JP2010059010A - Ceramic junction body for manufacturing semiconductor, and method for manufacturing the same - Google Patents
Ceramic junction body for manufacturing semiconductor, and method for manufacturing the same Download PDFInfo
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- JP2010059010A JP2010059010A JP2008225780A JP2008225780A JP2010059010A JP 2010059010 A JP2010059010 A JP 2010059010A JP 2008225780 A JP2008225780 A JP 2008225780A JP 2008225780 A JP2008225780 A JP 2008225780A JP 2010059010 A JP2010059010 A JP 2010059010A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 120
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 239000004065 semiconductor Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 37
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 238000005304 joining Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
【課題】接合部においても、接合する部品自体と同等レベルの強度を有し、接合部周辺に欠落箇所が生じた場合であっても、接合状態を保持し、一体の部材としての機能を維持することができ、半導体製造用部材として好適に用いることができるセラミックス接合体およびその製造方法を提供する。
【解決手段】凹部を有する第1のセラミックス焼結体に、同一組成からなる第2のセラミックス焼結体が前記第1のセラミックス焼結体の凹部に嵌挿されて接合されたセラミックス接合体を製造する際、前記セラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子を分散させたスラリー調製工程と、接合面へのスラリー塗布工程と、第1のセラミックス焼結体の仮焼体の凹部に、第2のセラミックス焼結体を嵌挿して、前記接合面同士を合わせた後、1500℃以上2000℃以下で焼結させて接合する工程とを経る。
【選択図】なしThe joint also has the same level of strength as the part itself to be joined, and maintains the joined state and maintains the function as an integral member even when a missing part occurs around the joint. A ceramic joined body that can be suitably used as a semiconductor manufacturing member and a method for manufacturing the same are provided.
A ceramic joined body in which a second ceramic sintered body having the same composition is inserted into a recessed portion of the first ceramic sintered body and joined to the first ceramic sintered body having a recessed portion. When manufacturing, a slurry preparation step in which ceramic particles having the same composition as the ceramic sintered body and having an average particle diameter of 5 nm to 75 nm are dispersed, a slurry applying step to the joint surface, and a first ceramic sintered body A second ceramic sintered body is inserted into the concave portion of the calcined body, and the joining surfaces are matched with each other, and then sintered and joined at 1500 ° C. or more and 2000 ° C. or less.
[Selection figure] None
Description
本発明は、セラミックス焼結体の凹部に、他のセラミックス焼結体が嵌挿されて接合された半導体製造用セラミックス接合体およびその製造方法に関する。 The present invention relates to a ceramic joined body for semiconductor production in which another ceramic sintered body is inserted and joined in a recess of the ceramic sintered body and a method for producing the same.
セラミックスは、耐熱性や耐食性、耐摩耗性に優れ、高硬度、高強度である等の特性を有していることから、各種構造部材として利用されており、特に、高純度セラミックスは、半導体製造用部材にも好適に用いられている。
しかしながら、セラミックスの多くは、硬くて脆いため、金属や樹脂に比べて難加工性であり、複雑な形状の部材は、一体成形による製造が困難な場合も多く、このような場合には、各部品を組み合わせて接合して部材を構成する。
Ceramics are used as various structural members because they have excellent heat resistance, corrosion resistance, wear resistance, high hardness, high strength, etc. In particular, high purity ceramics are used in semiconductor manufacturing. It is also used suitably for a member for use.
However, since many ceramics are hard and brittle, they are difficult to process as compared to metals and resins, and complicated-shaped members are often difficult to manufacture by integral molding. Combining and joining parts to form a member.
セラミックス部品同士を接合する方法としては、例えば、特許文献1に、セラミックス系スラリー接着剤を用いて接着し、焼成して接合する方法が記載されている。
また、孔や凹部を有するセラミックス部品に他のセラミックス部品を嵌挿させて一体化させた接合体を作製する場合には、例えば、特許文献2に記載されているように、各部品の焼成収縮率差を利用して、焼成により接合する、いわゆる焼き嵌めを用いること方法が知られている。
As a method for joining ceramic parts, for example, Patent Document 1 describes a method in which a ceramic-based slurry adhesive is used for bonding, followed by firing.
Moreover, when producing a joined body in which other ceramic parts are inserted and integrated into a ceramic part having a hole or a recess, for example, as described in Patent Document 2, firing shrinkage of each part is performed. A method of using so-called shrink fitting, in which the difference in rate is used to join by firing, is known.
しかしながら、上記特許文献1に記載されているようなセラミックス系スラリー接着剤は、該接着剤中に含まれるセラミックス粒子の純度が低く、接合部における強度が、接合する部品自体の強度に比べて1割程度劣る。また、セラミックス粒子成分以外の他の不純物成分が多く含まれているため、接合部の耐食性に劣るという課題を有していた。
さらに、該接着剤により接合したセラミックス接合体を半導体製造用部材として用いる場合には、該接着剤に含まれるセラミックス粒子成分以外の他の不純物成分により被処理ウェーハ等が汚染されるおそれがある。
However, the ceramic slurry adhesive as described in Patent Document 1 has a low purity of ceramic particles contained in the adhesive, and the strength at the joint is 1 compared to the strength of the parts to be joined. About inferior. Moreover, since many impurity components other than a ceramic particle component are contained, it had the subject that it is inferior to the corrosion resistance of a junction part.
Furthermore, when the ceramic joined body joined by the adhesive is used as a member for manufacturing a semiconductor, there is a possibility that the wafer to be processed and the like is contaminated by other impurity components other than the ceramic particle component contained in the adhesive.
また、上記特許文献2に記載されているような焼き嵌めによる接合方法は、前記接着剤を用いた接合よりも、高い接合強度が得られるものの、接合部近辺において、部品にクラックが入り、欠落箇所が生じることもある。
焼き嵌めは、外側の部品が、熱収縮により、内側の部品を締め付けて、形状および固定状態を保持しているにすぎないため、上記のように、一部でも欠落が生じた場合、両部品は容易に分離してしまう。
Moreover, although the joining method by shrink fitting as described in the above-mentioned Patent Document 2 provides higher joining strength than joining using the adhesive, the part is cracked and missing in the vicinity of the joining part. There may be places.
In shrink fitting, the outer part is only tightened to the inner part due to heat shrinkage and the shape and the fixed state are maintained. Are easily separated.
本発明は、上記技術的課題を解決するためになされたものであり、接合部においても、接合する部品自体と同等レベルの強度を有し、接合部周辺に欠落箇所が生じた場合であっても、接合状態を保持し、一体の部材としての機能を維持することができ、半導体製造用部材として好適に用いることができるセラミックス接合体およびその製造方法を提供することを目的とするものである。 The present invention has been made in order to solve the above technical problem, and the joint portion has the same level of strength as the part to be joined itself, and a missing portion occurs around the joint portion. Another object of the present invention is to provide a ceramic joined body that can maintain a joined state, maintain a function as an integral member, and can be suitably used as a semiconductor manufacturing member, and a method for manufacturing the same. .
本発明に係る半導体製造用セラミックス接合体は、凹部を有する第1のセラミックス焼結体に、同一組成からなる第2のセラミックス焼結体が前記第1のセラミックス焼結体の凹部に嵌挿されて接合されたセラミックス接合体であって、前記第1のセラミックス焼結体と第2のセラミックス焼結体との接合部は、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子の焼結体により密着していることを特徴とする。
このような構成のセラミックス接合体は、いわゆる焼き嵌めによる接合において、接合強度がより向上され、焼き嵌めの接合部においても、接合する部品自体と同等レベルの強度を有し、接合部周辺に欠落箇所が生じた場合であっても、接合状態を保持し、一体の部材としての機能を維持することができる。
In the ceramic joined body for manufacturing a semiconductor according to the present invention, the second ceramic sintered body having the same composition is inserted into the concave portion of the first ceramic sintered body in the first ceramic sintered body having the concave portion. The joined portion of the first ceramic sintered body and the second ceramic sintered body is an average composed of the same composition as that of the first and second ceramic sintered bodies. It is characterized by being in close contact with a sintered body of ceramic particles having a particle size of 5 nm to 75 nm.
The ceramic joined body having such a structure has a further improved joining strength in so-called shrink fitting, and has a strength equivalent to that of the parts to be joined even in the shrink fitting joint, and is missing around the joint. Even if a location is generated, the joined state can be maintained and the function as an integral member can be maintained.
前記セラミックス接合体は、高純度、接合特性、半導体用途等の観点から、特に、前記組成がアルミナであることが好ましい。 In particular, it is preferable that the ceramic bonded body has an alumina composition from the viewpoint of high purity, bonding characteristics, semiconductor use, and the like.
また、本発明に係る半導体製造用セラミックス接合体の製造方法は、凹部を有する第1のセラミックス焼結体に、同一組成からなる第2のセラミックス焼結体が前記第1のセラミックス焼結体の凹部に嵌挿されて接合されたセラミックス接合体の製造方法であって、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子を分散させたスラリーまたはペーストを調製する工程と、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体および前記第2のセラミックス焼結体の接合面の一方または両方に、前記スラリーまたはペーストを塗布する工程と、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体の凹部に、前記第2のセラミックス焼結体を嵌挿して、前記接合面同士を合わせた後、1500℃以上2000℃以下で焼結させて接合する工程とを備えていることを特徴とする。
上記のようなスラリーまたはペーストを用いて接合させると、焼結時の粒子の粒成長により、嵌挿した接合部に、前記第1および第2のセラミックス焼結体と同一組成のセラミックス粒子の焼結体が形成され、上記のような接合強度の高いセラミックス接合体を得ることができる。
Further, in the method for manufacturing a ceramic joined body for semiconductor production according to the present invention, the second ceramic sintered body having the same composition is added to the first ceramic sintered body having the concave portion. A method for producing a ceramic joined body that is inserted into a recess and joined thereto, wherein a slurry in which ceramic particles having the same composition as the first and second ceramic sintered bodies and having an average particle diameter of 5 nm to 75 nm are dispersed. Alternatively, the slurry or paste is applied to one or both of the step of preparing the paste and the bonding surface of the calcined body or the molded body that is the precursor of the first ceramic sintered body and the second ceramic sintered body. The second ceramic sintered body is inserted into the recess of the calcined body or molded body, which is a precursor of the first ceramic sintered body, and the coating step. , After adjusting the bonding faces, characterized in that it comprises a step of bonding by sintering at 1500 ° C. or higher 2000 ° C. or less.
When the above-described slurry or paste is used for bonding, ceramic particles having the same composition as that of the first and second ceramic sintered bodies are sintered in the inserted joint due to particle growth of the particles during sintering. A bonded body is formed, and a ceramic bonded body having high bonding strength as described above can be obtained.
上記製造方法は、特に、前記組成がアルミナである場合に好適に適用することができる。 The above production method can be suitably applied particularly when the composition is alumina.
本発明に係るセラミックス接合体は、高い接合強度を有し、接合部周辺に欠落箇所が生じた場合であっても、接合状態を保持し、一体の部材としての機能を維持することができる。
また、本発明に係るセラミックス接合体は、全体が同一組成からなるため、半導体製造用部材として用いた際の被処理ウェーハ等に対する不純物汚染の防止を図ることができる。
また、本発明に係る製造方法によれば、上記の本発明に係るセラミックス接合体を好適に得ることができる。
The ceramic bonded body according to the present invention has high bonding strength, and can maintain a bonded state and maintain a function as an integral member even when a missing portion is generated around the bonded portion.
Moreover, since the whole ceramic joined body which concerns on this invention consists of the same composition, it can aim at prevention of the impurity contamination with respect to the to-be-processed wafer etc. at the time of using as a member for semiconductor manufacture.
Moreover, according to the manufacturing method which concerns on this invention, the ceramic joined body which concerns on said this invention can be obtained suitably.
以下、本発明について詳細に説明する。
本発明に係る半導体製造用セラミックス接合体は、凹部を有する第1のセラミックス焼結体に、同一組成からなる第2のセラミックス焼結体が前記第1のセラミックス焼結体の凹部に嵌挿されて接合されたセラミックス接合体である。
そして、この接合体の接合部が、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子の焼結体により密着していることを特徴とするものである。
本発明は、焼結時の熱収縮を利用したいわゆる焼き嵌めによる接合において、その接合強度をより向上させたものである。
すなわち、本発明に係る接合体は、焼き嵌めの接合部においても、接合する部品自体と同等レベルの強度を有し、接合部周辺に欠落箇所が生じた場合であっても、接合状態を保持し、一体の部材としての機能を維持することができる接合体である。
Hereinafter, the present invention will be described in detail.
In the ceramic joined body for manufacturing a semiconductor according to the present invention, the second ceramic sintered body having the same composition is inserted into the concave portion of the first ceramic sintered body in the first ceramic sintered body having the concave portion. It is a ceramic joined body joined together.
And the junction part of this joined body is closely_contact | adhered by the sintered compact of the ceramic particle | grains with the average particle diameter of 5 nm or more and 75 nm or less which consists of the same composition as the said 1st and 2nd ceramic sintered compact. Is.
The present invention further improves the bonding strength in the so-called shrink-fit bonding utilizing the thermal shrinkage during sintering.
That is, the joined body according to the present invention has the same level of strength as the parts to be joined even in the shrink-fitted joint, and maintains the joined state even when a missing portion is generated around the joint. And it is a joined body which can maintain the function as an integral member.
前記第1および第2のセラミックス焼結体は、接合の際、焼結時における熱的挙動が同じとなるように、同一組成であることが好ましい。
さらに、同一の製造方法により製造された同一材料で構成されていることがより好ましい。
It is preferable that the first and second ceramic sintered bodies have the same composition so that the thermal behavior during sintering is the same during bonding.
Furthermore, it is more preferable that the same material manufactured by the same manufacturing method is used.
本発明に係るセラミックス接合体は、半導体製造に用いるものであるため、前記組成としては、アルミナ(Al2O3)、酸化亜鉛(ZnO)、シリカ(SiO2)、セリア(CeO2)、酸化ホルミウム(Ho2O3)、チタニア(TiO2)、マグネシア(MgO)、イットリア(Y2O3)、ジルコニア(ZrO2)等が好ましい。これらのうち、特に、高純度(純度99.9%以上)な微粒子を容易に入手することができ、優れた接合特性を得ることができるため好ましい。
なお、本発明に係るセラミックス接合体は、半導体製造用として、高純度、高耐食性等も要求されることから、純度99.9%以上の高純度であることが好ましい。
Since the ceramic joined body according to the present invention is used for semiconductor manufacture, the composition includes alumina (Al 2 O 3 ), zinc oxide (ZnO), silica (SiO 2 ), ceria (CeO 2 ), and oxidation. Holmium (Ho 2 O 3 ), titania (TiO 2 ), magnesia (MgO), yttria (Y 2 O 3 ), zirconia (ZrO 2 ) and the like are preferable. Among these, high purity (purity 99.9% or more) fine particles can be easily obtained and excellent bonding characteristics can be obtained, which is preferable.
The ceramic joined body according to the present invention is required to have high purity, high corrosion resistance, etc. for semiconductor production, and therefore preferably has a high purity of 99.9% or more.
また、前記接合部は、不純物を含まず、前記第1および第2のセラミックス焼結体を高い接合強度で一体化させるため、前記第1および第2のセラミックス焼結体と同一組成の焼結体で密着されていることが好ましい。
なお、第1および第2のセラミックス焼結体と接合部との熱膨張係数差による剥離や破損等を防止し、耐食性に優れた半導体製造用の接合体とするために、接合部も、いずれの組成においても、純度99.9%以上の高純度であることが好ましい。
さらに、前記接合部の焼結体は、高い接合強度を得る観点から、平均粒径5nm以上75nm以下のセラミックス粒子からなることが好ましい。
In addition, the bonding portion does not contain impurities, and the first and second ceramic sintered bodies are integrated with high bonding strength, so that the sintered portion has the same composition as the first and second ceramic sintered bodies. It is preferable that the body is closely attached.
In addition, in order to prevent exfoliation or breakage due to the difference in thermal expansion coefficient between the first and second ceramic sintered bodies and the joint, and to obtain a joined body for manufacturing semiconductors having excellent corrosion resistance, Also in the composition, it is preferable that the purity is 99.9% or more.
Furthermore, it is preferable that the sintered body of the joint portion is made of ceramic particles having an average particle diameter of 5 nm to 75 nm from the viewpoint of obtaining high bonding strength.
また、本発明に係る接合体は、焼き嵌めにより接合するものであるため、接合されている各セラミックス焼結体の形状は、第1のセラミックス焼結体は凹部を有しており、該凹部に第2のセラミックス部材が嵌挿されるように構成される。
前記凹部は、孔でもよく、接合体の態様は、例えば、管状体に柱状体を嵌挿させたものや、径の大きい管状体に、径の小さい管状体を嵌挿させたものであってもよい。
また、接合部の周面は、円状に限定されるものでなく、多角形状でもよい。
なお、本発明に係るセラミック接合体は、2個のセラミックス焼結体の接合体に限定されるものではなく、3個以上の同一組成からなるセラミックス焼結体がそれぞれ、接合部を介して接合されたものであってもよい。
In addition, since the joined body according to the present invention is joined by shrink fitting, the shape of each ceramic sintered body to be joined is such that the first ceramic sintered body has a concave portion. It is comprised so that a 2nd ceramic member may be inserted in.
The concave portion may be a hole, and the joined body may be formed by, for example, inserting a columnar body into a tubular body, or inserting a small diameter tubular body into a large diameter tubular body. Also good.
Moreover, the peripheral surface of a junction part is not limited to circular shape, A polygonal shape may be sufficient.
Note that the ceramic joined body according to the present invention is not limited to a joined body of two ceramic sintered bodies, and three or more ceramic sintered bodies having the same composition are joined via joints. It may be what was done.
前記セラミックス接合体は、具体的には、以下のような本発明に係る製造方法により得ることができる。
本発明に係るセラミックス接合体の製造方法は、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子を分散させたスラリーまたはペーストを調製する工程と、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体および前記第2のセラミックス焼結体の接合面の一方または両方に、前記スラリーまたはペーストを塗布する工程と、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体の凹部に、前記第2のセラミックス焼結体を嵌挿して、前記接合面同士を合わせた後、1500℃以上2000℃以下で焼結させて接合する工程とを経るものである。
上記のようなスラリーまたはペーストを用いて接合させると、焼結時の粒子の粒成長により、嵌挿した接合部に、前記第1および第2のセラミックス焼結体と同一組成のセラミックス粒子の焼結体が形成され、上記のようなセラミックス接合体を得ることができる。
Specifically, the ceramic joined body can be obtained by the following manufacturing method according to the present invention.
The method for producing a ceramic joined body according to the present invention comprises a step of preparing a slurry or paste in which ceramic particles having an average particle diameter of 5 nm to 75 nm and having the same composition as the first and second ceramic sintered bodies are dispersed. Applying the slurry or paste to one or both of a calcined body or a molded body that is a precursor of the first ceramic sintered body and a joint surface of the second ceramic sintered body; After inserting the second ceramic sintered body into the concave portion of the calcined body or molded body, which is a precursor of the ceramic sintered body 1, and matching the joint surfaces, the temperature is 1500 ° C. or higher and 2000 ° C. or lower. And a step of sintering and joining.
When the above-described slurry or paste is used for bonding, ceramic particles having the same composition as that of the first and second ceramic sintered bodies are sintered in the inserted joint due to particle growth of the particles during sintering. A bonded body is formed, and a ceramic joined body as described above can be obtained.
以下、上記製造方法を各工程順に説明する。
まず、周知の方法により、同一組成からなる第1および第2のセラミックス焼結体を作製する。
次に、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子を分散媒に分散させて混合し、スラリーまたはペーストを調製する。
前記分散媒は、セラミックス粒子の材料に応じた分散性、スラリーまたはペーストの粘性等を考慮して、適宜選択されるが、焼結処理後に残留成分が生じない液体であることが好ましい。一般には、純水、アルコール等が用いられる。
Hereinafter, the said manufacturing method is demonstrated in order of each process.
First, first and second ceramic sintered bodies having the same composition are produced by a known method.
Next, ceramic particles having the same composition as the first and second ceramic sintered bodies and having an average particle size of 5 nm to 75 nm are dispersed in a dispersion medium and mixed to prepare a slurry or paste.
The dispersion medium is appropriately selected in consideration of the dispersibility according to the material of the ceramic particles, the viscosity of the slurry or paste, and the like, but it is preferably a liquid that does not produce a residual component after the sintering treatment. In general, pure water, alcohol or the like is used.
次に、調製したスラリーまたはペーストを、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体および前記第2のセラミックス焼結体との接合面の一方または両方に塗布する。
凹部を有する第1のセラミックス焼結体については、焼結時の収縮による焼き嵌めにより接合することから、完全に焼結していない仮焼体や成形体の状態で、第2のセラミックス焼結体をその凹部に嵌挿させる。
前記スラリーまたはペーストの塗布は、例えば、刷毛等を用いて行う。塗布は、接合する第1および第2セラミックス焼結体の各接合面の一方のみでも、両方に行ってもよい。
Next, the prepared slurry or paste is applied to one or both of the bonding surface between the calcined body or the molded body, which is a precursor of the first ceramic sintered body, and the second ceramic sintered body.
About the 1st ceramic sintered compact which has a recessed part, since it joins by shrinkage | fitting by shrinkage | contraction at the time of sintering, in the state of the calcined body and the molded object which are not fully sintered, 2nd ceramic sintered The body is inserted into the recess.
The application of the slurry or paste is performed using, for example, a brush. The application may be performed on only one or both of the bonding surfaces of the first and second ceramic sintered bodies to be bonded.
最後に、前記第1のセラミックス焼結体の前駆体である仮焼体または成形体の凹部に、前記第2のセラミックス焼結体を嵌挿して、前記スラリーまたはペーストを塗布した接合面同士を合わせた後、1500℃以上2000℃以下で焼結させて接合する。
これにより、焼き嵌めによる接合力とスラリーまたはペースト中のセラミックス粒子の焼結体による接合力との両方の効果により、接合強度の高い接合体が得られる。
前記処理温度は1500℃未満である場合、スラリーまたはペースト中のセラミックス粒子の粒成長が十分に進行せず、接合部において十分な接合強度が得られない。
一方、前記処理温度が2000℃を超えても、温度に相応した接合強度の向上は望めない。
Finally, the second ceramic sintered body is inserted into the recess of the calcined body or the molded body, which is a precursor of the first ceramic sintered body, and the joining surfaces to which the slurry or paste is applied are bonded to each other. After combining, sintering is performed at 1500 ° C. or more and 2000 ° C. or less and bonding is performed.
Thereby, a bonded body with high bonding strength can be obtained by the effects of both the bonding force by shrink fitting and the bonding force by the sintered body of the ceramic particles in the slurry or paste.
When the treatment temperature is less than 1500 ° C., the grain growth of the ceramic particles in the slurry or paste does not proceed sufficiently, and sufficient joint strength cannot be obtained at the joint.
On the other hand, even if the treatment temperature exceeds 2000 ° C., it is not possible to improve the bonding strength corresponding to the temperature.
上記製造方法は、各種セラミックス接合体に適用することができるが、特に、アルミナセラミックス接合体を製造するのに好適である。 The manufacturing method can be applied to various ceramic joined bodies, and is particularly suitable for producing an alumina ceramic joined body.
また、本発明に係る製造方法は、焼き嵌めによる接合強度の向上を図るものであることから、径の異なる管状体同士を嵌挿させて接合する際に、優れた効果を発揮し得る。得られた管状接合体は、気密性に優れていることから、ガス管等として好適に利用することができる。
この場合、各管状体の嵌挿部において、両者の隙間は小さいことが好ましいが、高い気密性を得るためには、塗布したスラリーまたはペーストが剥離しない程度の余裕を持たせることが好ましい。
これにより、接合部周辺において、接合したセラミックス焼結体に欠落箇所が生じた場合であっても、接合面に塗布したスラリーまたはペーストによる焼結体が存在しているため、両セラミックス焼結体が容易に分離することなく、接合状態を保持し、一体の部材としての機能を維持することができ、該接合体を継続使用することが可能となる。
Moreover, since the manufacturing method which concerns on this invention aims at the improvement of the joining strength by shrink fitting, when inserting and joining the tubular bodies from which a diameter differs, it can exhibit the outstanding effect. Since the obtained tubular joined body is excellent in airtightness, it can be suitably used as a gas pipe or the like.
In this case, it is preferable that the gap between the fitting portions of each tubular body is small. However, in order to obtain high airtightness, it is preferable to have a margin that the applied slurry or paste does not peel off.
As a result, even if there is a missing portion in the bonded ceramic sintered body around the bonded portion, there is a sintered body of slurry or paste applied to the bonded surface. However, without being easily separated, the joined state can be maintained, the function as an integral member can be maintained, and the joined body can be used continuously.
以下、本発明を実施例に基づきさらに具体的に説明するが、本発明は下記の実施例により制限されるものではない。
[試験1]
外径12mm、肉厚2mm、長さ120mmのアルミナ焼結体のパイプAと、900℃で仮焼した内径12.2mm、肉厚1mm、長さ120mmのアルミナ仮焼体のパイプBを準備した。パイプAの接合部にアルミナ粒子を分散させたスラリーを塗布後、パイプBの孔に約10mm嵌挿し、大気中、1800℃で焼結させた。
前記スラリーのアルミナ粒子の平均粒径を表1に示すように変化させ、得られた各接合体について、接合部の気密性を評価した。
EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Test 1]
An alumina sintered body pipe A having an outer diameter of 12 mm, a wall thickness of 2 mm, and a length of 120 mm, and an alumina calcined body pipe B having an inner diameter of 12.2 mm, a wall thickness of 1 mm, and a length of 120 mm calcined at 900 ° C. were prepared. . After applying slurry in which alumina particles were dispersed to the joint portion of the pipe A, about 10 mm was inserted into the hole of the pipe B and sintered at 1800 ° C. in the atmosphere.
The average particle size of the alumina particles of the slurry was changed as shown in Table 1, and the airtightness of the joint was evaluated for each of the obtained joined bodies.
また、パイプAを嵌挿したパイプBの接合部に局所的に荷重を加え、クラックを発生させ、故意に、パイプBの外周の1/4程度に欠落箇所を生じさせた。
この欠落箇所を生じさせた接合体について、パイプが抜ける強度を評価する引っ張り試験を行った。
これらの結果を表1にまとめて示す。
なお、比較例4においては、スラリーを塗布せずに接合させた。
Further, a load was locally applied to the joint portion of the pipe B into which the pipe A was inserted, and a crack was generated, and a missing portion was intentionally generated at about 1/4 of the outer periphery of the pipe B.
A tensile test for evaluating the strength with which the pipe is pulled out was performed on the joined body in which the missing portion was generated.
These results are summarized in Table 1.
In Comparative Example 4, bonding was performed without applying the slurry.
表1に示したように、いずれの接合体も良好な気密性が得られたが、接合部に欠落箇所を生じさせた場合の接合強度は、塗布したスラリーのアルミナ粒子の平均粒径が100nm以上(比較例1〜3)では、400N程度で接合体のパイプが抜けてしまい、スラリーを塗布しない場合(比較例4)と同等程度であった。
これに対して、平均粒径5nm以上75nm以下のアルミナ粒子のスラリーを接合部に塗布した場合は、接合部に欠落が生じた場合でも、パイプの接合強度が十分であった。
As shown in Table 1, all of the bonded bodies had good airtightness, but the bonding strength when a missing portion was generated in the bonded portion was that the average particle diameter of the alumina particles of the applied slurry was 100 nm. In the above (Comparative Examples 1 to 3), the pipe of the joined body was pulled out at about 400 N, which was about the same as the case where no slurry was applied (Comparative Example 4).
On the other hand, when a slurry of alumina particles having an average particle size of 5 nm or more and 75 nm or less was applied to the joint, the joint strength of the pipe was sufficient even when the joint was missing.
[試験2]
焼結温度を表2に示すように変化させ、それ以外は実施例2と同様にして、接合体を作製し、各評価を行った。
これらの結果を表2にまとめて示す。
[Test 2]
Sintering temperature was changed as shown in Table 2, and other than that was performed in the same manner as in Example 2 to produce a joined body, and each evaluation was performed.
These results are summarized in Table 2.
表2に示したように、焼結温度が1500℃以上の場合(実施例2,5〜7)は、引っ張り強度が高く、スラリー塗布の効果が認められた。
これに対して、焼結温度が1500℃未満の場合(比較例5〜7)は、十分な接合強度が得られず、スラリー塗布の効果が認められなかった。
As shown in Table 2, when the sintering temperature was 1500 ° C. or higher (Examples 2 to 7), the tensile strength was high, and the effect of slurry application was recognized.
On the other hand, when the sintering temperature was less than 1500 ° C. (Comparative Examples 5 to 7), sufficient bonding strength was not obtained, and the effect of slurry application was not recognized.
[試験3]
パイプBの内径を表2に示すように変化させ、それ以外は実施例2と同様にして、接合体を作製し、各評価を行った。
これらの結果を表3にまとめて示す。
[Test 3]
The inner diameter of the pipe B was changed as shown in Table 2, and a joined body was produced in the same manner as in Example 2 except that, and each evaluation was performed.
These results are summarized in Table 3.
表3に示したように、パイプAの外径が12mmの場合、パイプBの内径がその1.05倍未満(試料1〜4)では、嵌挿する際、塗布したスラリーが擦れて剥離し、十分な接合強度が得られなかった。
一方、両パイプの接合部に、ある程度の隙間(パイプBの内径がパイプAの外径の1.05倍以上)を確保することができれば、スラリーは剥離せず、その機能を十分に果たすことが認められた。ただし、パイプBの内径がパイプAの外径の1.21倍を超えると(試料9)、パイプBの焼結による収縮が不十分となり、接合しなかった。
この試験においては、パイプBの内径がパイプAの外径の1.05倍以上1.13倍以下の場合が、より高い接合強度が得られた。
As shown in Table 3, when the outer diameter of the pipe A is 12 mm and the inner diameter of the pipe B is less than 1.05 times (samples 1 to 4), the applied slurry is rubbed and peeled when inserted. A sufficient bonding strength was not obtained.
On the other hand, if a certain amount of clearance (the inner diameter of pipe B is 1.05 times or more than the outer diameter of pipe A) can be secured at the joint between both pipes, the slurry will not peel off and perform its function sufficiently. Was recognized. However, when the inner diameter of the pipe B exceeded 1.21 times the outer diameter of the pipe A (sample 9), the shrinkage due to the sintering of the pipe B became insufficient, and the pipe B was not joined.
In this test, higher joint strength was obtained when the inner diameter of the pipe B was 1.05 times or more and 1.13 times or less of the outer diameter of the pipe A.
Claims (4)
前記第1のセラミックス焼結体と第2のセラミックス焼結体との接合部は、前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子の焼結体により密着していることを特徴とする半導体製造用セラミックス接合体。 A ceramic joined body in which a second ceramic sintered body having the same composition is inserted into and joined to the concave portion of the first ceramic sintered body to the first ceramic sintered body having a concave portion,
The joint between the first ceramic sintered body and the second ceramic sintered body is formed by firing ceramic particles having the same composition as the first and second ceramic sintered bodies and having an average particle size of 5 nm to 75 nm. A ceramic joined body for manufacturing a semiconductor, characterized in that the bonded body is in close contact.
前記第1および第2のセラミックス焼結体と同一組成からなる平均粒径5nm以上75nm以下のセラミックス粒子を分散させたスラリーまたはペーストを調製する工程と、
前記第1のセラミックス焼結体の前駆体である仮焼体または成形体および前記第2のセラミックス焼結体の接合面の一方または両方に、前記スラリーまたはペーストを塗布する工程と、
前記第1のセラミックス焼結体の前駆体である仮焼体または成形体の凹部に、前記第2のセラミックス焼結体を嵌挿して、前記接合面同士を合わせた後、1500℃以上2000℃以下で焼結させて接合する工程とを備えていることを特徴とする半導体製造用セラミックス接合体の製造方法。 A method of manufacturing a ceramic joined body in which a second ceramic sintered body having the same composition is inserted into a concave portion of the first ceramic sintered body and joined to the first ceramic sintered body having a concave portion. And
Preparing a slurry or paste in which ceramic particles having an average particle size of 5 nm or more and 75 nm or less and having the same composition as the first and second ceramic sintered bodies are dispersed;
Applying the slurry or paste to one or both of the calcined body or molded body, which is a precursor of the first ceramic sintered body, and the joint surface of the second ceramic sintered body;
The second ceramic sintered body is inserted into the recessed portion of the calcined body or the molded body that is the precursor of the first ceramic sintered body, and after joining the joining surfaces, 1500 ° C. or more and 2000 ° C. A method for producing a ceramic joined body for semiconductor production, comprising: sintering and joining in the following.
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