JPS63210079A - Manufacture of ceramic porous body - Google Patents
Manufacture of ceramic porous bodyInfo
- Publication number
- JPS63210079A JPS63210079A JP62043741A JP4374187A JPS63210079A JP S63210079 A JPS63210079 A JP S63210079A JP 62043741 A JP62043741 A JP 62043741A JP 4374187 A JP4374187 A JP 4374187A JP S63210079 A JPS63210079 A JP S63210079A
- Authority
- JP
- Japan
- Prior art keywords
- porous body
- ceramic
- porous
- space
- manufacturing
- 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.)
- Granted
Links
- 239000000919 ceramic Substances 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000463 material Substances 0.000 claims description 37
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 9
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 7
- 229910000394 calcium triphosphate Inorganic materials 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- RFWLACFDYFIVMC-UHFFFAOYSA-D pentacalcium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O.[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O RFWLACFDYFIVMC-UHFFFAOYSA-D 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 239000002657 fibrous material Substances 0.000 claims 4
- 238000000034 method Methods 0.000 description 21
- 239000011148 porous material Substances 0.000 description 17
- 239000007943 implant Substances 0.000 description 14
- 239000011324 bead Substances 0.000 description 9
- 210000000988 bone and bone Anatomy 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 239000004793 Polystyrene Substances 0.000 description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 6
- 239000004926 polymethyl methacrylate Substances 0.000 description 6
- 229920002223 polystyrene Polymers 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000002612 dispersion medium Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000011505 plaster Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 235000002566 Capsicum Nutrition 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000006002 Pepper Substances 0.000 description 1
- 235000016761 Piper aduncum Nutrition 0.000 description 1
- 235000017804 Piper guineense Nutrition 0.000 description 1
- 244000203593 Piper nigrum Species 0.000 description 1
- 235000008184 Piper nigrum Nutrition 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔−産業上の利用分野〕
本発明はセラミック多孔体の製造方法に関するものであ
る。本発明により得られるセラミック多孔体は人工骨ま
たは骨補綴用のセラミックインブラント材、シ濾過材等
の用途に有用である。DETAILED DESCRIPTION OF THE INVENTION [-Industrial Application Field] The present invention relates to a method for manufacturing a ceramic porous body. The ceramic porous body obtained by the present invention is useful for applications such as ceramic implant materials for artificial bones or bone prostheses, and filtration materials.
セラミック多孔体は、生体適合性が良く機械的強度も比
較的大きいことから人工歯根、人工骨などの生体硬Ｍｉ
礒代替材料としてのセラミックインブラント材に使用さ
れてきている。Ceramic porous materials have good biocompatibility and relatively high mechanical strength, so they can be used as biological hard materials such as artificial tooth roots and artificial bones.
It has been used as a ceramic implant material as a substitute material for pepper.
孔径５０μ以□上の多孔体と骨を接触させると新生骨が
侵入する。他方、孔径の大きな多孔体は機械的強度が低
い。この問題を解決するための一方法として、特開昭４
９−１０９４０７号公報（引例１）には金属あるいは緻
密質セラミック物質と多孔性セラミック物質とから構成
される骨の補綴部材の製法が提案されている。この方法
は、一定寸法のセラミック物質の顆粒をその焼結温度以
下に加熱し、ついで少なくとも約１トン／ ｃｉｉの圧
力で圧縮して圧縮塊状物となし、さらに前記塊状物を焼
結することを特徴とするものであって、金属との組合せ
の場合は、塊状物で焼結したのち鋳型内に設置して金属
を鋳造することによって金属ロンドに固定され、セラミ
ック物質との組合せの場合は、焼結前の上記塊状物と、
別途製造した孔のないセラミック物質のための圧縮塊状
物とを一緒に圧縮したのち焼結することによって一体化
される。多孔体の孔の半径は１００〜２００ミクロンで
多孔度は３０％であると記載されている。他の方法とし
て実公昭５６−３４７３１号公報（引例２）には単結晶
アルミナの芯体の周囲に多孔質のアルミナセラミックを
固着せしめた骨内インブラント材が提案されている。When a porous body with a pore diameter of 50μ or more is brought into contact with bone, new bone invades. On the other hand, porous bodies with large pore diameters have low mechanical strength. As one way to solve this problem,
Publication No. 9-109407 (Reference 1) proposes a method for manufacturing a prosthetic bone member made of a metal or a dense ceramic material and a porous ceramic material. The method comprises heating granules of ceramic material of fixed size below its sintering temperature, then compressing them at a pressure of at least about 1 ton/cii into a compacted mass, and further sintering said mass. In the case of combination with metal, it is sintered in a lump and then placed in a mold and fixed to the metal iron by casting the metal, and in the case of combination with ceramic material, The above lump before sintering,
It is integrated by compacting the compacted mass for the non-porous ceramic material, produced separately, together and then sintering it. It is stated that the pore radius of the porous body is 100 to 200 microns and the porosity is 30%. As another method, Japanese Utility Model Publication No. 56-34731 (Reference 2) proposes an intraosseous implant material in which porous alumina ceramic is fixed around a single crystal alumina core.
この方法は、まずセラミック粉末と焼失性材料とが混合
され、圧粉成形、ののち焼成して多孔体を得る。つぎに
芯体であるアルミナ単結晶の外殻に上記多孔体を接着剤
を介して、あるいはねじどめにより固着する。多孔体の
口径は０．２〜０．ｌｌｌ１ｍ中であると記載されてい
る。In this method, first, ceramic powder and burnable material are mixed, compacted, and then fired to obtain a porous body. Next, the above-mentioned porous body is fixed to the outer shell of the alumina single crystal that is the core body through an adhesive or by screwing. The diameter of the porous body is 0.2 to 0. It is described as being in ll1m.
〔発明が解決しようとする問題点］
引例１においては、直径０．５〜１．５．ｍｍアルミナ
顆粒を焼結温度以下で加熱後、圧縮塊状物を焼結するこ
とで多孔体を得る方法であるので、直径が０．５〜１
、５＋ｍｓ＋のアルミナ顆粒が必要であること、アルミ
ナ顆粒の予備焼成を要すること、圧縮のために１〜４ト
ン／ｃｍｔ の圧力を要するので大型のものや複雑形状
のものに適用し難いことなどの問題点がある。引例２に
おいては、セラミック粉末と焼失性材料とが混合され、
圧粉成形ののち焼成して多孔体を得る方法であるので、
圧粉成形体の中の焼失性材料の位置を制御することがで
きず、従って焼成後の多孔体中の孔が独立気孔か連続気
孔か、また気孔の大きさあるいは方向を１１ＪＬ１ｔｌ
ｌすることができない。即ち、多孔体中の気孔の大きさ
・方向を制御ｎすることが可能で、特別な装置を要しな
い成形方法は解決すべき！！ｌ！題であった。[Problems to be solved by the invention] In Reference 1, the diameter is 0.5 to 1.5. This is a method to obtain a porous body by heating the alumina granules below the sintering temperature and then sintering the compressed lumps, so the diameter is 0.5 to 1 mm.
, 5+ms+ alumina granules are required, pre-calcination of the alumina granules is required, and pressure of 1 to 4 tons/cmt is required for compression, making it difficult to apply to large items or items with complex shapes. There is a problem. In Reference 2, ceramic powder and burnable material are mixed,
Since this is a method of obtaining a porous body by compacting and then firing,
It is not possible to control the position of the burnable material in the powder compact, and therefore it is difficult to determine whether the pores in the porous body after firing are independent or continuous, and the size or direction of the pores.
I can't do it. In other words, a molding method that can control the size and direction of pores in a porous body and that does not require special equipment should be developed! ! l! It was a question.
ｃ問題点を解決するための手段〕
本発明者らは、構造の制？１１された熱分解性物質多孔
体の空間部分にセラミック粉末の泥しようを満たした後
に焼成すれば、気孔の大きさおよび方向の制御されたセ
ラミック多孔体が得られるとの構想のもとにａ意検討を
重ねた結果、本発明の完成に至ったものである。Means for Solving the Problem c] The present inventors have developed a method for solving the problem of structure. Based on the idea that a ceramic porous body with controlled pore size and direction can be obtained by filling the voids of a porous body made of a pyrolyzable material with ceramic powder slurry and then firing it. As a result of repeated discussions, the present invention has been completed.
本発明は熱分解性物質からなり、隣接する構成単位が連
絡部分と空間とを共有する三次元連結構造である多孔体
の空間部分を、セラミック粉末の泥しようで満たした後
、加熱焼成することを特徴とするセラミック多孔成形体
の製造方法、さらには、熱分解性物質からなり、隣接す
る構成単位が連結部分と空間とを共有する三次元連結構
造である多孔体をセラミック基村上に接触または近接し
て配置し、該セラミック基材と同質のセラミック粉末の
泥しようでセラミック基材と多孔体間および多孔体の空
間部分を満たした後、加熱焼成することを特徴とする表
面にセラミック多孔体層を有するセラミック成形体の製
造方法を提供することにある。The present invention involves filling the space of a porous body made of a pyrolyzable material and having a three-dimensional connected structure in which adjacent structural units share a space with a connecting part with slurry of ceramic powder, and then heating and firing it. A method for producing a porous ceramic molded body, characterized in that the porous body is made of a pyrolyzable material and has a three-dimensional connected structure in which adjacent structural units share a connecting portion and a space, in contact with or on a ceramic base. A ceramic porous body having a surface that is arranged close to each other and filled with a slurry of ceramic powder of the same quality as the ceramic base material in the spaces between the ceramic base material and the porous body and in the porous body, and then heated and fired. An object of the present invention is to provide a method for manufacturing a ceramic molded body having layers.
以下本発明について詳述する。The present invention will be explained in detail below.
本発明において使用される熱分解性物質としては、セラ
ミックの焼結温度までに熱分解、燃焼または昇華して焼
失し、灰分を残さないものかまたは灰分が人体に無害な
ものであり、その例として合成樹脂、天然樹脂、パラフ
ィン、ワックスなどがある。The pyrolyzable substance used in the present invention is one that thermally decomposes, burns, or sublimates and burns out up to the sintering temperature of the ceramic and does not leave any ash, or one whose ash content is harmless to the human body. Examples include synthetic resins, natural resins, paraffin, and wax.
本発明における熱分解性物質多孔体は、隣接する構成単
位が連結部分と空間とを共有する三次元連結構造を存す
るもので、構成単位としては球状、粒状、多角形、繊維
状あるいはこれらの多少変形したものなどの形状を有す
るもので、隣接する構成単位が部分的に連結されて三次
元に連なり、かつ隣接する構成単位の間に空間が存在し
てこの空間が二次元に連なる構造を有する。連結の方法
は例えば融着、接着など通常の方法でよい、連結の程度
は、用途により異なるので目的とする多孔体の平均孔径
、空孔率等を考慮して適宜きめることができ、通常厚み
方向は１〜１５Ｎの範囲であるがこれに限定されるもの
ではない。The porous body of a thermally decomposable material in the present invention has a three-dimensional connected structure in which adjacent constituent units share a connecting part and space, and the constituent units may be spherical, granular, polygonal, fibrous, or some of these. It has a deformed shape, etc., and has a structure in which adjacent structural units are partially connected and connected in three dimensions, and there is a space between adjacent structural units, and this space is connected in two dimensions. . The connection method may be any conventional method such as fusion or adhesion.The degree of connection varies depending on the purpose, so it can be determined as appropriate by considering the average pore diameter, porosity, etc. of the intended porous body. The direction is in the range of 1 to 15N, but is not limited thereto.
特にインブラント材として使用する場合は、インブラン
トの大きさに依存するが、厚み方向は１〜３層が好まし
く、”これより多層になると奥の方まで清掃・滅菌する
のが困難になる。構成単位の大きさはセラミック多孔体
としての気孔の大きさによって決まるが通常０．Ｏ１〜
２．５ｍｍ程度、好ましくは０．０５〜１ 、５ｍｍ程
度である。特にインブラント材として使用する場合は、
０．０５〜１ 、５＋＋＋＋程度、連結部分の大きさは
通常０．０１＝ ０．５ｍｍが好ましい。Particularly when used as an implant material, it is preferable to have 1 to 3 layers in the thickness direction, although it depends on the size of the implant; if the layer is more than this, it becomes difficult to clean and sterilize deep inside. The size of the structural unit is determined by the size of the pores in the ceramic porous body, but is usually 0.01~
It is about 2.5 mm, preferably about 0.05 to 1.5 mm. Especially when used as an implant material,
0.05 to 1.5++++ or so, and the size of the connecting portion is usually preferably 0.01=0.5 mm.
インブラント材の場合、これらの大きさは、造管細胞の
侵入しうる大きさによって下限が定まり、また余りに大
きいと強度が低下するので上限が定まる。多孔体の形状
は、平板、円筒、半球状など目的に応じて適宜法めるこ
とができる。In the case of an implant material, the lower limit of these sizes is determined by the size that the duct-forming cells can invade, and the upper limit is determined because if the size is too large, the strength will decrease. The shape of the porous body can be determined as appropriate depending on the purpose, such as a flat plate, a cylinder, or a hemisphere.
本発明の他の態様として表面に多孔体の層を有するセラ
ミック成形体を製造する場合はセラミック基材を使用す
る。該セラミック基材としては、アルミナ、ジルコニア
、三燐酸カルシウム、ヒドロキシアパタイト、窒化ケイ
素、炭化ケイ素等、周知のセラミックが使用できるが、
インブラントとじて使用する場合はアルミナ、ジルコニ
ア、三燐酸カルシウムまたはヒドロキシアパタイトが好
ましく、所望のインブラントの形状に成形されたもの、
または成形後に焼成された焼結体である。In another embodiment of the present invention, a ceramic base material is used when producing a ceramic molded body having a porous layer on its surface. As the ceramic base material, well-known ceramics such as alumina, zirconia, calcium triphosphate, hydroxyapatite, silicon nitride, and silicon carbide can be used.
When used as an implant, alumina, zirconia, calcium triphosphate or hydroxyapatite are preferred, and are molded into the desired shape of the implant.
Or it is a sintered body that is fired after molding.
セラミック粉末の泥しようはセラミック粉末、バインダ
ーおよび分散媒からなる泥しようである。Ceramic powder slurry is a slurry consisting of ceramic powder, binder and dispersion medium.
セラミック原料粉体としてはアルミナ、ジルコニア、三
燐酸カルシウム、ヒドロキシアパタイト、窒化ケイ素、
炭化ケイ素等、周知のセラミック粉体が使用できるが、
インブラントとして使用する場合はアルミナ、ジルコニ
ア、三燐酸カルシウムおよびヒドロキシアパタイトが生
体に対する為害性がないので好ましい。Ceramic raw material powders include alumina, zirconia, calcium triphosphate, hydroxyapatite, silicon nitride,
Well-known ceramic powders such as silicon carbide can be used, but
When used as an implant, alumina, zirconia, calcium triphosphate and hydroxyapatite are preferred since they are not harmful to living organisms.
セラミック原料粉体の粒径は５μ以下好ましくは１μ以
下のものである。粒径が小さいほど焼結性にすぐれ、か
つ泥しようの安定性が良いので好ましい。バ・イングー
および分散媒は、溶解により溶液となる組合せによって
選択し、当業者の周知のもあが使用できる。その例とし
て、分散媒が水の場合はポリビニルアルコール、ポリエ
チレンオキシド、ヒドロキシエチルセルロースなどがあ
り、非水溶媒の場合はポリビニルブチラール、ポリメチ
ルメタクリレート、セルロースアセテートブチレートな
どがある。泥しようの調製法は周知の方法が採用でき、
バインダーの溶液にセラミック粉体を混合してよく分散
させて調製する。バインダーおよびセラミック粉体の濃
度は泥しようの粘度を支配する重要な因子である。The particle size of the ceramic raw material powder is 5 μm or less, preferably 1 μm or less. The smaller the particle size, the better the sinterability and the better the stability of the slurry, which is preferable. The base material and the dispersion medium are selected depending on the combination that results in a solution upon dissolution, and methods well known to those skilled in the art can be used. Examples thereof include polyvinyl alcohol, polyethylene oxide, hydroxyethyl cellulose, etc. when the dispersion medium is water, and polyvinyl butyral, polymethyl methacrylate, cellulose acetate butyrate, etc. when the dispersion medium is a non-aqueous solvent. Well-known methods can be used to prepare the slurry.
It is prepared by mixing ceramic powder into a binder solution and dispersing it well. The concentration of binder and ceramic powder are important factors governing the viscosity of the slurry.
泥しようの粘度は前述の三次元連結構造である多孔体の
空間部分にセラミック粉末の泥しょうが浸透しつる程度
のものであって、前述の構成単位の大きさ、連結部分の
大きさを考慮して５〜１０００センチボイズ程度の範囲
で適宜法めればよい。The viscosity of the slurry is such that the slurry of ceramic powder penetrates into the space of the porous body which is the three-dimensional connected structure mentioned above, and the viscosity is such that the slurry of ceramic powder can penetrate into the space of the porous body which is the above-mentioned three-dimensional connected structure. It may be adjusted appropriately within the range of about 5 to 1000 centiboise.
セラミック粉体濃度は１５〜６０重■χが望ましく、バ
インダー濃度は重！！ｔ２〜２０％（セラミックに対し
て）が望ましいが、両者の組合せによっ−で粘度が決ま
るので上記の濃度に限定されるものではない。The ceramic powder concentration is preferably 15 to 60 weight■χ, and the binder concentration is heavy! ! Although t2 to 20% (based on ceramic) is desirable, the viscosity is determined by the combination of the two, so it is not limited to the above concentration.
セラミック多孔体の製造については周知の成形技術によ
り製造することができる。例えば、熱分解性物質多孔体
を型枠の中のおき、これにセラミック粉末の泥しようを
注入した後、乾燥して成形体を得、または鋳込み成形法
により成形体を得、これを周知の方法で加熱して脱バイ
ンダーおよび焼結をさせる。The ceramic porous body can be manufactured using a well-known molding technique. For example, a porous body of a pyrolyzable material is placed in a mold, a slurry of ceramic powder is injected into it, and then dried to obtain a molded body, or a molded body is obtained by a cast molding method, which is then processed using the well-known method. Debinding and sintering are performed by heating in a method.
この場合は多孔体の成形体が得られるが、別の態様によ
りセラミック基材と多孔体が強固に結合した成形体を得
ることができる。In this case, a porous body molded body is obtained, but in another embodiment, a molded body in which the ceramic base material and the porous body are firmly bonded can be obtained.
インブラントとして使用する場合は強度の点からこのよ
うな構造のものが好ましい。When used as an implant, such a structure is preferred from the viewpoint of strength.
その場合は熱分解性物質多孔体とセラミック基材とを接
触させるか少し離して配置し、セラミック基材と同質の
セラミック粉末の泥しようで多孔体とセラミック基材の
間および多孔体の空間部分を満たした後、乾燥して成形
体を得る。あるいは鋳込み成形法によって表面に凹部を
有する成形体を得、この四部に多孔体を入れてさらに鋳
込むことにより一体化させ、乾燥後脱枠する。得られた
成形体を周知の方法で加熱して脱バインダーおよび焼成
する。In that case, the porous body of the pyrolyzable material and the ceramic base material should be brought into contact with each other or placed a little apart, and the space between the porous body and the ceramic base material and the space between the porous body and the porous body should be covered with a slurry of ceramic powder of the same quality as the ceramic base material. After filling, a molded body is obtained by drying. Alternatively, a molded body having concave portions on the surface is obtained by a cast molding method, a porous body is placed in the four parts, and the molded body is further integrated by casting, and the molded body is removed from the frame after drying. The obtained molded body is heated to remove the binder and to be fired by a well-known method.
構造の制御された熱分解性物質多孔体の空間部分にセラ
ミック粉末の泥しようを満たしたのち焼成することによ
って、′熱分解性物質を焼失させて気孔の大きさおよび
方向の制御されたセラミック多孔体が得られる。A pyrolyzable material with a controlled structure By filling the voids of a porous body with ceramic powder slurry and firing it, the pyrolyzable material is burned out and the ceramic pores with a controlled pore size and direction are created. You get a body.
本発明の方法によれば、気孔の大きさおよび方向の制御
されたセラミック多孔体およびセラミック多孔構造を表
面に有するセラミック成形体が特殊な装置を用いずに容
易に製造できる。According to the method of the present invention, a ceramic porous body in which the size and direction of pores are controlled and a ceramic molded body having a ceramic porous structure on the surface can be easily produced without using special equipment.
このセラミック成形体はインブラント材、３濾過材等に
使用することができる。This ceramic molded body can be used as an implant material, a 3-filter material, etc.
特にインブラント材として用いた場合、該インブラント
材は埋入後に多孔構造に新生骨が侵入し、インターロッ
キング効果によって骨との固着性に優れる。また多孔構
造の強度が高く、かつ滅菌または清掃の点でも著しく改
善されたものである。Particularly when used as an implant material, new bone invades the porous structure of the implant material after implantation, resulting in excellent adhesion to bone due to the interlocking effect. In addition, the porous structure has high strength and is significantly improved in terms of sterilization and cleaning.
以下本発明の一例を実施例により説明する。なお、実施
例において゛部゛は重量部である。An example of the present invention will be explained below using Examples. In the examples, "parts" are parts by weight.
実施例 １
直径３５ｖｍの１ 、０００メツシユの金網に直径０．
５ｎ＋ｍのポリスチレンビーズ（住人化学工業ｅ助製、
ニスブライト０ビーズＴ−８Ｋ ” ）を堆積層数が３
層となるよう□に注入した。これにメチルエチルケトン
とエタノールの混合溶剤（容積比７：３）を堆積層をく
ずさないように注入し、直ちに吸引シ戸遇した。この操
作を２回くり返した。自然乾燥後、グラスフィルターか
らとり出したポリスチレンビーズはビーズ間が接着され
て全体がブロック状に連結され、かつビーズ間に空間も
存在する多孔体であり、寸法は直径３２１１ｓ＋厚さ７
■であった。板状パラフィンで直径３２ｍｍ深さ１５ｎ
＋ｍ厚さ１５ｍ５の石膏型の中に上記ポリスチレン多孔
体をおき、これに次の組成のアルミナ泥しようを鋳込み
成形した。Example 1 A wire mesh of 1,000 mesh with a diameter of 35 vm was coated with a wire mesh having a diameter of 0.
5n+m polystyrene beads (manufactured by Susumu Kagaku Kogyo e-suke,
The number of deposited layers is 3.
Injected into □ so as to form a layer. A mixed solvent of methyl ethyl ketone and ethanol (volume ratio 7:3) was injected into the solution without destroying the deposited layer, and the solution was immediately placed under suction. This operation was repeated twice. After air-drying, the polystyrene beads taken out from the glass filter are porous, with the beads being glued together and connected as a block, with spaces between the beads, and the dimensions are 3211s in diameter + 7 in thickness.
■It was. Paraffin sheet with a diameter of 32 mm and a depth of 15 nm.
The polystyrene porous body was placed in a plaster mold having a thickness of 15 m, and an alumina slurry having the following composition was cast into the mold.
アルミナ（住友化学工業■製、
ＡＫＰ−２０、粒径０．６μ） １００部ポリビニ
ールアルコール（重合ｊｌＪ ５００） ２部Ｍｇ（
Ｎｏｉ）ｉ・６１１２０ ０．
３部水
６７部乾燥後脱枠し、５００℃に加熱
してポリスチレンを熱分解したのち、１６００°Ｃ１時
間加熱してアルミナを焼結させた。得られたアルミナ多
孔体は直径約０．４ｍｓ＋の球状空孔を有し、更に空孔
間を連結する直径０．０４〜０．０６５ｍ空孔を有する
ものであった。Alumina (manufactured by Sumitomo Chemical ■, AKP-20, particle size 0.6μ) 100 parts Polyvinyl alcohol (polymerization jlJ 500) 2 parts Mg (
Noi) i・61120 0.
3 parts water
After drying 67 parts, the frame was removed, heated to 500°C to thermally decompose the polystyrene, and then heated to 1600°C for 1 hour to sinter the alumina. The obtained alumina porous body had spherical pores with a diameter of approximately 0.4 ms+, and further had pores with a diameter of 0.04 to 0.065 m connecting the pores.
実施例 ２
ガラス平板で５０ｓｖ＋ Ｘ ５０ｓ＋＋ｅ Ｘ深さ１
０ｍ＋ｗの型枠をつくり、底板上に紙を敷き、この中に
直径０．３ｍｍのポリメチルメタアクリレートビーズ（
住友化学工業■製スミペックス＠−０１１）を堆積層が
３層となるように注入した。これに、ポリメチルメタア
クリレートの１０％クロロホルム溶液を上層のビーズが
一様に濡れる程度に注入し、自然乾燥した。Example 2 Glass flat plate 50sv+ x 50s++e x depth 1
Make a formwork of 0 m + w, spread paper on the bottom plate, and place polymethyl methacrylate beads (0.3 mm in diameter) in it.
Sumipex@-011) manufactured by Sumitomo Chemical Co., Ltd. was injected so that there were three deposited layers. A 10% chloroform solution of polymethyl methacrylate was poured into this to an extent that the beads in the upper layer were evenly wetted, and the mixture was air-dried.
脱枠後のポリメチルメタアクリレートビーズはビーズ間
が接着されて全体がブロック状に連結され、かつビーズ
間に空間も存在する多孔体であり、寸法は５０＃ｌｌｌ
×５０１１ＩＩＩ×厚さ １１であった。板状パラフィ
ンで５０ｍｍ Ｘ ５（ｌａ＋ｍ Ｘ深さｌ０ｎ−の石
膏型の中に上記ポリメチルメタアクリレート多孔体をお
き、これに次の組成のヒドロキシアパタイト泥しようを
鋳込み成形した。After removing the frame, the polymethyl methacrylate beads are porous, with the beads being glued together and connected in the form of a block, and there are also spaces between the beads, and the size is 50#lll.
×5011III×thickness 11. The polymethyl methacrylate porous body was placed in a plaster mold of 50 mm x 5 (la+m x depth 10 n-) made of paraffin plate, and hydroxyapatite slurry having the following composition was cast into the mold.
ヒドロキシアパタイト
（粒径０．０５〜２ ｔｔ 、Ｃａ／ｐ＝１．（３７）
１００部ポリビニルアルコール（重合度約５００）
２部水
６７部乾燥後脱枠し、３５０′
Ｃに加熱してポリメチルメタアクリレートを熱分解した
のち、１１００°Ｃ１時間加熱してアルミナを焼結させ
た。得られたヒドロキシアパタイト多孔体は直径０．２
５ｍｍの球状空孔を有し、更に空孔間を連結する直径０
．０３〜０．０５ｍｍの空孔を有するものであった。Hydroxyapatite (particle size 0.05-2 tt, Ca/p=1.(37)
100 parts polyvinyl alcohol (degree of polymerization approximately 500)
2 parts water
After drying, 67 parts were removed from the frame, and 350'
After heating at 1100° C. to thermally decompose polymethyl methacrylate, the alumina was sintered by heating at 1100° C. for 1 hour. The obtained hydroxyapatite porous body has a diameter of 0.2
It has a spherical hole of 5 mm, and a diameter of 0 connecting the holes.
．． It had pores of 0.03 to 0.05 mm.
実施例 ３
寸法５０Ｉｌ１１１×７０１１ＩＩ１１×深さ５１×厚
み１５＋ａｍの石膏型に実施例１のアルミナ泥しようを
鋳込み、中央に寸法３０ｍｍ Ｘ ５０ｍｍ Ｘ深さ２
ＩＩＩＩ１１の凹部を有する成形体を得た。この四部に
、直径ｌｌｌｌ１１のポリスチレンを実施例Ｉの方法で
処理して得た寸法３０ａ＋ｍ Ｘ ５０ｍｍ Ｘ厚さ２
ｍＬａのポリスチレン多孔体をおき、これに実施例１と
同様にアルミナ泥しようを鋳込んだ、乾燥後脱枠し、加
熱処理を行った。アルミナ繊密焼結体の表面にアルミナ
多孔体が形成された。Example 3 The alumina plaster of Example 1 was cast into a plaster mold with dimensions of 50Il111 x 7011II11 x depth 51 x thickness 15+am, and the dimensions 30mm x 50mm x depth 2 were placed in the center.
A molded article having III11 concavities was obtained. For these four parts, a piece of polystyrene with a diameter of lllll11 was treated by the method of Example I, and the dimensions were 30a+m x 50mm x thickness 2.
A polystyrene porous body of mLa was placed, and alumina slurry was cast therein in the same manner as in Example 1. After drying, the frame was removed and heat treatment was performed. An alumina porous body was formed on the surface of the alumina dense sintered body.
Claims (8)
部分と空間とを共有する三次元連結構造である多孔体の
空間部分を、セラミック粉末の泥しょうで満たしたのち
、加熱焼成することを特徴とするセラミツク多孔体の製
造方法。(1) Filling the space of a porous body made of a pyrolyzable material and having a three-dimensional connected structure in which adjacent structural units share a space with a connection part with slurry of ceramic powder, and then heating and firing it. A method for producing a ceramic porous body characterized by:
三次元連結構造体である特許請求の範囲第１項記載の製
造方法。(2) The manufacturing method according to claim 1, wherein the porous body is a three-dimensional connected structure of spherical, granular and/or fibrous materials.
状および／または繊維状物質の三次元連結構造体である
特許請求の範囲第２項記載の製造方法。(3) The manufacturing method according to claim 2, wherein the porous body is a three-dimensional connected structure of spherical, granular and/or fibrous materials with a diameter of 50 to 1500 microns.
シウムまたはヒドロキシアパタイトである特許請求の範
囲第１、２または３項記載の製造方法。(4) The manufacturing method according to claim 1, 2 or 3, wherein the ceramic is alumina, zirconia, calcium triphosphate or hydroxyapatite.
部分と空間とを共有する三次元連結構造である多孔体と
セラミック基材を接触または近接して配置し、該セラミ
ック基材と同質のセラミック粉末の泥しょうでセラミッ
ク基材と多孔体間および多孔体の空間部分を満たしたの
ち、加熱焼成することを特徴とするセラミック多孔体の
製造方法。(5) A porous body made of a thermally decomposable substance and having a three-dimensional connected structure in which adjacent structural units share a connecting part and space is placed in contact with or in close proximity to a ceramic base material, and is of the same quality as the ceramic base material. A method for producing a porous ceramic body, which comprises filling the space between the ceramic base material and the porous body and the space in the porous body with slurry of ceramic powder, and then heating and firing the mixture.
三次元連結構造体である特許請求の範囲第５項記載の製
造方法。(6) The manufacturing method according to claim 5, wherein the porous body is a three-dimensional connected structure of spherical, granular and/or fibrous materials.
状および／または繊維状物質の三次元連結構造体である
特許請求の範囲第６項記載の製造方法。(7) The manufacturing method according to claim 6, wherein the porous body is a three-dimensional connected structure of spherical, granular and/or fibrous materials with a diameter of 50 to 1500 microns.
シウムまたはヒドロキシアパタイトである特許請求の範
囲第５、６または７項記載の製造方法。(8) The manufacturing method according to claim 5, 6 or 7, wherein the ceramic is alumina, zirconia, calcium triphosphate or hydroxyapatite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62043741A JP2759147B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing porous ceramic body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62043741A JP2759147B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing porous ceramic body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63210079A true JPS63210079A (en) | 1988-08-31 |
| JP2759147B2 JP2759147B2 (en) | 1998-05-28 |
Family
ID=12672193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62043741A Expired - Fee Related JP2759147B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing porous ceramic body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2759147B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02116684A (en) * | 1988-10-21 | 1990-05-01 | Permelec Electrode Ltd | Production of porous body of calcium phosphate compound |
| JPH03228883A (en) * | 1990-01-31 | 1991-10-09 | Murata Mfg Co Ltd | Porous lightweight tool material and its production |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100536938C (en) * | 2007-02-06 | 2009-09-09 | 西北工业大学 | Process for preparing porous biological ceramics supporting frame |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS49109407A (en) * | 1973-01-18 | 1974-10-17 | ||
| JPS5075608A (en) * | 1973-11-07 | 1975-06-20 | ||
| JPS5634731U (en) * | 1979-08-24 | 1981-04-04 | ||
| JPS61127678A (en) * | 1984-11-21 | 1986-06-14 | 株式会社ブリヂストン | Manufacture of ceramic porous body |
| JPS61141682A (en) * | 1984-12-12 | 1986-06-28 | 東芝セラミツクス株式会社 | Ceramic foam and manufacture |
| JPS62202880A (en) * | 1986-02-28 | 1987-09-07 | 京セラ株式会社 | Manufacture of porous ceramic body |
-
1987
- 1987-02-25 JP JP62043741A patent/JP2759147B2/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS49109407A (en) * | 1973-01-18 | 1974-10-17 | ||
| JPS5075608A (en) * | 1973-11-07 | 1975-06-20 | ||
| JPS5634731U (en) * | 1979-08-24 | 1981-04-04 | ||
| JPS61127678A (en) * | 1984-11-21 | 1986-06-14 | 株式会社ブリヂストン | Manufacture of ceramic porous body |
| JPS61141682A (en) * | 1984-12-12 | 1986-06-28 | 東芝セラミツクス株式会社 | Ceramic foam and manufacture |
| JPS62202880A (en) * | 1986-02-28 | 1987-09-07 | 京セラ株式会社 | Manufacture of porous ceramic body |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02116684A (en) * | 1988-10-21 | 1990-05-01 | Permelec Electrode Ltd | Production of porous body of calcium phosphate compound |
| JPH03228883A (en) * | 1990-01-31 | 1991-10-09 | Murata Mfg Co Ltd | Porous lightweight tool material and its production |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2759147B2 (en) | 1998-05-28 |
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