０３と、第１の端蓋１０２に取り付けられ絶縁バルブ１０１内に突出された固定電極１０４と、第２の端蓋１０３に摺動自在に配置された可動電極１０５とを備え、固定電極１０４と可動電極１０５により接点１０６を構成している。   Specifically, as shown in FIG. 5, the vacuum load switch 100 includes an insulating valve 101, first and second end covers 102 and 103 attached by closing the end of the insulating valve 101, A fixed electrode 104 attached to the end lid 102 and projecting into the insulating valve 101 and a movable electrode 105 slidably disposed on the second end lid 103 are provided. A contact 106 is formed by the fixed electrode 104 and the movable electrode 105. Is configured.

前記絶縁バルブ１０１は、アルミナ９２重量％のセラミック焼成体で形成され、内径８０ｍｍ×肉厚５ｍｍ程度×長さ１００ｍｍの略円筒形である。また、絶縁バルブ１０１は、内径が一定の直胴部１１０及び内周壁１１１の中間にて内側に突出して周設される凸状部１１２を有している。更に、絶縁バルブ１０１の外周面には、釉薬層１１５を備えている。   The insulating valve 101 is made of a ceramic fired body of 92% by weight of alumina and has a substantially cylindrical shape with an inner diameter of 80 mm, a thickness of about 5 mm, and a length of 100 mm. Further, the insulating valve 101 has a straight body portion 110 having a constant inner diameter and a convex portion 112 that protrudes inwardly in the middle of the inner peripheral wall 111. Further, a glaze layer 115 is provided on the outer peripheral surface of the insulating valve 101.

前記第１、２端蓋１０２，１０３は、円板状のコバール（Ｆｅ−Ｎｉ−Ｃｏ）板で形成され、各中央部に固定電極１０４、ガイド１３１を固着するための穴１２１、１３２が設けられている。このガイド１３１は、可動電極１０５の可動軸１５１が摺動し易いように設けられている。   The first and second end covers 102 and 103 are formed of a disk-shaped Kovar (Fe—Ni—Co) plate, and holes 121 and 132 for fixing the fixed electrode 104 and the guide 131 are provided in the respective central portions. It has been. The guide 131 is provided so that the movable shaft 151 of the movable electrode 105 can easily slide.

前記固定電極１０４は、先端が穴１２１に固着される固定軸１４１となり、先端が絶縁バルブ１０１内に突出される円環状の電極１４２となっている。
前記可動電極１０５は、後端がガイド１３１内を摺動する可動軸１５１となり、先端が固定電極１０４側の電極１４２に接触する電極１５２となっている。この可動電極１０５は、電極１５２付近の可動軸１５１と第２の端蓋１０３との間に設けられる蛇腹状の金属べローズ１５３により、真空保持状態で開閉動作を可能とされている。 The fixed electrode 104 is a fixed shaft 141 whose tip is fixed to the hole 121, and an annular electrode 142 whose tip is projected into the insulating valve 101.
The movable electrode 105 has a movable shaft 151 that slides in the guide 131 at the rear end, and an electrode 152 that contacts the electrode 142 on the fixed electrode 104 side. The movable electrode 105 can be opened and closed in a vacuum state by a bellows-shaped metal bellows 153 provided between the movable shaft 151 near the electrode 152 and the second end cover 103.

前記金属ベローズ１５３は、ベローズカバー１５４で囲まれ、電流開閉時に、電極１４２，１５２（即ちその先端の接触子１４３、１５５）から発生する金属蒸気が直接触れるのを防いでいる。   The metal bellows 153 is surrounded by a bellows cover 154 to prevent direct contact with metal vapor generated from the electrodes 142 and 152 (that is, the contacts 143 and 155 at the tips) when the current is opened and closed.

前記接点１０６は、電極１４２，１５２の接触が行われる接触子１４３、１５５に、高融点のタングステン系の焼結金属を用い、発生する真空アークにより溶着し難い構造となっている。   The contact 106 has a structure in which a high melting point tungsten-based sintered metal is used for the contacts 143 and 155 with which the electrodes 142 and 152 are contacted, and is difficult to be welded by a generated vacuum arc.

また、接点１０６を囲んでアークシールド１６１が配置されている。このアークシールド１６１は、前述の金属蒸気が絶縁バルブ１０１の内周壁１１１に付着して絶縁が低下するのを防止するために、絶縁バルブ１０１の凸状部１１２にロー付けにより接合されている。   An arc shield 161 is disposed around the contact 106. This arc shield 161 is joined to the convex portion 112 of the insulating valve 101 by brazing in order to prevent the above-described metal vapor from adhering to the inner peripheral wall 111 of the insulating valve 101 and lowering the insulation.

つまり、本実施例の高負荷開閉器１００では、前記実施例１の接合体と同様に、接合用セラミック部材である絶縁バルブ１０１の凸状部１１２に、金属部材であるアークシールド１６１がロー材１６２によるロー付けにより接合されている。   That is, in the high load switch 100 of the present embodiment, the arc shield 161 that is a metal member is provided on the convex portion 112 of the insulating valve 101 that is a ceramic member for bonding, as in the joined body of the first embodiment. Joined by brazing with 162.

詳しくは、図６に要部を模式的に示す様に、絶縁バルブ１０１の凸状部１１２の先端には、前記実施例１に示した様に、低温でのメタライズにより、メタライズ層１７１が形成され、このメタライズ層１７１上に合金層１７３が形成され、この合金層１７３とアークシールド１６１とがロー材１６２によるロー付けによって接合されているのである。   Specifically, as schematically shown in FIG. 6, a metallized layer 171 is formed at the tip of the convex portion 112 of the insulating valve 101 by metallization at a low temperature as shown in the first embodiment. Then, an alloy layer 173 is formed on the metallized layer 171, and the alloy layer 173 and the arc shield 161 are joined by brazing with a brazing material 162.

これにより、アークシールド１６１を備えた絶縁バルブ１０１（従って高負荷開閉器１００）を、低コストで製造でき、また、高い寸法精度及び高い接合強度を実現することができる。
（実施例４）
次に、実施例４について説明するが、前記実施例３と同様な箇所の説明は省略する。 Thereby, the insulation valve 101 (hence, high load switch 100) provided with the arc shield 161 can be manufactured at low cost, and high dimensional accuracy and high joint strength can be realized.
Example 4
Next, Example 4 will be described, but the description of the same parts as Example 3 will be omitted.

本実施例は、前記実施例３の様に、接合用セラミック部材と金属部材からなる接合体を真空スイッチに用いた例であるが、アークシールドと絶縁バルブの構造が異なる。
図７に要部を模式的に示す様に、本実施例の真空スイッチ（高負荷開閉器）２００は、上絶縁バルブ２０１と下絶縁バルブ２０３との間に、無酸素銅からなる金属製の接続部材２０５がロー付けされ、その接続部材２０５の先端側に、アークシールド２０７がロー付け接合されている。 The present embodiment is an example in which a joined body made of a joining ceramic member and a metal member is used for a vacuum switch as in the third embodiment, but the structures of the arc shield and the insulating valve are different.
As schematically shown in FIG. 7, the vacuum switch (high load switch) 200 of this embodiment is made of a metal made of oxygen-free copper between the upper insulating valve 201 and the lower insulating valve 203. The connecting member 205 is brazed, and the arc shield 207 is brazed and joined to the distal end side of the connecting member 205.

特に、前記上絶縁バルブ２０１及び下絶縁バルブ２０３と接続部材２０５とが固定される部分（固定部２０９）には、前記実施例１と同様な方法で、それぞれメタライズ層２１１、２１３が形成され、各メタライズ層２１１、２１３上にはそれぞれ合金層２１５、２１７が形成されている。   In particular, metallized layers 211 and 213 are respectively formed in portions (fixed portions 209) where the upper insulating valve 201 and the lower insulating valve 203 and the connection member 205 are fixed in the same manner as in the first embodiment. Alloy layers 215 and 217 are formed on the metallized layers 211 and 213, respectively.

そして、この合金層２１５、２１７と接続部材２０５とが、それぞれロー材２１９、２２１により接合されることにより、両絶縁バルブ２０１、２０３と接続部材２０５とが接合一体化されている。   The alloy layers 215 and 217 and the connecting member 205 are joined by the brazing materials 219 and 221 respectively, so that both the insulating valves 201 and 203 and the connecting member 205 are joined and integrated.

尚、両絶縁バルブ２０１、２０３の外周面には 前記実施例３と同様の釉薬層２２３、２２５がそれぞれ形成されている。
本実施例によっても、前記実施例３と同様な効果を奏する。 Note that glaze layers 223 and 225 similar to those of the third embodiment are formed on the outer peripheral surfaces of the both insulating valves 201 and 203, respectively.
Also according to this embodiment, the same effects as those of the third embodiment can be obtained.

尚、本発明は前記実施例になんら限定されるものではなく、本発明の要旨を逸脱しない範囲において種々の態様で実施しうることはいうまでもない。 The present invention is not limited in any way to the embodiments, it is not needless to say that without departing from the scope of the present invention may be practiced in various forms.

実施例１の接合体の要部を破断して示す説明図である。It is explanatory drawing which fractures | ruptures and shows the principal part of the conjugate | zygote of Example 1. FIG. 実施例１の接合体を示す斜視図である。1 is a perspective view showing a joined body of Example 1. FIG. 実施例１の接合体の接合強度の測定方法を示す説明図である。It is explanatory drawing which shows the measuring method of the joint strength of the joined body of Example 1. FIG. 実施例２の接合体の要部を破断して示す説明図である。It is explanatory drawing which fractures | ruptures and shows the principal part of the conjugate | zygote of Example 2. FIG. 実施例３の真空スイッチを破断して示す説明図である。It is explanatory drawing which fractures | ruptures and shows the vacuum switch of Example 3. FIG. 実施例３の真空スイッチの要部を破断して示す説明図である。It is explanatory drawing which fractures | ruptures and shows the principal part of the vacuum switch of Example 3. FIG. 実施例４の真空スイッチの要部を破断して示す説明図である。It is explanatory drawing which fractures | ruptures and shows the principal part of the vacuum switch of Example 4. FIG.

符号の説明Explanation of symbols

１…接合用セラミック部材
３…金属部材
５、３５、１６２、２１９、２２１…ロー材
７、３７…接合体
９…セラミック基材
１１、１７１、２１１、２１３…メタライズ層
１３、１７４、２１５、２１７…合金層
３１…第１接合用セラミック部材
３３…第２接合用セラミック部材
３９…第１セラミック基材
４１…第１メタライズ層
４３…第１合金層
４５…第２セラミック基材
４７…第２メタライズ層
４９…第２合金層
１６１、２０７…アークシールド
１０１…絶縁バルブ
１００、２００…真空スイッチ（高負荷開閉器）
２０１…上絶縁バルブ
２０３…下絶縁バルブ
２０５…接続部材 DESCRIPTION OF SYMBOLS 1 ... Ceramic member for joining 3 ... Metal member 5, 35, 162, 219, 221 ... Raw material 7, 37 ... Joined body 9 ... Ceramic base material 11, 171, 211, 213 ... Metallized layer 13, 174, 215, 217 ... Alloy layer 31 ... First joining ceramic member 33 ... Second joining ceramic member 39 ... First ceramic substrate 41 ... First metallized layer 43 ... First alloy layer 45 ... Second ceramic substrate 47 ... Second metallized Layer 49 ... Second alloy layer 161, 207 ... Arc shield 101 ... Insulation valve 100, 200 ... Vacuum switch (high load switch)
201 ... Upper insulation valve 203 ... Lower insulation valve 205 ... Connection member

Claims (6)

モリブデン粉末及びニッケル粉末を含有する第１混合物と、有機バインダとを混合した第１ペーストを、セラミック焼成体であるセラミック基材に塗布し乾燥して第１層を形成する第１工程と、
ニッケル粉末又は酸化ニッケル粉末と、銅粉末、酸化銅粉末、マンガン粉末、及び酸化マンガン粉末のうち少なくとも１種と、を含有する第２混合物、あるいは、ニッケル−銅の合金粉末又はニッケル−マンガンの合金粉末を含有する第２混合物と、有機バインダとを混合した第２ペーストを、前記第１層上に塗布し乾燥して第２層を形成する第２工程と、
前記第１層及び第２層を加熱して焼き付ける第３工程と、
を備え、
前記第２混合物として、前記ニッケル成分を３５〜７５重量％と、銅成分又はマンガン成分を２５〜６５重量％と、を含有する混合物を用いることを特徴とする接合用セラミック部材の製造方法。 A first mixture comprising molybdenum powder, and nickel powder, a first step of forming a first paste obtained by mixing an organic binder, the first layer was applied to the ceramic substrate is a ceramic fired body dry,
Second mixture containing nickel powder or nickel oxide powder and at least one of copper powder, copper oxide powder, manganese powder, and manganese oxide powder, or nickel-copper alloy powder or nickel-manganese alloy a second mixture containing a powder, a second step of forming a second layer of the second paste were mixed with an organic binder, it was applied and dried on the first layer,
A third step of heating and baking the first layer and the second layer;
Bei to give a,
A method for producing a ceramic member for joining , wherein a mixture containing 35 to 75% by weight of the nickel component and 25 to 65% by weight of a copper component or a manganese component is used as the second mixture . セラミック焼成体であるセラミック基材表面に、モリブデン及びニッケルを含有する下層であるメタライズ層を備えるとともに、
前記メタライズ層の表面側に、ニッケルと、銅又はマンガンと、を含有する上層である合金層を備え、
前記合金層は、前記ニッケルを３６〜６１．３重量％と、銅を３３〜６０重量％又はマンガンを２〜３０重量％と、を含むことを特徴とする接合用セラミック部材。 While equipped with a metallized layer, which is a lower layer containing molybdenum and nickel, on the surface of the ceramic substrate that is a ceramic fired body,
On the surface of the metallization layer, Introduction Preparations and nickel, and copper or manganese, an alloy layer is a layer containing,
The alloy layer includes 36 to 61.3% by weight of the nickel, 33 to 60% by weight of copper, or 2 to 30% by weight of manganese . 前記請求項２に記載の接合用セラミック部材に、少なくとも前記メタライズ層及び前記合金層を介して金属部材を接合したことを特徴とする接合体。 A joined body comprising the metal member joined to the joining ceramic member according to claim 2 through at least the metallized layer and the alloy layer. 前記請求項２に記載の接合用セラミック部材に、少なくとも前記メタライズ層及び前記合金層を介して他の接合用セラミック部材を接合したことを特徴とする接合体。 The joined ceramic member according to claim 2 , wherein at least another joining ceramic member is joined via the metallized layer and the alloy layer. 前記請求項３又は４の接合体を備えたことを特徴とする真空スイッチ。 A vacuum switch comprising the joined body according to claim 3 or 4 . 前記請求項３又は４の接合体を備えたことを特徴とする真空容器。 A vacuum vessel comprising the joined body according to claim 3 or 4 .
JP2005236642A 2005-08-17 2005-08-17 Method of manufacturing ceramic member for bonding, ceramic member for bonding, bonded body, vacuum switch, and vacuum container Expired - Fee Related JP4457056B2 (en)

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