JPH0388758A - Production of spherical ceramics particle - Google Patents

Production of spherical ceramics particle

Info

Publication number
JPH0388758A
JPH0388758A JP1225068A JP22506889A JPH0388758A JP H0388758 A JPH0388758 A JP H0388758A JP 1225068 A JP1225068 A JP 1225068A JP 22506889 A JP22506889 A JP 22506889A JP H0388758 A JPH0388758 A JP H0388758A
Authority
JP
Japan
Prior art keywords
particles
spherical
binder
density
ceramic particles
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
Application number
JP1225068A
Other languages
Japanese (ja)
Inventor
Hidetoshi Yamauchi
山内 英俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ibiden Co Ltd
Original Assignee
Ibiden Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ibiden Co Ltd filed Critical Ibiden Co Ltd
Priority to JP1225068A priority Critical patent/JPH0388758A/en
Publication of JPH0388758A publication Critical patent/JPH0388758A/en
Pending legal-status Critical Current

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  • Glanulating (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

PURPOSE:To easily obtain spherical ceramics particles which are high in molding density and have fine particle diameter at good mass-productivity at low cost by adding a binder to ceramics powder and treating the mixture while combining both a rolling granulating method and a rubber pressing method. CONSTITUTION:Ceramics powder (e.g. hydroxyapatite) and a binder (e.g. a mixed aq. soln. of polyethylene glycol and PVA) are introduced into a rotary cylinder 1. Then the rotary cylinder 1 is rotated in such a state that it is tilted and spherical ceramics particles are rolled and granulated. The rolled and granulated spherical ceramics particles 4 are introduced into a rubber mold 6 in which a plurality of cavities 7 are provided. Then the spherical ceramics particles are obtained by pressure-molding the ceramics particles 4 from the outside so that the particle diameter is regulated to <=5mm and molding density is regulated to 55% or more of theoretical density. The ceramics particles are preferably utilized for the fields of chemical industry, food processing and pharmaco-industry.

Description

【発明の詳細な説明】 [産業上の利用分野] この発明は化学工業、食品、医薬工業等に使用される球
状セラミックス粒子の製造方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing spherical ceramic particles used in the chemical industry, food industry, pharmaceutical industry, etc.

[従来の技術」 従来、球状セラξ・7クス粒子を製造する方法として、
転勤造粒法、ラバープレス法及びインジエクシッン成形
法等が知ら机でいる。
[Conventional technology] Conventionally, as a method for producing spherical Ceraξ/7X particles,
The transfer granulation method, rubber press method and in-die excine molding method are well known.

転勤造粒法は、6〜50″程度傾けた円筒内にセラミッ
クス粉体とバインダーを投入してその円筒を回転させる
ことにより、球状セラミックス粒子を転動成形する方法
である。
The rolling granulation method is a method in which ceramic powder and a binder are placed in a cylinder tilted by about 6 to 50 inches, and the cylinder is rotated to form spherical ceramic particles by rolling.

又、ラバープレス法は、セラミックス粉体をゴム型に入
れ、これを水圧室や加圧機等によって加圧成形する方法
である。
Further, the rubber press method is a method in which ceramic powder is placed in a rubber mold and then pressure-molded using a water pressure chamber, a pressure machine, or the like.

更に、インジェクション成形性は、セラミックス粉体に
バインダーとしての樹脂を加えた後、金型に射出して冷
却固化させる方法である。
Furthermore, injection moldability is a method in which a resin as a binder is added to ceramic powder, and then injected into a mold and cooled and solidified.

[発明が解決しようとする課題] ところが、前記転勤造粒法では、多量の球状セラミック
ス粒子を安価に製造できるものの、粒子の成形密度が理
論密度(TD)の45〜55%と低く、それを焼成した
場合に強度の良好な焼結体を得ることが難しいという問
題があった。
[Problems to be Solved by the Invention] However, although the transfer granulation method can produce a large amount of spherical ceramic particles at low cost, the compacted density of the particles is as low as 45 to 55% of the theoretical density (TD). There was a problem in that it was difficult to obtain a sintered body with good strength when fired.

又、前記ラバープレス法では13粒径が5mm以上の球
状セラミックス粒子については、高い成形密度の粒子を
得ることができるものの、粒径がl〜3mmの微小粒子
については、セラミックス粉体の充填が不十分となり、
成形密度の高い粒子を得ることができないという問題が
あった。
In addition, in the rubber press method, 13 particles with a high compaction density can be obtained for spherical ceramic particles with a particle size of 5 mm or more, but for small particles with a particle size of 1 to 3 mm, filling with ceramic powder is difficult. becomes insufficient,
There was a problem that particles with high compaction density could not be obtained.

更には、前記インジェクション成形法では、高い成形密
度で微小粒径の球状セラミックス粒子が得られるものの
、金型の費用が高くなったり、装置が大掛かりになった
り、面倒なバインダーの脱脂が必要となったりする等の
問題があった。
Furthermore, although the injection molding method allows spherical ceramic particles with a high molding density and a fine particle size to be obtained, the cost of the mold is high, the equipment is large-scale, and the troublesome degreasing of the binder is required. There were problems such as

この発明は前述した事情に鑑みてなされたものであって
、その目的は、成形密度の高い微小粒径の球状セラミッ
クス粒子を比較的簡易かつ安価に多量に製造することが
可能な球状セラミックス粒子の製造方法を提供すること
にある。
The present invention has been made in view of the above-mentioned circumstances, and its purpose is to produce spherical ceramic particles that can be manufactured in large quantities relatively easily and inexpensively with a high compaction density and a fine particle size. The purpose is to provide a manufacturing method.

[課題を解決するための手段] 上記の目的を達成するためにこの発明においては、回転
円筒内にセラミックス粉体及びバインダーを投入し、そ
の回転円筒を傾けた状態で回転させて球状セラミックス
粒子を転動成形した後、その転動成形された球状セラミ
ックス粒子をゴム型に入れ、その粒径が5mm以下で、
かつ成形密度が理論密度の55%以上となるように外部
から加圧成形している。
[Means for Solving the Problems] In order to achieve the above object, in the present invention, ceramic powder and a binder are put into a rotating cylinder, and the rotating cylinder is rotated in an inclined state to form spherical ceramic particles. After rolling, the rolling-molded spherical ceramic particles are placed in a rubber mold, and the particle size is 5 mm or less.
In addition, external pressure molding is performed so that the molding density is 55% or more of the theoretical density.

[作用コ 従って、回転円筒内にセラミックス粉体及びバインダー
を投入し、その回転円筒を傾けた状態で回転させること
により、成形密度が高まっていない多量の球状セラミッ
クス粒子が同時に転動成形される。そして、その転動成
形された球状セラミックス粒子をゴム型に入れ、その粒
径が5mm以下で、かつ成形密度が理論密度の55%以
上となるように外部から加圧することにより、各粒子が
圧縮されて所望の粒径及び成形密度よりなる球状セラミ
ックス粒子が得られる。
[Operations] Therefore, by putting ceramic powder and a binder into a rotating cylinder and rotating the rotating cylinder in an inclined state, a large amount of spherical ceramic particles whose compaction density has not been increased are rolled at the same time. Then, the rolling-molded spherical ceramic particles are placed in a rubber mold, and each particle is compressed by applying pressure from the outside so that the particle size is 5 mm or less and the molding density is 55% or more of the theoretical density. Then, spherical ceramic particles having a desired particle size and compaction density are obtained.

[実施例] 以下、この発明を具体化した一実施例を第1図〜第5図
に基いて詳細に説明する。
[Example] Hereinafter, an example embodying the present invention will be described in detail with reference to FIGS. 1 to 5.

第1図〜第5図はこの実施例における球状セラくフクス
粒子の製造方法における一連の製造工程を表している。
FIGS. 1 to 5 show a series of manufacturing steps in the method for manufacturing spherical cerafukusu particles in this example.

第1の工程として、先ず第1図に示すように、予め所定
角度θだけ傾けた状態で支持された回転円?#1内にセ
ラミックス粉体2及びバインダー3を投入し、次に第2
図に示すように、その回転円筒1を傾けた状態で回転さ
せる。
As the first step, as shown in FIG. Ceramic powder 2 and binder 3 are put into #1, then the second
As shown in the figure, the rotating cylinder 1 is rotated in an inclined state.

ここで、セラくツクス粉体2として、比表面積50m2
/gのハイドロキシアパタイトを20kg使用し、それ
に対するバインダー3として、有機バインダーである濃
度1%のポリエチレングリコール(PEG)を200g
及び濃度2%のポリビニルアルコール(PVA)を40
0g、水を1kgを使用する。
Here, as the Cerax powder 2, the specific surface area is 50 m2
/g of hydroxyapatite, and as binder 3, 200g of polyethylene glycol (PEG), an organic binder, with a concentration of 1%.
and 40% polyvinyl alcohol (PVA) at a concentration of 2%.
Use 0g and 1kg of water.

又、回転円筒1の傾は角度である所定角度θは51″で
あり、その回転数は13rpmであり、回転時間は12
分である。
Further, the predetermined angle θ, which is the angle at which the rotating cylinder 1 is inclined, is 51″, the rotation speed is 13 rpm, and the rotation time is 12
It's a minute.

前記第1の工程の結果、成形密度が高まっていない、粒
径1〜5mm程度のバラツキを有する1次底形物として
の球状セラミックス粒子4が同時に多量に転動成形され
る。
As a result of the first step, a large number of spherical ceramic particles 4 as primary bottom-shaped objects having a particle size variation of about 1 to 5 mm and whose compaction density is not increased are roll-formed in large quantities at the same time.

続いて、第2の工程として、第3図に示すように、粒径
1〜5mm程度のバラツキを有する球状セラミックス粒
子4を篩5にかける。
Subsequently, as a second step, as shown in FIG. 3, spherical ceramic particles 4 having particle diameters varying from about 1 to 5 mm are passed through a sieve 5.

この場合、先ず最初に2.4 m mメソシュの篩5に
かけて粒径2.4mm以下の小さい粒子を除去した後、
残った大きめの粒子を3.3mmメツシュの篩5にかけ
て粒径3.3 m mより大きい粒子を除去する。これ
によって、粒径2.4〜3.3mmの球状セラミックス
粒子4のみを得る。
In this case, first, after passing through a 2.4 mm mesh sieve 5 to remove small particles with a particle size of 2.4 mm or less,
The remaining larger particles are passed through a 3.3 mm mesh sieve 5 to remove particles larger than 3.3 mm in diameter. As a result, only spherical ceramic particles 4 having a particle size of 2.4 to 3.3 mm are obtained.

次に、第3の工程として、先ず第4図に示すように、第
2の工程において篩5にかけて得た2、4〜3.3mm
の球状セラミックス粒子4を、上下のゴム型6に入れて
型締めした後、第5図に示すように図示しない加圧機に
かけて外部から加圧する。
Next, in the third step, as shown in FIG.
After putting the spherical ceramic particles 4 into upper and lower rubber molds 6 and clamping the molds, as shown in FIG. 5, pressure is applied from the outside using a pressurizer (not shown).

即ち、乾式の加圧を行う。That is, dry pressurization is performed.

ここで、上下のゴム型6は内径4m、mのキャビティ7
を複数有するものであり、各キャビティ7に対して1個
の球状セラミックス粒子4を入れる。
Here, the upper and lower rubber molds 6 have an inner diameter of 4 m and a cavity 7 of m.
One spherical ceramic particle 4 is placed in each cavity 7.

又、加圧機にて加える圧力は1.5 ton / c 
m2である。即ち、粒径が5mm以下で、かつ成形密度
が理論密度の55%以上となるように設定されている。
Also, the pressure applied by the pressure machine is 1.5 ton/c
It is m2. That is, the particle size is set to be 5 mm or less, and the compacted density is set to be 55% or more of the theoretical density.

上記の第3の工程の結果、第2の工程までに得た成形密
度の高くない球状セラミックス粒子4が圧縮されて、粒
径2.2〜3.1で、成形密度が理論密度の58〜62
%の球状セラミックス粒子を得た。
As a result of the above-mentioned third step, the spherical ceramic particles 4 having a low compacted density obtained up to the second step are compressed to have a particle size of 2.2 to 3.1 and a compacted density of 58 to the theoretical density. 62
% of spherical ceramic particles were obtained.

以上のように、この実施例の製造方法によれば、粒径が
5mm以下で成形密度が理論密度の55%以上である、
高い成形密度の微小粒子を同時に多量に得るこεができ
る。しかも、この実施例の製造方法によれば、従来例の
インジヱクシッン成形法とは異なり、球状セラミックス
粒子を得るために、高価な金型や大掛かりな装置を必要
とせず、面倒なバインダーの脱脂を行う必要がなく、比
較的簡易で安価な製造を行うことができる。
As described above, according to the manufacturing method of this example, the particle size is 5 mm or less and the compacted density is 55% or more of the theoretical density.
It is possible to obtain a large amount of microparticles with high compaction density at the same time. Moreover, according to the manufacturing method of this example, unlike the conventional injection molding method, in order to obtain spherical ceramic particles, expensive molds and large-scale equipment are not required, and the troublesome degreasing of the binder is performed. It is not necessary and can be manufactured relatively easily and inexpensively.

尚、この発明は前記実施例に限定されるものではなく、
発明の趣旨を逸脱しない範囲において構成の一部を適宜
に変更して次のように実施することもできる。
Note that this invention is not limited to the above embodiments,
The present invention can be implemented as follows by changing a part of the structure as appropriate without departing from the spirit of the invention.

(1)前記実施例では、回転円筒1の傾は角度としての
所定角度θを51°、回転数を13rpm、回転時間を
12分としたが、所定角度θ、回転数及び回転時間を適
宜に変更してもよい。
(1) In the above embodiment, the rotation cylinder 1 was tilted at a predetermined angle θ of 51 degrees, a rotation speed of 13 rpm, and a rotation time of 12 minutes. May be changed.

(2)前記実施例では、バインダー3として有機バイン
ダーである、PEG及びPVAを使用したが、同じく有
機バインダーであるポリアクリル酸エステル(PAE)
を使用したり、無機バインダーを使用したり、それらを
適宜に組、み合わせて使用したりしてもよい。
(2) In the above examples, PEG and PVA, which are organic binders, were used as the binder 3, but polyacrylic ester (PAE), which is also an organic binder, was used.
, an inorganic binder, or an appropriate combination of these.

(3)前記実施例では、球状セラミックス粒子4をゴム
型6に入れて加圧機にて加圧する乾式の加圧を行ったが
、球状セラミックス粒子を入れたゴム型を水圧室にいれ
て加圧する湿式の加圧を行ってもよい。
(3) In the above embodiment, dry pressurization was performed in which the spherical ceramic particles 4 were placed in a rubber mold 6 and pressurized with a pressurizer, but the rubber mold containing the spherical ceramic particles was placed in a water pressure chamber and pressurized. Wet pressurization may also be performed.

(4)前記実施例では、第3図に示すように篩5にかけ
る第2の工程を実施したが、これを省略して第1の工程
と第3の工程のみを組み合わせて実施してもよい。
(4) In the above embodiment, the second step of passing through the sieve 5 was carried out as shown in FIG. good.

(5)前記実施例では、セラミックス粉体2としてハイ
ドロキシアパタイトを使用したが、他にアルミナ、ムラ
イト、シリカ、マグネシア、カルシア、コージェライト
、チタニア、炭化ケイ素、炭化ホウ素、炭化チタン、窒
化ケイ素、窒化アルミニウム、窒化ホウ素、窒化チタン
、サイアロン、ジルコニア、リン酸カルシウム、及びそ
れらの混合物から成る粉体を使用することもできる。特
に、平均粒径が1μm以下の微粉でカサ比重の小さい粉
体に適している。
(5) In the above example, hydroxyapatite was used as the ceramic powder 2, but other materials include alumina, mullite, silica, magnesia, calcia, cordierite, titania, silicon carbide, boron carbide, titanium carbide, silicon nitride, and nitride. Powders of aluminum, boron nitride, titanium nitride, sialon, zirconia, calcium phosphate, and mixtures thereof can also be used. In particular, it is suitable for fine powder with an average particle size of 1 μm or less and a small bulk specific gravity.

[発明の効果] 以上詳述したようにこの発明によれば、成形密度の高い
微小粒径の球状セラ雫フクス粒子を比較的簡易で安価に
多量に製造することができるという優れた効果を発揮す
る。
[Effects of the Invention] As detailed above, the present invention exhibits the excellent effect of being able to produce large quantities of spherical Sera Shizuku Fukusu particles with a high compaction density and a fine particle size relatively easily and inexpensively. do.

【図面の簡単な説明】[Brief explanation of drawings]

第1図〜第5図はこの発明を具体化した一実施例におけ
る一連の製造工程を表す図面であって、第1図及び第2
図は第1の工程を説明する図、第3図は第2の工程を説
明する図、第4図及び第5図は第3の工程を説明する図
である。 1・・・回転円筒、2・・・セラミックス粉体、3・・
・バインダー、4・・・球状セラミックス粒子、6・・
・ゴム型。
1 to 5 are drawings showing a series of manufacturing steps in an embodiment embodying the present invention, and FIGS.
The drawings are diagrams for explaining the first step, FIG. 3 is a diagram for explaining the second step, and FIGS. 4 and 5 are diagrams for explaining the third step. 1... Rotating cylinder, 2... Ceramic powder, 3...
・Binder, 4... Spherical ceramic particles, 6...
・Rubber type.

Claims (1)

【特許請求の範囲】[Claims] 1 回転円筒(1)内にセラミックス粉体(2)及びバ
インダー(3)を投入し、その回転円筒(1)を傾けた
状態で回転させて球状セラミックス粒子(4)を転動成
形した後、その転動成形された球状セラミックス粒子(
4)をゴム型(6)に入れ、その粒径が5mm以下で、
かつ成形密度が理論密度の55%以上となるように外部
から加圧成形する球状セラミックス粒子の製造方法。
1. Ceramic powder (2) and binder (3) are placed in a rotating cylinder (1), and the rotating cylinder (1) is rotated in an inclined state to form spherical ceramic particles (4) by rolling. The rolling-molded spherical ceramic particles (
4) into a rubber mold (6), and the particle size is 5 mm or less,
A method for producing spherical ceramic particles, which is externally pressure-molded so that the compacted density is 55% or more of the theoretical density.
JP1225068A 1989-08-31 1989-08-31 Production of spherical ceramics particle Pending JPH0388758A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1225068A JPH0388758A (en) 1989-08-31 1989-08-31 Production of spherical ceramics particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1225068A JPH0388758A (en) 1989-08-31 1989-08-31 Production of spherical ceramics particle

Publications (1)

Publication Number Publication Date
JPH0388758A true JPH0388758A (en) 1991-04-15

Family

ID=16823532

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1225068A Pending JPH0388758A (en) 1989-08-31 1989-08-31 Production of spherical ceramics particle

Country Status (1)

Country Link
JP (1) JPH0388758A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006090506A1 (en) * 2005-02-23 2006-08-31 Kikuo Sugita Turnover preventive sheet

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006090506A1 (en) * 2005-02-23 2006-08-31 Kikuo Sugita Turnover preventive sheet
GB2439855A (en) * 2005-02-23 2008-01-09 Kikuo Sugita Turnover preventive sheet
GB2439855B (en) * 2005-02-23 2009-09-16 Kikuo Sugita Turnover preventive sheet
US8182910B2 (en) 2005-02-23 2012-05-22 Kikuo Sugita Tip-resistant sheet for standing articles

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