JP2008037728A - Mullite refractory - Google Patents
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- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 58
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002245 particle Substances 0.000 claims abstract description 119
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 77
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000010304 firing Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- 229910002026 crystalline silica Inorganic materials 0.000 claims abstract description 12
- 239000011819 refractory material Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 22
- 239000011230 binding agent Substances 0.000 claims description 18
- 238000013001 point bending Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 7
- 239000000377 silicon dioxide Substances 0.000 description 13
- 238000002156 mixing Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 238000007429 general method Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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Abstract
【課題】焼成時における寸法変化が抑制され、機械的強度にも優れ、電子部品の焼成用道具材に好適なムライト質耐火物を提供する。
【解決手段】平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子または平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２６重量％とを原料とし、シリカ粒子が残留しない焼成体とすることにより、気孔率２０％以上、かつ、焼成時の寸法変化率が±１％以内であるムライト質耐火物を得る。
【選択図】なしDisclosed is a mullite refractory material that suppresses dimensional changes during firing, has excellent mechanical strength, and is suitable as a tool material for firing electronic parts.
74 to 85% by weight of alumina particles having an average particle diameter of 1 to 10 μm, and 15 to 26% by weight of amorphous silica particles having an average particle diameter of 10 to 200 μm or crystalline silica particles having an average particle diameter of 5 to 50 μm Is used as a raw material to obtain a mullite refractory having a porosity of 20% or more and a dimensional change rate during firing within ± 1%.
[Selection figure] None
Description
本発明は、主に電子部品用セラミックスの焼成、熱処理工程において使用される道具材として好適なムライト質耐火物に関する。 The present invention relates to a mullite refractory suitable as a tool material mainly used in firing and heat treatment processes for ceramics for electronic parts.
電子部品の焼成道具材用の耐火物としては、アルミナ質やムライト質の耐火物が主に使用されている。
ムライトは、アルミナに比べて、熱膨張係数が小さく、耐熱衝撃性に優れており、また、高温での強度が大きく、高温における機械的強度を求められる場合に、好適な材料である。
As refractories for firing electronic parts, alumina and mullite refractories are mainly used.
Mullite has a smaller thermal expansion coefficient and superior thermal shock resistance than alumina, and is a suitable material when it has a high strength at high temperatures and requires mechanical strength at high temperatures.
上記のような優れた特徴を有するムライト質の耐火物を製造する方法として、従来から、耐火物原料の一部に粘土を加えて、それが分解して生成するムライトを耐火物の結合に利用する方法が行われていた。 As a method for producing mullite refractories having the above-mentioned excellent characteristics, conventionally, clay is added to a part of the refractory raw material, and mullite produced by decomposition is used for refractory bonding. There was a way to do it.
また、焼成時にムライトを生成するような原料組成物を用いて、ムライト質耐火物を製造する方法も知られている。
例えば、特許文献１には、平均粒径０．１〜２μｍのアルミナ粉末およびその粒径の０．５倍以下の平均粒径をもつ非晶質シリカ粉末の混合粉末を成形し、焼成するムライト質焼結体の製造方法が記載されている。
また、特許文献２には、平均粒径４０ｎｍ以下のアルミナ粉末およびシリカ粉末と、平均粒径５０ｎｍ〜５μｍのムライト粉末の混合物を焼成するムライト質焼結体の製造方法が記載されている。
In addition, a method for producing a mullite refractory using a raw material composition that generates mullite upon firing is also known.
For example, Patent Document 1 discloses a mullite in which a mixed powder of an alumina powder having an average particle size of 0.1 to 2 μm and an amorphous silica powder having an average particle size not more than 0.5 times the particle size is molded and fired. A method for producing a sintered material is described.
Patent Document 2 describes a method for producing a mullite sintered body in which a mixture of alumina powder and silica powder having an average particle diameter of 40 nm or less and mullite powder having an average particle diameter of 50 nm to 5 μm is fired.
さらに、焼成時にムライトを生成するような原料組成物を耐火物の結合材として用いることにより、ムライト結合を有する耐火物を得る方法も知られている。
例えば、特許文献３には、アルミナおよびムライトからなる骨材成分と、焼成後にアルミナとムライトになるような組成比で混合したアルミナとシリカ微粉を含む結合材を混練・成形・焼成し、アルミナ・ムライト系の多孔質シート状の耐火物を製造する方法が記載されている。
For example, in Patent Document 3, an aggregate component composed of alumina and mullite, and a binder containing alumina and silica fine powder mixed at a composition ratio so as to become alumina and mullite after firing are kneaded, molded, and fired. A method for producing a mullite porous sheet refractory is described.
しかしながら、上記特許文献１〜３に記載されているような従来の原料配合組成または製造方法によるムライト質耐火物は、焼成時における寸法収縮が大きく、それに伴い、耐火物製品の変形や断裂が生じやすく、また、収縮に伴う歪の残留により、製品の機械的強度が低下する等の課題を有していた。 However, the mullite refractories by the conventional raw material blending composition or manufacturing method as described in the above-mentioned Patent Documents 1 to 3 have large dimensional shrinkage during firing, and accordingly, deformation and tearing of the refractory product occur. In addition, there is a problem that the mechanical strength of the product is reduced due to residual strain accompanying shrinkage.
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、焼成時における寸法変化が抑制され、機械的強度にも優れ、電子部品の焼成用道具材に好適なムライト質耐火物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 is a mullite refractory material that suppresses dimensional changes during firing, is excellent in mechanical strength, and is suitable for a tool for firing electronic components. It is intended to provide.
本発明に係るムライト質耐火物は、平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子または平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２６重量％とを原料とする焼成体からなり、該焼成体中にシリカ粒子が残留していないことを特徴とする。
上記のような配合組成からなる原料を用いて焼成時にムライトを生成させることにより、焼成時における寸法変化が抑制され、機械的強度に優れたムライト質耐火物が得られる。
The mullite refractory according to the present invention comprises 74 to 85% by weight of alumina particles having an average particle diameter of 1 to 10 μm and amorphous silica particles having an average particle diameter of 10 to 200 μm or crystalline silica particles having an average particle diameter of 5 to 50 μm. It consists of a fired body made from 15 to 26% by weight, and no silica particles remain in the fired body.
By generating mullite at the time of firing using the raw material having the above composition, dimensional change at the time of firing is suppressed, and a mullite refractory excellent in mechanical strength is obtained.
前記ムライト質耐火物によれば、気孔率２０％以上、かつ、焼成時の寸法変化率が±１％以内とすることができ、電子部品の焼成用道具材に好適に用いることができる。 According to the mullite refractory, the porosity can be 20% or more and the dimensional change rate during firing can be within ± 1%, which can be suitably used as a tool material for firing electronic parts.
また、本発明の他の態様のムライト質耐火物は、平均粒径５０〜５０００μｍのアルミナ粒子またはムライト粒子からなる骨材９０重量％以下と、結合材１０重量％以上とを原料とする焼成体からなり、前記結合材が、平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子または平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２６重量％との混合物からなることを特徴とする。
上記と同様のアルミナ粒子とシリカ粒子との混合物を結合材とし、それ以外に骨材を配合したものを原料とすることにより、より一層、焼成時における寸法変化が抑制され、機械的強度に優れたムライト質耐火物を得ることができる。
具体的には、焼成時の寸法変化率が±０．１％以内であり、３点曲げ強度が１０ＭＰａ以上とすることができる。
Further, the mullite refractory according to another aspect of the present invention is a fired body made of 90% by weight or less of an aggregate made of alumina particles or mullite particles having an average particle size of 50 to 5000 μm and 10% by weight or more of a binder. The binder comprises 74 to 85% by weight of alumina particles having an average particle diameter of 1 to 10 μm, and amorphous silica particles having an average particle diameter of 10 to 200 μm or crystalline silica particles 15 to 5 having an average particle diameter of 5 to 50 μm. It consists of a mixture with 26% by weight.
By using a mixture of alumina particles and silica particles similar to the above as a binder, and using a mixture of other aggregates as a raw material, the dimensional change during firing is further suppressed, and the mechanical strength is excellent. A mullite refractory can be obtained.
Specifically, the dimensional change rate during firing is within ± 0.1%, and the three-point bending strength can be 10 MPa or more.
上述したとおり、本発明によれば、焼成時における寸法変化が抑制され、機械的強度に優れたムライト質耐火物を提供することができる。
したがって、このようなムライト質耐火物は、電子部品の焼成用道具材に好適に用いることができる。
As described above, according to the present invention, it is possible to provide a mullite refractory that is suppressed in dimensional change during firing and has excellent mechanical strength.
Therefore, such a mullite refractory can be suitably used for a tool material for firing electronic parts.
以下、本発明をより詳細に説明する。
本発明に係るムライト質耐火物は、アルミナ粒子とシリカ粒子とを原料とする焼成体からなり、該焼成体中にはシリカ粒子が残留していないことを特徴とするものである。
すなわち、本発明に係る耐火物は、原料であるアルミナ粒子とシリカ粒子とを、焼成により反応させてムライトを生成させたものである。
Hereinafter, the present invention will be described in more detail.
The mullite refractory according to the present invention comprises a fired body made of alumina particles and silica particles as raw materials, and no silica particles remain in the fired body.
That is, the refractory according to the present invention is obtained by reacting alumina particles and silica particles as raw materials by firing to produce mullite.
前記原料中の配合組成は、平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子または平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２６重量％である。
このように、原料の配合組成は、アルミナ粒子の方が、シリカ粒子よりも配合量が多く、かつ、粒径が小さいため、焼成前の成形体中では、アルミナ粒子とシリカ粒子、または、シリカ粒子同士が接触している状態よりも、アルミナ粒子同士が接触している状態で存在している割合が多い。
The compounding composition in the raw materials is 74 to 85% by weight of alumina particles having an average particle diameter of 1 to 10 μm, amorphous silica particles having an average particle diameter of 10 to 200 μm, or crystalline silica particles 15 to 5 μm of average particle diameter. 26% by weight.
As described above, the composition of the raw material is such that the alumina particles have a larger amount and a smaller particle size than the silica particles, so in the molded body before firing, alumina particles and silica particles, or silica There is a greater proportion of the alumina particles in contact with each other than in the state where the particles are in contact.
したがって、焼成時の反応においては、まず、アルミナ粒子同士が焼結し始める。そして、アルミナ粒子間の空隙が残存しているうちに、シリカ粒子が拡散し、ムライトが生成し始め、アルミナ粒子が存在していた箇所でムライトが生成する。
このため、ムライトの生成箇所は、比較的緻密な焼結組織となるのに対して、シリカ粒子が存在していた箇所は空隙（気孔）となる。このようにしてムライトが生成した焼成体は、気孔を含んだ状態で、ムライトの緻密な焼結組織により、焼成体全体が支持されるため、焼成時における寸法収縮が抑制される。
Therefore, in the reaction during firing, first, the alumina particles start to sinter. And while the space | gap between alumina particles remains, a silica particle spread | diffuses, a mullite begins to produce | generate and a mullite produces | generates in the location where the alumina particle existed.
For this reason, the production | generation location of a mullite becomes a comparatively precise | minute sintered structure, On the other hand, the location where the silica particle existed becomes a space | gap (pore). Thus, since the whole sintered body is supported by the dense sintered structure of a mullite in the state containing a pore, the calcination which the mullite produced | generated has suppressed the dimensional shrinkage at the time of baking.
上記のように、本発明においては、原料であるアルミナ粒子には、平均粒径１〜１０μｍ、好ましくは、２〜６μｍの粒子を用いる。
アルミナ粒子の平均粒径が１μｍ未満である場合、アルミナ粒子同士の接触面積が大きく、ムライトの生成開始前に、アルミナ粒子同士の焼結が進行しすぎてしまい、焼成時の収縮率が大きくなる。
一方、アルミナ粒子の平均粒径が１０μｍを超える場合、アルミナ粒子とシリカ粒子とが反応しにくく、未反応のアルミナおよびシリカが焼成体中に残留することとなる。
As described above, in the present invention, particles having an average particle diameter of 1 to 10 [mu] m, preferably 2 to 6 [mu] m are used as the alumina particles as a raw material.
When the average particle diameter of the alumina particles is less than 1 μm, the contact area between the alumina particles is large, the sintering of the alumina particles proceeds too much before the start of mullite generation, and the shrinkage ratio during firing increases. .
On the other hand, when the average particle diameter of the alumina particles exceeds 10 μm, the alumina particles and the silica particles hardly react, and unreacted alumina and silica remain in the fired body.
また、原料のシリカ粒子は、非晶質シリカを用いる場合、平均粒径１０〜２００μｍ、好ましくは、３０〜１００μｍの粒子を用いる。
非晶質シリカ粒子の平均粒径が１０μｍ未満である場合、アルミナ粒子との反応が早い段階で起き、焼結の進行に伴って、シリカ粒子が存在した箇所に残存すべき空隙が焼成体外に追い出され、焼成体全体が収縮する。
一方、非晶質シリカの平均粒径が２００μｍを超える場合、シリカ粒子近傍に生成した緻密なムライト焼結組織によって、シリカ粒子の拡散が困難となり、シリカ粒子全量がムライト生成反応に関与することができず、未反応のシリカが残留する。
Further, as the raw silica particles, when amorphous silica is used, particles having an average particle diameter of 10 to 200 μm, preferably 30 to 100 μm are used.
When the average particle size of the amorphous silica particles is less than 10 μm, the reaction with the alumina particles occurs at an early stage, and as the sintering proceeds, voids that should remain in the places where the silica particles existed are outside the fired body. It is expelled and the entire fired body shrinks.
On the other hand, when the average particle diameter of the amorphous silica exceeds 200 μm, the dense mullite sintered structure formed in the vicinity of the silica particles makes it difficult to diffuse the silica particles, and the total amount of the silica particles may be involved in the mullite generation reaction. Unreacted, unreacted silica remains.
また、原料のシリカ粒子として、結晶質シリカを用いる場合、平均粒径５〜５０μｍ、好ましくは、１０〜３０μｍの粒子を用いる。
結晶質シリカ粒子は、非晶質シリカ粒子に比べて拡散しにくいため、上記のように、より微細な粒子を用いる。
結晶質シリカ粒子の平均粒径が５μｍ未満である場合、アルミナ粒子との反応性が高く、早期にムライト生成反応が起き、粒径が小さい非晶質シリカ粒子を用いた場合と同様に、シリカ粒子が存在した箇所に残存すべき空隙が消失し、焼成体全体が収縮する。
一方、結晶質シリカ粒子の平均粒径が５０μｍを超える場合、粒径が大きい非晶質シリカ粒子を用いた場合と同様に、未反応のシリカが残留する。
前記結晶質シリカ粒子としては、石英を用いることが好ましい。
Further, when crystalline silica is used as the raw material silica particles, particles having an average particle diameter of 5 to 50 μm, preferably 10 to 30 μm are used.
Crystalline silica particles are less likely to diffuse than amorphous silica particles, so finer particles are used as described above.
When the average particle size of the crystalline silica particles is less than 5 μm, the reactivity with the alumina particles is high, the mullite generation reaction occurs at an early stage, and the silica particles as in the case of using amorphous silica particles with a small particle size are used. The voids that should remain in the places where the particles existed disappeared, and the entire fired body contracted.
On the other hand, when the average particle diameter of the crystalline silica particles exceeds 50 μm, unreacted silica remains as in the case of using amorphous silica particles having a large particle diameter.
Quartz is preferably used as the crystalline silica particles.
原料中のアルミナ粒子とシリカ粒子との配合比率は、アルミナ粒子７４〜８５重量％、シリカ粒子１５〜２６重量％とする。
シリカ粒子が１５重量％未満である場合、ムライトの生成量が少なくなる。
一方、シリカ粒子が２６％を超える場合、生成したムライトの結晶粒子間にガラス状のシリカが残留する。
ムライト（３Ａｌ2Ｏ3・２ＳｉＯ2）を生成するのに必要なＡｌ2Ｏ3／ＳｉＯ2重量比の理論値は７１．８／２８．２であるが、実際上、上記のような粒径の粒子同士の反応を考慮すると、シリカ粒子の配合比率は、２０〜２６重量％であることが好ましい。
The mixing ratio of the alumina particles and the silica particles in the raw material is set to 74 to 85% by weight of alumina particles and 15 to 26% by weight of silica particles.
When the silica particles are less than 15% by weight, the amount of mullite produced is reduced.
On the other hand, when the silica particles exceed 26%, glassy silica remains between the produced mullite crystal particles.
The theoretical value of the Al 2 O 3 / SiO 2 weight ratio required to produce mullite (3Al 2 O 3 .2SiO 2 ) is 71.8 / 28.2, but in practice the particle size as described above Considering the reaction between the particles, the mixing ratio of the silica particles is preferably 20 to 26% by weight.
上記のような原料配合組成からなり、未反応シリカが残留していない焼成体は、気孔率２０％以上、かつ、焼成時の寸法変化率が±１％以内のムライト質耐火物として得ることができ、電子部品の焼成用道具材に好適に用いることができる。 A fired body comprising the above raw material blend composition and having no unreacted silica remaining can be obtained as a mullite refractory having a porosity of 20% or more and a dimensional change rate during firing within ± 1%. And can be suitably used as a tool material for firing electronic components.
本発明に係る他の態様のムライト質耐火物は、上記と同様のアルミナ粒子とシリカ粒子とからなる混合物を結合材とし、それ以外に骨材を配合したものを原料とした焼成体からなるものである。
すなわち、前記原料組成は、平均粒径５０〜５０００μｍのアルミナ粒子またはムライト粒子からなる骨材９０重量％以下、および、平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子もしくは平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２５重量％との混合物からなる結合材１０重量％以上である。
The mullite refractory according to another aspect of the present invention is composed of a fired body obtained by using a mixture of alumina particles and silica particles similar to the above as a binder, and other than that, a mixture of aggregate. It is.
That is, the raw material composition is 90% by weight or less of aggregate made of alumina particles or mullite particles having an average particle size of 50 to 5000 μm, 74 to 85% by weight of alumina particles having an average particle size of 1 to 10 μm, and an average particle size of 10 It is 10% by weight or more of a binder composed of a mixture of amorphous silica particles having a particle diameter of ˜200 μm or crystalline silica particles having an average particle diameter of 5 to 50 μm.
上記のように、骨材には、平均粒径５０〜５０００μｍ以上のアルミナ粒子またはムライト粒子を用いる。
骨材の平均粒径が５０μｍ未満である場合は、焼成時おける収縮率が大きくなる。
骨材の平均粒子径は、大きい方が好ましいが、実際上、耐火物を構成する上では、５０００μｍ以下であることが好ましい。
As described above, alumina particles or mullite particles having an average particle size of 50 to 5000 μm or more are used for the aggregate.
When the average particle size of the aggregate is less than 50 μm, the shrinkage rate during firing increases.
The average particle size of the aggregate is preferably larger, but in practice, it is preferably 5000 μm or less in constituting the refractory.
また、前記原料の配合比率は、骨材９０重量％以下、結合材１０重量％以上とする。
結合材の配合比率が１０重量％未満である場合、焼成時における収縮率を小さくすることはできるが、機械的強度が低下する。
前記結合材の配合比率は、１０重量％以上５０重量％以下であることが好ましい。
The mixing ratio of the raw materials is 90% by weight or less of aggregate and 10% by weight or more of binder.
When the blending ratio of the binder is less than 10% by weight, the shrinkage during firing can be reduced, but the mechanical strength is lowered.
The blending ratio of the binder is preferably 10% by weight or more and 50% by weight or less.
上記のような骨材と結合材とを原料とするムライト質耐火物は、焼成時の寸法変化率が±０．１％以内とより一層抑制され、３点曲げ強度が１０ＭＰａ以上と機械的強度にも優れたものである。 The mullite refractories using the aggregate and the binder as described above are further suppressed in the dimensional change rate during firing within ± 0.1%, and the three-point bending strength is 10 MPa or more and the mechanical strength. It is also excellent.
なお、本発明に係るムライト質耐火物を製造する際は、前記原料の混合時に、均一分散性、成形性等の向上のため、ポリビニルアルコール（ＰＶＡ）等の有機結合剤、ポリエチレングリコール等の分散剤、水等を必要に応じて、適宜添加して差し支えない。 In addition, when producing the mullite refractory according to the present invention, an organic binder such as polyvinyl alcohol (PVA), a dispersion of polyethylene glycol or the like is added to improve the uniform dispersibility and moldability when the raw materials are mixed. An agent, water, etc. may be added as needed.
また、混合方法は、一般的な方法を用いることができ、例えば、ミキサー、ボールミル、ジェットミル等により行うことができる。
また、成形方法も、特に限定されるものではなく、加圧成形、押出し成形、鋳込み成形等の一般的な方法を用いることができる。
Moreover, the mixing method can use a general method, for example, can be performed by a mixer, a ball mill, a jet mill, etc.
Also, the molding method is not particularly limited, and general methods such as pressure molding, extrusion molding, and casting molding can be used.
成形体の焼成は、焼成体中に、気孔を消失させることなく、ムライトの緻密な焼結組織を生成させる観点から、１５００〜１８００℃であることが好ましい。 Firing of the molded body is preferably 1500 to 1800 ° C. from the viewpoint of generating a dense sintered structure of mullite without eliminating pores in the fired body.
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。
［実施例１〜９、比較例１〜７］
表１に示した平均粒径のアルミナ粒子およびシリカ粒子に有機結合剤としてＰＶＡ１重量％を加えて混合・成形した後、ガス炉で１７５０℃で６時間焼成し、実施例１〜９および比較例１〜７の各焼成耐火物を得た。
得られた各耐火物について、焼成時の寸法変化率および気孔率を測定し、また、顕微鏡観察により、未反応シリカの有無を確認した。
これらの結果を表１にまとめて示す。
EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Examples 1-9, Comparative Examples 1-7]
Examples 1 to 9 and Comparative Examples were prepared by adding 1% by weight of PVA as an organic binder to the alumina particles and silica particles having the average particle size shown in Table 1 and mixing and molding them, followed by firing at 1750 ° C. for 6 hours in a gas furnace. 1 to 7 fired refractories were obtained.
About each obtained refractory, the dimensional change rate and the porosity at the time of baking were measured, and the presence or absence of the unreacted silica was confirmed by microscopic observation.
These results are summarized in Table 1.
表１に示したように、本発明に係る配合組成からなるムライト質耐火物（実施例１〜９）は、気孔率が２０％以上であり、未反応シリカの残留もなく、焼成時の寸法変化率が±１％以内に抑制されていることが認められた。 As shown in Table 1, the mullite refractories (Examples 1 to 9) having the composition according to the present invention have a porosity of 20% or more, no unreacted silica remains, and dimensions during firing. It was observed that the rate of change was suppressed within ± 1%.
［実施例１０〜１３、比較例８〜１２］
表２に示す粒径のアルミナ５０重量％およびムライト５０重量％の混合物からなる骨材に、平均粒径６μｍのアルミナ粒子８０重量％および平均粒径１５μｍのシリカ（石英）粒子２０重量％の混合物からなる結合材を、表２に示す配合量で添加混合し、さらに、有機結合剤としてＰＶＡ１重量％、水３重量％を加えて混合した後、成形体を作製し、ガス炉で１７５０℃で６時間焼成し、実施例１０〜１３および比較例８〜１２の各焼成耐火物を得た。
得られた各耐火物について、焼成時の寸法変化率および３点曲げ強度を測定した。
これらの結果を表２にまとめて示す。
[Examples 10 to 13, Comparative Examples 8 to 12]
A mixture composed of an aggregate of 50% by weight of alumina and 50% by weight of mullite shown in Table 2 and a mixture of 80% by weight of alumina particles having an average particle diameter of 6 μm and 20% by weight of silica (quartz) particles having an average particle diameter of 15 μm After adding and mixing a binder composed of the following components in the blending amounts shown in Table 2, and further adding 1% by weight of PVA and 3% by weight of water as an organic binder, a molded body was prepared and the mixture was heated at 1750 ° C. in a gas furnace. It fired for 6 hours and obtained each baked refractory of Examples 10-13 and Comparative Examples 8-12.
About each obtained refractory, the dimensional change rate at the time of baking and three-point bending strength were measured.
These results are summarized in Table 2.
表２に示したように、本発明に係る骨材と結合材とを原料としたムライト質耐火物（実施例１０〜１３）は、焼成時の寸法変化率が±０．１％以内に抑制され、また、３点曲げ強度が１０ＭＰａ以上と機械的強度にも優れていることが認められた。 As shown in Table 2, in the mullite refractories (Examples 10 to 13) using the aggregate and the binder according to the present invention as raw materials, the dimensional change rate during firing is suppressed within ± 0.1%. In addition, it was confirmed that the three-point bending strength was 10 MPa or more and excellent in mechanical strength.
Claims (4)
前記結合材が、平均粒径１〜１０μｍのアルミナ粒子７４〜８５重量％と、平均粒径１０〜２００μｍの非晶質シリカ粒子または平均粒径５〜５０μｍの結晶質シリカ粒子１５〜２６重量％との混合物からなることを特徴とするムライト質耐火物。 It consists of a fired body made of 90% by weight or less of an aggregate made of alumina particles or mullite particles having an average particle size of 50 to 5000 μm and a binder of 10% by weight or more,
The binder is 74 to 85% by weight of alumina particles having an average particle diameter of 1 to 10 μm and 15 to 26% by weight of amorphous silica particles having an average particle diameter of 10 to 200 μm or crystalline silica particles having an average particle diameter of 5 to 50 μm. A mullite refractory characterized by comprising a mixture of
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