JP2959770B2 - Method for producing high-purity porous silica material - Google Patents
Method for producing high-purity porous silica materialInfo
- Publication number
- JP2959770B2 JP2959770B2 JP63250460A JP25046088A JP2959770B2 JP 2959770 B2 JP2959770 B2 JP 2959770B2 JP 63250460 A JP63250460 A JP 63250460A JP 25046088 A JP25046088 A JP 25046088A JP 2959770 B2 JP2959770 B2 JP 2959770B2
- Authority
- JP
- Japan
- Prior art keywords
- silica powder
- slip
- sol
- silica
- porous
- 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.)
- Expired - Fee Related
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 75
- 239000000377 silicon dioxide Substances 0.000 title claims description 37
- 239000000463 material Substances 0.000 title description 10
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000843 powder Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910052602 gypsum Inorganic materials 0.000 description 4
- 239000010440 gypsum Substances 0.000 description 4
- 238000007569 slipcasting Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 10 mol of H 2 O Chemical compound 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は高純度のシリカ質多孔体を製造する方法に関
する。The present invention relates to a method for producing a high-purity porous silica material.
例えば、光学的に良質な石英ガラスを得るためには、
一旦良質なシリカ質多孔体を製造し、これを焼成する必
要がある。For example, to obtain optically good quartz glass,
It is necessary to once produce a high-quality porous silica material and fire it.
従来、良質なシリカ質多孔体を製造する方法として
は、スリップキャスト法、VAD法、ゾルーゲル法などが
知られている。Conventionally, a slip casting method, a VAD method, a sol-gel method and the like are known as methods for producing a high-quality porous silica material.
スリップキャスト法は石膏型にシリカ質のスリップを
流し込み、溶媒を排出させてシリカ質多孔体を得る方法
である。The slip casting method is a method of pouring a siliceous slip into a gypsum mold and discharging the solvent to obtain a siliceous porous body.
VAD法は四塩化珪素を酸水素炎で加水分解し、ターゲ
ット上にスートを堆積させる方法である。The VAD method is a method of hydrolyzing silicon tetrachloride with an oxyhydrogen flame and depositing soot on a target.
ゾルーゲル法は液相で金属アルコキシドを加水分解し
て重縮合させてシリカ質多孔体を得る方法である。この
方法では、高純度のシリカ質多孔体が得られる。The sol-gel method is a method in which a metal alkoxide is hydrolyzed and polycondensed in a liquid phase to obtain a porous silica material. In this method, a high-purity porous silica material is obtained.
しかし、従来の方法にはそれぞれ以下のような問題が
あった。However, each of the conventional methods has the following problems.
すなわち、スリップキャスト法では、比較的気孔半径
の大きいシリカ質多孔体が得られるが、石膏型を使用す
るという性格上、特に溶媒が酸性の場合には石膏が侵さ
れてCaが溶出し、多孔体が汚染されるので、高純度のシ
リカ質多孔体を得ることができなかった。しかも、水分
量の増加に伴い、石膏型による吸水速度が減少してしま
うという問題があった。That is, in the slip casting method, a silica porous body having a relatively large pore radius can be obtained.However, due to the use of a gypsum mold, particularly when the solvent is acidic, gypsum is attacked and Ca is eluted, and the porous material is porous. Since the body was contaminated, a high-purity porous silica material could not be obtained. In addition, there is a problem that the water absorption rate of the gypsum mold decreases with an increase in the water content.
また、VAD法では、原料歩留まりが低く、しかも高強
度のシリカ質多孔体が得られず、その形状も限定される
という問題があった。In addition, the VAD method has a problem in that the yield of the raw material is low and a high-strength porous silica material cannot be obtained, and the shape thereof is limited.
また、ゾルーゲル法では、沈降速度を考慮して粒径が
非常に小さくBET比表面積100m2/g以上の微粉を用いるた
め、成形される多孔体の気孔も非常に小さく、気孔半径
は0.1μｍ以下に限られていた。このため、乾燥工程に
おいて多孔体にはキャピラリーストレスによってクラッ
クが入りやすく、大型の多孔体が得られないという問題
があった。こうした問題を解決するために、ゾルーゲル
法では超臨界溶媒抽出法や乾燥制御添加剤（DCCA）が検
討されている。In addition, in the sol-gel method, since the fine particles having a very small particle size and a BET specific surface area of 100 m 2 / g or more are used in consideration of the sedimentation velocity, the pores of the formed porous body are also very small, and the pore radius is 0.1 μm or less. Was limited to For this reason, in the drying step, cracks easily occur in the porous body due to capillary stress, and there is a problem that a large-sized porous body cannot be obtained. In order to solve these problems, supercritical solvent extraction and drying control additives (DCCA) have been studied in the sol-gel method.
本発明はこれらの問題点を解決するためになされたも
のであり、短い成形時間で、高純度でかつ乾燥時に割れ
にくいシリカ質多孔体を製造し得る方法を提供すること
を目的とする。The present invention has been made in order to solve these problems, and an object of the present invention is to provide a method capable of producing a high-purity siliceous porous material which is hard to be broken when dried in a short molding time.
本発明の高純度シリカ質多孔体の製造方法は、金属ア
ルコキシシランを部分的に加水分解させたゾルと、平均
粒子径が１〜10μｍのシリカ粉末とを、該シリカ粉末が
20〜60vol％となるように混合してスリップを調製した
後、該スリップをフィルターを有する圧力容器に収容
し、ガスの圧力によって溶媒をろ過して成形し、さらに
ガスを流し続けて乾燥させることを特徴とするものであ
る。The method for producing a high-purity porous silica material of the present invention comprises: a sol obtained by partially hydrolyzing a metal alkoxysilane; and a silica powder having an average particle diameter of 1 to 10 μm.
After preparing a slip by mixing so as to have a volume of 20 to 60% by volume, the slip is housed in a pressure vessel having a filter, the solvent is filtered by a gas pressure, the solvent is formed, and the gas is kept flowing and dried. It is characterized by the following.
以下、本発明方法を更に詳細に説明する。 Hereinafter, the method of the present invention will be described in more detail.
本発明方法は0.2μｍ程度の比較的大きい気孔半径を
有する多孔体を得るのに有利な方法である。The method of the present invention is an advantageous method for obtaining a porous body having a relatively large pore radius of about 0.2 μm.
本発明においては、まず金属アルコキシシラン、アル
コール、純水、塩酸を混合して、金属アルコキシシラン
を部分的に加水分解させたゾルを調製する。標準的なゾ
ルの組成としては、例えばTEOS（テトラエトキシシラ
ン）１モル、エタノール５モル、H2O10モルからなり、H
Clを添加してpH4に調整したものを挙げることができ
る。このような系でエタノール５モル、H2O10モル、及
びHClを添加してpH4に調整するという条件を固定し、TE
OSの添加量を変化させた場合、TEOSの添加量は0.1モル
以上とすることが望ましい。In the present invention, a sol in which a metal alkoxysilane is partially hydrolyzed is prepared by mixing a metal alkoxysilane, an alcohol, pure water and hydrochloric acid. The composition of a standard sol is, for example, 1 mol of TEOS (tetraethoxysilane), 5 mol of ethanol, 10 mol of H 2 O,
One that has been adjusted to pH 4 by adding Cl can be mentioned. In such a system, the condition of adding 5 mol of ethanol, 10 mol of H 2 O, and HCl to adjust to pH 4 was fixed, and TE was fixed.
When the amount of OS is changed, the amount of TEOS is desirably 0.1 mol or more.
次に、このゾルに高純度シリカ粉末を混合してスリッ
プを調製する。この際、適度の粘性を有するスリップが
得られるように、ゾルとシリカ粉末との混合割合を調整
する。また、わずかな溶媒をろ過するだけで成形できる
ように濃度を調整すれば、成形スピード（着肉スピー
ド）が速くなるので効率的である。スリップの粘性は、
シリカ粉末の添加量が増加するにつれて、大きくなる傾
向を示し、ゾルとシリカ粉末との混合割合はシリカ粉末
が20〜60vol％、最適には40〜50vol％の範囲であること
が好ましい。これは、シリカ粉末が20vol％未満である
と成形スピード（着肉スピード）が遅くなりシリカ粉末
が沈降しやすくなって均一な多孔体が得られず、一方60
vol％を超えると粘性が高くなりすぎて流動性がなくな
るためである。ただし、スリップの粘性はシリカ粉末の
添加量だけでなく、粒径、粒子形状などによっても影響
を受けるので、これらの要因も考慮してゾルとシリカ粉
末との混合割合を決定することが望ましい。また、シリ
カ粉末の粒径に応じて多孔体の気孔半径を調整すること
ができ、比較的大きい気孔半径を有する多孔体を得るた
めには比較的粒径の大きいシリカ粉末を用いる。シリカ
粉末の平均粒子径は１〜10μｍで、かつ粒度分布がシャ
ープであることが望ましい。シリカ粉末の平均粒子径が
１μｍ未満では多孔体が割れやすくなり、一方10μｍを
超えると（例えば50μｍでは）シリカ粉末が沈降しやす
くなる。Next, a high-purity silica powder is mixed with the sol to prepare a slip. At this time, the mixing ratio of the sol and the silica powder is adjusted so that a slip having a proper viscosity is obtained. In addition, if the concentration is adjusted so that molding can be performed only by filtering a small amount of solvent, the molding speed (inlaying speed) is increased, which is efficient. The viscosity of the slip is
As the addition amount of the silica powder increases, it tends to increase, and the mixing ratio of the sol and the silica powder is preferably in the range of 20 to 60 vol%, most preferably 40 to 50 vol%. If the silica powder is less than 20 vol%, the molding speed (the inking speed) becomes slow, and the silica powder tends to settle, and a uniform porous body cannot be obtained.
If it exceeds vol%, the viscosity becomes too high and the fluidity is lost. However, the viscosity of the slip is affected not only by the amount of silica powder added but also by the particle size, particle shape, and the like. Therefore, it is desirable to determine the mixing ratio between the sol and the silica powder in consideration of these factors. Further, the pore radius of the porous body can be adjusted according to the particle size of the silica powder, and a silica powder having a relatively large particle size is used to obtain a porous body having a relatively large pore radius. It is desirable that the silica powder has an average particle size of 1 to 10 μm and a sharp particle size distribution. If the average particle diameter of the silica powder is less than 1 μm, the porous body is easily broken, while if it exceeds 10 μm (for example, 50 μm), the silica powder tends to settle.
従来のスリップキャスト法はこのような酸を含むスリ
ップを成形するには適さない。また、従来のゾル−ゲル
法でもこのように沈降しやすいシリカ粉末の成形は考え
られない。Conventional slip casting is not suitable for forming such acid-containing slips. Further, even with the conventional sol-gel method, molding of such a silica powder that easily precipitates cannot be considered.
次いで、前記スリップをフィルターを有する圧力容器
に収容し、ガスにより一方向から加圧して成形し、更に
ガスを流し続けて乾燥させる。この場合、次式で求めら
れるΔＰより高い圧力が加えられる。Next, the slip is accommodated in a pressure vessel having a filter, pressed and molded from one direction by a gas, and further dried by flowing a gas. In this case, a pressure higher than ΔP determined by the following equation is applied.
ΔＰ＝２γ/r （なお、γは表面張力、ｒは気孔半径である）。この場
合、使用するシリカ粉末の平均粒子径が大きくなればな
るほど、圧力ΔＰは小さくてよいという傾向を示す。前
述したようにシリカ粉末として平均粒子径１〜10μｍの
ものを用いた場合、圧力ΔＰはほぼ40〜3kgf/cm2の範囲
に設定される。例えば平均粒子径10μｍのシリカ粉末を
ゾルに混合し、0.2μｍ程度の気孔半径を有する多孔体
を得ようとする場合、混合割合、重縮合の程度でも変化
するが、３〜10kgf/cm2の圧力でろ過が可能で、しかも
成形時間は短い。ΔP = 2γ / r (where γ is the surface tension and r is the pore radius). In this case, the pressure ΔP tends to be smaller as the average particle size of the silica powder used increases. As described above, when silica powder having an average particle diameter of 1 to 10 μm is used, the pressure ΔP is set in a range of approximately 40 to 3 kgf / cm 2 . For example, when a silica powder having an average particle diameter of 10 μm is mixed with a sol to obtain a porous body having a pore radius of about 0.2 μm, the mixing ratio varies depending on the degree of polycondensation, but 3 to 10 kgf / cm 2 . Filtration is possible by pressure, and the molding time is short.
得られた成形体はゾル中の加水分解生成物がシリカ粉
末のバインダーとして作用しているので、強度が高く、
しかも気孔半径が比較的大きいので、乾燥時のキャピラ
リーストレスの影響が小さく、割れにくい。The resulting molded body has high strength because the hydrolysis product in the sol acts as a binder for silica powder,
In addition, since the pore radius is relatively large, the effect of capillary stress during drying is small, and cracking is unlikely.
以下、本発明を実施例に基づいて更に詳細に説明す
る。Hereinafter, the present invention will be described in more detail based on examples.
TEOS（テトラエトキシシラン）１モル、エタノール５
モル、H2O10モルを混合し、HClを添加してpH4のゾルを
調製した。このゾル40vol％と平均粒径10μｍのSiO2粉
末60vol％とを混合してスリップを調製した。1 mol of TEOS (tetraethoxysilane), ethanol 5
Mol, mixed H 2 O10 moles, to prepare a pH4 sol by the addition of HCl. A slip was prepared by mixing 40 vol% of this sol and 60 vol% of SiO 2 powder having an average particle size of 10 μm.
このスリップを第１図に示す圧力容器に収容した。第
１図において、パイレックス製のチャンバー１の底部に
はろ液の排出口2aを有するフィルター保持具２が設けら
れ、このフィルター保持具２には支持板３を介してフィ
ルター４が保持されている。このフィルター４は、平均
気孔半径２μｍ、見掛け気孔率20％のカーボン材からな
るものである。また、チャンバー１の上部にはスリップ
の注入口5aを有する蓋体５が設けられている。この蓋体
５と前記フィルター保持具２とはボルト６によって固定
されている。更に、蓋体５の注入口5aの上部にはガスケ
ット７を介してガス導入管８が取り付けられている。This slip was stored in the pressure vessel shown in FIG. In FIG. 1, a filter holder 2 having a filtrate outlet 2a is provided at the bottom of a Pyrex chamber 1, and a filter 4 is held in the filter holder 2 via a support plate 3. The filter 4 is made of a carbon material having an average pore radius of 2 μm and an apparent porosity of 20%. Further, a lid 5 having a slip inlet 5a is provided at the upper part of the chamber 1. The lid 5 and the filter holder 2 are fixed by bolts 6. Further, a gas inlet pipe 8 is attached to the upper portion of the inlet 5 a of the lid 5 via a gasket 7.
第１図の圧力容器にスリップ９を収容し、真空ポンプ
で充分脱気した後、上部より窒素ガスで加圧した。そし
て、3kgf/cm2の圧力がかかった時点でろ過され始め、4k
gf/cm2の圧力で１時間加圧することにより、厚さ10cmの
シリカ質多孔体10を成形した。更に、窒素ガスを流し続
けて乾燥することにより、割れのないシリカ質多孔体10
が得られた。The slip 9 was accommodated in the pressure vessel shown in FIG. 1 and sufficiently degassed by a vacuum pump, and then pressurized with nitrogen gas from above. Then, when pressure of 3 kgf / cm 2 was applied, filtration started, and 4 k
By pressurizing at a pressure of gf / cm 2 for 1 hour, a siliceous porous body 10 having a thickness of 10 cm was formed. Furthermore, by continuously flowing nitrogen gas and drying, a crack-free silica
was gotten.
得られたシリカ質多孔体を指で擦っても指に粒子が付
着することはなく、高強度を有していた。Even when the obtained porous silica material was rubbed with a finger, particles did not adhere to the finger and had high strength.
比較のために溶媒として水のみを用いてシリカ粉末を
成形し、100℃で乾燥した場合、息を吹きかけるだけで
粒子が飛散した。For comparison, when silica powder was formed using only water as a solvent and dried at 100 ° C., particles were scattered only by blowing.
以上詳述したように本発明方法によれば、使用するシ
リカ粉の粒子径で多孔体の気孔半径を調整することがで
き、気孔半径が0.2μｍ以上であれば10kgf/cm2以下の比
較的低圧で成形が可能であり、高価な圧力容器を必要と
せず、成形時間も短いので工業的に有利である。また、
得られる成形体は高強度で、しかも気孔半径が大きいの
で乾燥時にもキャピラリーストレスの影響を受けること
が少なく、割れにくい高純度のシリカ質多孔体を得るこ
とができる。As described in detail above, according to the method of the present invention, the pore radius of the porous body can be adjusted by the particle size of the silica powder to be used.If the pore radius is 0.2 μm or more, the pore radius is relatively 10 kgf / cm 2 or less. It is industrially advantageous because it can be molded at low pressure, does not require expensive pressure vessels, and has a short molding time. Also,
Since the obtained molded body has high strength and a large pore radius, it is less affected by capillary stress even during drying, and a high-purity silica-based porous body that is difficult to crack can be obtained.
第１図は本発明の実施例において用いられた圧力容器の
断面図である。 １…チャンバー、２…フィルター保持具、３…支持体、
４…フィルター、５…蓋体、６…ボルト、７…ガスケッ
ト、８…ガス導入管、９…スリップ、10…シリカ質多孔
体。FIG. 1 is a sectional view of a pressure vessel used in an embodiment of the present invention. 1 ... chamber, 2 ... filter holder, 3 ... support,
4 ... Filter, 5 ... Lid, 6 ... Bolt, 7 ... Gasket, 8 ... Gas inlet tube, 9 ... Slip, 10 ... Silica porous body.
フロントページの続き (72)発明者 阿部 一 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (56)参考文献 特開 昭63−166777（ＪＰ，Ａ) 実願 昭62−37230号（実開 昭63− 145852号）の願書に添付した明細書及び 図面の内容を撮影したマイクロフィルム （ＪＰ，Ｕ)Continuation of the front page (72) Inventor Kazu Abe 378, Oguni-machi, Oguni-machi, Nishiokitama-gun, Yamagata Pref. Microfilm (JP, U) photographing the contents of the specification and drawings attached to the application form No. 37230 (Japanese Utility Model Application No. Sho 63-145852)
Claims (1)
させたゾルと、平均粒子径が１〜10μｍのシリカ粉末と
を、該シリカ粉末が20〜60vol％となるように混合して
スリップを調製した後、該スリップをフィルターを有す
る圧力容器に収容し、ガスの圧力によって溶媒をろ過し
て成形し、さらにガスを流し続けて乾燥させることを特
徴とする高純度シリカ質多孔体の製造方法。1. A slip is prepared by mixing a sol obtained by partially hydrolyzing a metal alkoxysilane and a silica powder having an average particle diameter of 1 to 10 μm so that the silica powder becomes 20 to 60 vol%. After that, the slip is accommodated in a pressure vessel having a filter, the solvent is filtered by gas pressure, the solvent is formed, and the gas is further kept flowing to dry the method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63250460A JP2959770B2 (en) | 1988-10-04 | 1988-10-04 | Method for producing high-purity porous silica material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63250460A JP2959770B2 (en) | 1988-10-04 | 1988-10-04 | Method for producing high-purity porous silica material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0297471A JPH0297471A (en) | 1990-04-10 |
| JP2959770B2 true JP2959770B2 (en) | 1999-10-06 |
Family
ID=17208206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63250460A Expired - Fee Related JP2959770B2 (en) | 1988-10-04 | 1988-10-04 | Method for producing high-purity porous silica material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2959770B2 (en) |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH085729B2 (en) * | 1986-12-27 | 1996-01-24 | 新日本製鐵株式会社 | Method for manufacturing ceramic precursor compact |
| JPS63145852U (en) * | 1987-03-16 | 1988-09-27 |
-
1988
- 1988-10-04 JP JP63250460A patent/JP2959770B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0297471A (en) | 1990-04-10 |
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