JPH0446058A - Alumina-silica-based sintered body and production thereof - Google Patents
Alumina-silica-based sintered body and production thereofInfo
- Publication number
- JPH0446058A JPH0446058A JP2154654A JP15465490A JPH0446058A JP H0446058 A JPH0446058 A JP H0446058A JP 2154654 A JP2154654 A JP 2154654A JP 15465490 A JP15465490 A JP 15465490A JP H0446058 A JPH0446058 A JP H0446058A
- Authority
- JP
- Japan
- Prior art keywords
- mullite
- silica
- alumina
- particle size
- sintered body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 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 claims abstract description 51
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 51
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 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 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000002734 clay mineral Substances 0.000 claims abstract description 4
- 239000004575 stone Substances 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 37
- 239000000463 material Substances 0.000 abstract description 12
- 238000005245 sintering Methods 0.000 abstract description 6
- 229910052681 coesite Inorganic materials 0.000 abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 abstract description 4
- 229910052593 corundum Inorganic materials 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 abstract 2
- 238000004131 Bayer process Methods 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 4
- 239000005995 Aluminium silicate Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 235000012211 aluminium silicate Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003779 heat-resistant material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WHOPEPSOPUIRQQ-UHFFFAOYSA-N oxoaluminum Chemical compound O1[Al]O[Al]1 WHOPEPSOPUIRQQ-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はアルミナ・シリカ系焼結体及びその製造方法に
係り、特に高温強度等の特性に優れ、しかも安価に提供
されるアルミナ・シリカ系焼結体及びその製造方法に関
する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an alumina-silica-based sintered body and a method for producing the same, and particularly relates to an alumina-silica-based sintered body that has excellent properties such as high-temperature strength and is inexpensively provided. The present invention relates to a sintered body and a method for manufacturing the same.
Ｃ従来の技術］
ムライトはＡ Ｊ２２．０ 、とＳｉＯ２からなり、化
学組成は理論的には３ＡＩＬ２０３−２Ｓ ｉ ０２で
あり、その特性としては、耐熱性に優れ、特にクリープ
特性が良好である。また、熱衝撃特性は良好であるが電
気的特性はあまり良くない。C. Prior Art] Mullite is composed of A J22.0 and SiO2, and its chemical composition is theoretically 3AIL203-2S i 02, and its properties include excellent heat resistance and particularly good creep properties. Also, although the thermal shock properties are good, the electrical properties are not so good.
ムライトセラミックスはオールドセラミックスに属し、
その研究の歴史は永く、原料としては、アルミナ源とし
てカオリン、バイヤーアルミナ、シリカ源として珪石が
主に用いられている。最近では、天然ムライトを改賞す
ることにより、合成ムライト並の物性を比すことができ
るようになったが、この研究の主体はムライト組成中の
シソカ相の析出及びガラス化の防止であり、原料の調製
や焼結条件などを検討したものである。Mullite ceramics belong to old ceramics.
This research has a long history, and the main raw materials used are kaolin and Bayer alumina as an alumina source, and silica as a silica source. Recently, by modifying natural mullite, it has become possible to compare its physical properties to those of synthetic mullite, but the focus of this research is to prevent the precipitation and vitrification of the shisoka phase in the mullite composition. The preparation of raw materials and sintering conditions were studied.
一方、ファインセラミックス技術を用いた高純度合成ム
ライトという理論組成の素材もあり、これは金属アルコ
キシド等の方法で理論組成となるように共沈法で製造し
たものが主である。On the other hand, there is also a material with a theoretical composition called high-purity synthetic mullite using fine ceramics technology, and this is mainly produced by a coprecipitation method using methods such as metal alkoxides to achieve the theoretical composition.
しかして、これらの原料を目的に合わせて混合し、焼結
したものがムライト系セラミックス材料といわれ、ムラ
イト系セラミックスはアルミナセラミックスと同様、高
温強度が比較的大きく、天然原料を用いたものは安価な
素材であることから、炉材、サヤ、セッター材、耐熱材
、構造材等、主に耐火材料として用いられてきた。Mullite ceramics are made by mixing and sintering these raw materials according to the purpose, and like alumina ceramics, mullite ceramics have relatively high high-temperature strength, and those made from natural raw materials are inexpensive. Because it is a durable material, it has been mainly used as a refractory material, such as furnace materials, sheaths, setter materials, heat-resistant materials, and structural materials.
［発明が解決しようとするａ題］
従来のムライト系セラミックスのうち、天然ムライトを
改質したものでは、長期間の使用や高温使用時に、Ａｆ
１２０３−５ ｉ ０２ボンデイングが分解し、シリカ
がムライトの結晶粒界にガラス相として析出する。この
ため、強度が著しく低下し、連続的な使用や繰り返しの
使用に難があつた。[Problem a to be solved by the invention] Among conventional mullite-based ceramics, those made by modifying natural mullite have a problem in that Af
1203-5 i 02 bonding decomposes and silica precipitates as a glass phase at the grain boundaries of mullite. As a result, the strength was significantly reduced, making it difficult to use continuously or repeatedly.
アルコシキト法による高純度合成ムライトは、上記欠点
を解決するために開発されたものであるが、高純度ムラ
イトは高温強度、耐久性等に大きな改善効果を有するも
のの、価格が高いために従来より用いられている耐熱材
料等の工業材料の分野で使用するにはコスト的に不利で
あった。High-purity synthetic mullite using the alkoxyquito method was developed to solve the above-mentioned drawbacks. Although high-purity mullite has the effect of greatly improving high-temperature strength and durability, it is expensive and has not been used in the past. It was disadvantageous in terms of cost for use in the field of industrial materials such as heat-resistant materials.
本発明は上記従来の問題点を解決し、高温強度等の特性
に優れ、かつ安価に提供されるムライト組成のアルミナ
・シリカ系焼結体及びその製造方法を提供することを目
的とする。It is an object of the present invention to solve the above-mentioned conventional problems and to provide an alumina-silica-based sintered body having a mullite composition that has excellent properties such as high-temperature strength and can be provided at low cost, and a method for producing the same.
［課題を解決するための手段］
請求項（１）のアルミナ・シリカ系焼結体は、ＺｒＯ２
（酸化ジルコニウム）及びムライトよりなり、Ｚ ｒｏ
２含有量がムライトに対して３〜３０重量％であって、
ムライト粒径が１０〜１００μｍであることを特徴とす
る
請求項（２）のアルミナ・シリカ系焼結体の製造方法は
、精製粘土鉱物、バイヤーアルミナ、水酸化アルミニウ
ム及び珪石よりなる群から選ばれる少なくとも２種を主
原料として、ＡＪ２２０３／ＳｉＯ２の組成比がムライ
ト生成範囲となるように調合し、該調合原料を９０％以
上が粒径５μｍ以下となるように湿式粉砕した後、粒径
３０μｍ以下のＺ ｒ０２を前記調合原料に対して３〜
３０重量％添加混合し、次いで、得られた混合物を乾燥
、解砕し、その後、有機質バインダーを用いて成形し、
成形体を１６００℃以上の温度で１時間以上焼成するこ
とを特徴とする。[Means for solving the problem] The alumina-silica-based sintered body of claim (1) comprises ZrO2
(zirconium oxide) and mullite, Z ro
2 content is 3 to 30% by weight based on mullite,
The method for producing an alumina-silica-based sintered body according to claim (2), characterized in that the mullite particle size is 10 to 100 μm, is selected from the group consisting of refined clay minerals, Bayer alumina, aluminum hydroxide, and silica stone. At least two types of main raw materials are blended so that the composition ratio of AJ2203/SiO2 falls within the mullite production range, and the blended raw materials are wet-pulverized so that 90% or more have a particle size of 5 μm or less, and then the particle size is 30 μm or less. Z r02 of 3 to 3 to the above blended raw materials
30% by weight was added and mixed, then the resulting mixture was dried and crushed, and then molded using an organic binder,
It is characterized in that the molded body is fired at a temperature of 1600° C. or higher for 1 hour or more.
即ち、本発明は、原料として従来より用いられている安
価な原料を用い、物性改良の手段として、特定のセラミ
ックス粒子を第２相としてムライト結晶内又は粒界面に
分散させることにより高強度化を図り、高純度合成ムラ
イト並の特性を有する材料を提供するものである。That is, the present invention uses inexpensive raw materials that have been conventionally used as raw materials, and as a means of improving physical properties, high strength is achieved by dispersing specific ceramic particles as a second phase within mullite crystals or at grain boundaries. The aim is to provide a material with properties comparable to that of high-purity synthetic mullite.
以下に本発明の詳細な説明する。The present invention will be explained in detail below.
請求項（１）のアルミナ・シリカ系焼結体は、ムライト
に対して３〜３０重量％のＺ ｒ０２を含有するもので
ある。Ｚｒ０ａの含有量がムライトに対して３重量％未
満では本発明による強度の改善効果が得られず、３０重
量％を超えるとＺ ｒｏ２の量が多くなり過ぎて、アル
ミナ・シリカ系焼結体としての特性が損なわれる。従っ
て、本発明においては、ＺｒＯ２含有量はムライトに対
して３〜３０重量％とする。特に、ＺｒＯ２含有量がム
ライトに対して５〜２０重量％であると、とりわけ高強
度なアルミナ・シリカ系焼結体を得ることができる。The alumina-silica-based sintered body according to claim (1) contains Zr02 in an amount of 3 to 30% by weight based on mullite. If the content of Zr0a is less than 3% by weight based on mullite, the strength improvement effect according to the present invention cannot be obtained, and if it exceeds 30% by weight, the amount of Zro2 becomes too large, making it difficult to use as an alumina-silica-based sintered body. characteristics are impaired. Therefore, in the present invention, the ZrO2 content is 3 to 30% by weight based on mullite. In particular, when the ZrO2 content is 5 to 20% by weight based on mullite, an alumina-silica sintered body with particularly high strength can be obtained.
請求項（１）のアルミナ・シリカ系焼結体中のムライト
結晶は、粒径が１００μｍの範囲のものである。ムライ
ト結晶の粒径が１００μｍよりも大きいと得られるアル
ミナ・シリカ系焼結体の曲げ強度が低下し、また１０μ
ｍよりも小さいとＺｒＯ２粒子が結晶内又は粒界面に取
り込まれ難くなる。従って、ムライト結晶の粒径は１０
〜１００μｍ、好ましくは１０〜５０μｍとする。The mullite crystals in the alumina-silica sintered body according to claim (1) have a grain size in the range of 100 μm. If the grain size of the mullite crystal is larger than 100 μm, the bending strength of the alumina-silica sintered body obtained will decrease;
When it is smaller than m, it becomes difficult for ZrO2 particles to be taken into the crystal or at the grain interface. Therefore, the grain size of mullite crystals is 10
~100 μm, preferably 10-50 μm.
一方、ＺｒＯ２粒子の粒径が微細過ぎると、ムライトと
均一に混合することが難しい、逆にＺｒＯ２粒子の粒径
が大き過ぎるとムライト結晶粒界にのみＺｒＯ２が存在
するようになり、粒界クランク発生の原因となる。従っ
て、本発明において、ＺｒＯ２粒子の粒径は３０μｍ以
下、特に１０μｍ以下、とりわけ３〜１０μｍであるこ
とが好ましい。On the other hand, if the particle size of ZrO2 particles is too fine, it is difficult to mix uniformly with mullite.On the other hand, if the particle size of ZrO2 particles is too large, ZrO2 will exist only at the mullite grain boundaries, causing grain boundary cranking. cause the occurrence. Therefore, in the present invention, the particle size of the ZrO2 particles is preferably 30 μm or less, particularly 10 μm or less, particularly 3 to 10 μm.
なお、アルミナ・シリカ系焼結体中のムライトはその組
成が理論組成のＡｌ２Ｏ３ ／Ｓ ｉ ０２ ＝３／２
（モル比） 即ち７１．８／２８．２（重量％）である
ことが好ましい。ムライト組成のＡｌ２Ｏ２が理論組成
よりも多過ぎるとＡ、、１２２ｏ３中にムライト結晶が
分散した形となり十分な強度が得られない。逆に、ムラ
イト組成のＳｉｏ２が理論組成よりも多過ぎると、ムラ
イト中に遊離シリカ相がガラス相となって生成し、十分
な高温強度が得られない。従って、アルミナ・シリカ系
焼結体中のムライトは、理論組成Ａｌ１２０３ ／Ｓ
ｉ ０２ ＝３／２ （モル比）にできるだけ近い組成
であることが好ましい。The composition of mullite in the alumina-silica sintered body is the theoretical composition Al2O3 /S i 02 = 3/2
(Mole ratio) That is, it is preferably 71.8/28.2 (wt%). If the Al2O2 of the mullite composition is too much than the theoretical composition, mullite crystals will be dispersed in A, 122o3, and sufficient strength will not be obtained. On the other hand, if Sio2 in the mullite composition is too much than the theoretical composition, a free silica phase will form in the mullite as a glass phase, making it impossible to obtain sufficient high-temperature strength. Therefore, the mullite in the alumina-silica sintered body has the theoretical composition Al1203/S
It is preferable that the composition be as close as possible to i 02 =3/2 (molar ratio).
このような請求項（１）のアルミナ・シリカ系焼結体は
請求項（２）の方法により容易かつ効率的に低コストに
て製造することができる。The alumina-silica-based sintered body of claim (1) can be easily and efficiently produced at low cost by the method of claim (2).
以下に請求項（２）のアルミナ・シリカ系焼結体の製造
方法について説明する。The method for producing an alumina-silica-based sintered body according to claim (2) will be explained below.
請求項（２）の方法においては、まず、原料として精製
粘土鉱物、バイヤーアルミナ、水酸化アルミニウム又は
珪石（シワ力）を用い、ＡｕａＯ３／ＳｉＯ２組成比が
ムライト生成範囲、好ましくはＡ Ｊ２２０３ ／ Ｓ
ｉ Ｏ２＋３／２（モル比）となるように調合する。In the method of claim (2), first, refined clay minerals, Bayer alumina, aluminum hydroxide, or silica stone (wrinkle strength) are used as raw materials, and the AuaO3/SiO2 composition ratio is within the mullite production range, preferably A J2203/S.
i Mix to obtain O2+3/2 (molar ratio).
この場合、特にぶ料としては精製カオリンとバイヤーア
ルミナ又は水酸化アルミニウム、或いは、バイヤーアル
ミナ又は水酸化アルミニウムと珪石を用いるのが好まし
い。これらの原料はその所要量をボールミル、又はアト
ライター等によりアルコール等を用いて９０％以上が粒
径５μｍ以下となるように湿式粉砕する。次に、得られ
た粉砕物に粒径３０μｍ以下、好ましくは１０μｍ以下
、特に３〜１０μｍのＺｒＯ２を該粉砕物に対して３〜
３０重量％、好ましくは５〜２０重量％添加し、ボール
ミル等で混合する。In this case, it is particularly preferable to use purified kaolin and Bayer alumina or aluminum hydroxide, or Bayer alumina or aluminum hydroxide and silica stone as the materials. The required amount of these raw materials is wet-milled using alcohol or the like using a ball mill or attritor so that 90% or more of the powder has a particle size of 5 μm or less. Next, ZrO2 having a particle size of 30 μm or less, preferably 10 μm or less, particularly 3 to 10 μm is added to the resulting pulverized product.
Add 30% by weight, preferably 5 to 20% by weight, and mix using a ball mill or the like.
得られた混合物は乾燥・、解砕した後、ポリビニルアル
コール（ＰＶＡ）等の有機質バインダーを用いて成形す
る。成形は３００ ｋ ｇ ｆ ／ ｃ ｒｎ’以上で
の加圧成形後、１０００ ｋ ｇ ｆ ／ ｃ ｒｎ’
以上での静水圧プレス成形による２段成形で行なうの−
が好ましい。The obtained mixture is dried and crushed, and then molded using an organic binder such as polyvinyl alcohol (PVA). Molding is performed at 1000 kg f/c rn' after pressure molding at 300 kg f/c rn' or more.
This is done in two stages using isostatic press molding as described above.
is preferred.
得られた成形体はホットプレス又は寓圧焼結により焼成
し、アルミナ・シリカ系焼結体を得る。The obtained molded body is fired by hot pressing or pressure sintering to obtain an alumina-silica sintered body.
この場合、昇温速度は５０〜ｂ
るのが好ましく、焼成温度は１６００℃以上、好ましく
は１６００〜１６５０℃とし、焼成時間は１時間以上、
好ましくは１〜３時間とするのが好ましい。なお、ホッ
トプレスを採用する場合、圧力は３００〜６００ ｋ
ｇ ／ ｃ ｒｎ’程度とするのが好ましい。In this case, it is preferable that the temperature increase rate is 50 to 50°C, the firing temperature is 1600°C or higher, preferably 1600 to 1650°C, and the firing time is 1 hour or more.
Preferably, the time is 1 to 3 hours. In addition, when using a hot press, the pressure is 300 to 600 k
It is preferable to set it to about g/crn'.
〔作用］
一般に、精製カオリン、バイヤーアルミナ、水酸化アル
ミニウム又は珪石等の原料を用いて、これをボールミル
等で微粉砕して混合しても、原子レベルで理論組成に混
合することは不可能であり、焼結により拡散させるため
には長時間を必要とする。[Function] In general, even if raw materials such as refined kaolin, Bayer alumina, aluminum hydroxide, or silica stone are used and mixed by finely pulverizing them with a ball mill, etc., it is impossible to mix them to the theoretical composition at the atomic level. However, it takes a long time to diffuse through sintering.
これに対して、ムライト組成中に第２相としてＺｒＯ２
粒子を３〜３０重量％添加するど、ボールミル等による
粉砕混合でも、通常の成形、焼成により高温強度に優れ
たアルミナ・シリカ系焼結体が得られる。On the other hand, ZrO2 is present as a second phase in the mullite composition.
When particles are added in an amount of 3 to 30% by weight, an alumina-silica-based sintered body having excellent high-temperature strength can be obtained by conventional molding and firing, even by pulverizing and mixing using a ball mill or the like.
本発明において、ＺｒＯ２添加による高温強度改善の機
構の詳細は明らかではないが、ムライト結晶内又は粒界
面に取り込まれたＺ ｒ０２粒子がムライト中の５ｉ０
２のガラス相への移動をブロックしているため、更には
、ｚ「０２粒子がムライト結晶粒内や結晶粒界−＼分散
し、ムライト結晶の成長を抑制しているためと考えられ
る。In the present invention, although the details of the mechanism of high-temperature strength improvement due to the addition of ZrO2 are not clear, the Zr02 particles incorporated into the mullite crystals or at the grain interfaces increase the 5i0
It is thought that this is because the movement of 2 to the glass phase is blocked, and furthermore, the z'02 particles are dispersed within the mullite crystal grains and at the grain boundaries, suppressing the growth of the mullite crystals.
［実施例］
以下に実施例及び比較例を挙げて本発明をより具体的に
説明する。[Example] The present invention will be described in more detail with reference to Examples and Comparative Examples below.
実施例１．２、比較例１
精製したカオリナイトに組成がＡｆ１２０３ ／５ｔＯ
２＝３／２（モル比）となるようにアルミすを添加、シ
、ボールミル（Ｚｒ０２ボール）によりアルコールを用
いて４８時時間式粉砕した。なお、この場合、メディア
攪拌型粉砕機（アトライター）を用いると１〜２時間で
処理することが可能である。原料を９０％以上が粒径５
μｍ以下となるように粉砕した後、これにＺｒＯ２粉末
（試薬特級を焼結、分級したもの）を第１表に示す量添
加しく比較例１は添加せず）、更にボールミルで５時間
混合した。これを乾燥、解砕した後、有機質バインダー
（ＰＶＡ）を５重量％添加して十分に混練した。Example 1.2, Comparative Example 1 Purified kaolinite with composition Af1203/5tO
Aluminum was added so that the molar ratio was 2=3/2, and the mixture was milled using alcohol in a ball mill (Zr02 ball) for 48 hours. In this case, if a media agitation type pulverizer (attritor) is used, the treatment can be completed in 1 to 2 hours. More than 90% of the raw materials have a particle size of 5
After pulverizing to a particle size of μm or less, ZrO2 powder (sintered and classified special grade reagent) was added in the amount shown in Table 1 (not added in Comparative Example 1), and further mixed in a ball mill for 5 hours. . After drying and crushing this, 5% by weight of an organic binder (PVA) was added and thoroughly kneaded.
混練物をプレス成形により５０ｍｍφＸ５ｍｍに５００
ｋｇ／ｃｍ”で成形した後、ラバープレスにより１５０
０ｋｇ／ｃｍ”で更に加圧して成形体を得た。この成形
体を焼結してムライト組成のアルミナ・シリカ系焼結体
を得た。なお、焼結はホットプレスを用い、昇温速度は
１５０℃／ ｈ ｒとし、３００ｋｇ／ｃｒｎ’にて１
６００℃で１時間行なった。The kneaded material was press-molded into a size of 50 mmφ x 5 mm.
kg/cm” and then rubber press to 150 kg/cm”.
A compact was obtained by further pressurizing at 0 kg/cm''. This compact was sintered to obtain an alumina-silica sintered compact with a mullite composition. The sintering was performed using a hot press, and the heating rate was is 150℃/hr, 1 at 300kg/crn'
The test was carried out at 600°C for 1 hour.
得られた焼結体の諸特性を第１表に示す。Table 1 shows various properties of the obtained sintered body.
第
表
第１表より所定量のＺｒＯ２を添加したムライト組成の
アルミナ・シリカ系焼結体により、常温から１０００℃
といった高温まで安定して著しく高い強度が得られるこ
とが明らかである。Table 1 shows that the alumina-silica sintered body with a mullite composition added with a specified amount of ZrO2 can be heated from room temperature to 1000℃.
It is clear that extremely high strength can be obtained stably up to such high temperatures.
［発明の効果］
以上詳述した通り、本発明のアルミナ・シリカ系焼結体
は、安価な原料を用いて低コストに提供されるものであ
り、しかも、高温強度、耐久性等の特性に著しく優れる
。従って、本焼結体は、工業用耐火材料等として、長期
にわたり極めて有効に使用することができる。[Effects of the Invention] As detailed above, the alumina-silica-based sintered body of the present invention is provided at low cost using inexpensive raw materials, and has excellent properties such as high-temperature strength and durability. Remarkably superior. Therefore, the present sintered body can be used extremely effectively over a long period of time as an industrial fireproof material.
しかして、このような本発明の焼結体は、本発明の方法
により容易かつ効率的に低コストにて製造することが可
能とされる。Therefore, such a sintered body of the present invention can be manufactured easily, efficiently, and at low cost by the method of the present invention.
Claims (2)
あって、ムライト粒径が１０〜１００μｍであることを
特徴とするアルミナ・シリカ系焼結体。(1) An alumina-silica-based sintered body consisting of ZrO_2 and mullite, characterized in that the ZrO_2 content is 3 to 30% by weight based on the mullite, and the mullite particle size is 10 to 100 μm.
ニウム及び珪石よりなる群から選ばれる少なくとも２種
を主原料として、Ａｌ＿２Ｏ＿３／ＳｉＯ＿２の組成比
がムライト生成範囲となるように調合し、該調合原料を
９０％以上が粒径５μｍ以下となるように湿式粉砕した
後、粒径３０μｍ以下のＺｒＯ＿２を前記調合原料に対
して３〜３０重量％添加混合し、次いで、得られた混合
物を乾燥、解砕し、その後、有機質バインダーを用いて
成形し、成形体を１６００℃以上の温度で１時間以上焼
成することを特徴とするアルミナ・シリカ系焼結体の製
造方法。(2) At least two selected from the group consisting of purified clay minerals, Bayer alumina, aluminum hydroxide, and silica stone are blended as main raw materials so that the composition ratio of Al_2O_3/SiO_2 falls within the mullite production range, and the blended raw materials are After wet-pulverizing so that 90% or more of the particles have a particle size of 5 μm or less, 3 to 30% by weight of ZrO_2 with a particle size of 30 μm or less is added and mixed to the blended raw materials, and then the resulting mixture is dried and crushed. A method for producing an alumina-silica-based sintered body, which comprises: then molding using an organic binder, and firing the molded body at a temperature of 1600° C. or higher for 1 hour or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2154654A JPH0446058A (en) | 1990-06-13 | 1990-06-13 | Alumina-silica-based sintered body and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2154654A JPH0446058A (en) | 1990-06-13 | 1990-06-13 | Alumina-silica-based sintered body and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0446058A true JPH0446058A (en) | 1992-02-17 |
Family
ID=15588964
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2154654A Pending JPH0446058A (en) | 1990-06-13 | 1990-06-13 | Alumina-silica-based sintered body and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0446058A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013514960A (en) * | 2009-12-21 | 2013-05-02 | コンセホ スペリオール デ インベスティガシオネス シエンティフィカス（セエセイセ） | COMPOSITE MATERIAL WITH CONTROLLED CTE, INCLUDING OXIDE CERAMIC AND PROCESS FOR OBTAINING THE COMPOSITE MATERIAL |
| US20180327314A1 (en) * | 2015-11-05 | 2018-11-15 | Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh | Sintered zirconia mullite refractory composite, methods for its production and use thereof |
-
1990
- 1990-06-13 JP JP2154654A patent/JPH0446058A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013514960A (en) * | 2009-12-21 | 2013-05-02 | コンセホ スペリオール デ インベスティガシオネス シエンティフィカス（セエセイセ） | COMPOSITE MATERIAL WITH CONTROLLED CTE, INCLUDING OXIDE CERAMIC AND PROCESS FOR OBTAINING THE COMPOSITE MATERIAL |
| US20180327314A1 (en) * | 2015-11-05 | 2018-11-15 | Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh | Sintered zirconia mullite refractory composite, methods for its production and use thereof |
| US11208354B2 (en) | 2015-11-05 | 2021-12-28 | Imertech Sas | Sintered zirconia mullite refractory composite, methods for its production and use thereof |
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