JPS6364954A - Manufacture of porous ceramic sintered body - Google Patents
Manufacture of porous ceramic sintered bodyInfo
- Publication number
- JPS6364954A JPS6364954A JP61207288A JP20728886A JPS6364954A JP S6364954 A JPS6364954 A JP S6364954A JP 61207288 A JP61207288 A JP 61207288A JP 20728886 A JP20728886 A JP 20728886A JP S6364954 A JPS6364954 A JP S6364954A
- Authority
- JP
- Japan
- Prior art keywords
- hydroxyapatite
- sintered body
- inorganic substance
- porous
- ceramic sintered
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000919 ceramic Substances 0.000 title claims description 6
- 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 37
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 36
- 239000000126 substance Substances 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 210000000988 bone and bone Anatomy 0.000 description 3
- 239000012620 biological material Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 206010008631 Cholera Diseases 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
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) [Abstract] 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、多孔質ヒドロキシアパタイト焼結体ｏｔｍ造
方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing a porous hydroxyapatite sintered body (OTM).
多孔質ヒドロキシアパタイト焼結体は１人工骨などの生
体材料用として有望視されてお）、通常発泡法によ〕多
孔化された成形体を焼成することＫよ〕製造されてきた
。Porous hydroxyapatite sintered bodies are considered promising as biomaterials such as artificial bones, and have been produced by firing a porous molded body, usually by a foaming method.
しかし、発泡操作が煩雑であるため、多孔質口
ヒドロ中シアパタイト焼結体の製造！困難であった。そ
のため１人工骨などの主体材料用に使用し得る多孔質ヒ
ドロキシアパタイト焼結体を製造し得る新規な方法が望
まれていた。However, since the foaming operation is complicated, it is difficult to produce porous siapatite sintered bodies! It was difficult. Therefore, there has been a need for a new method for producing porous hydroxyapatite sintered bodies that can be used as main materials such as artificial bones.
本発明者等は上記の点に鑑み種々検討した結果、意外に
も、特定の性質を有する無機化合物を混合することによ
って、極めて容ＡＫ多孔質な焼結体が得られることを知
得して本発明に到達した。As a result of various studies in view of the above points, the inventors of the present invention have surprisingly found that by mixing inorganic compounds with specific properties, an extremely porous sintered body can be obtained. We have arrived at the present invention.
すなわち１本発明の要旨は、ヒドロキシアパタイトの粉
末と他の無機物質を、ヒドロキシアパタイトに対する他
の無機物質の重量比が０．００ ／以上で７以下の割合
で混合して成形し焼成することによシ、ヒドロキシアパ
タイトを主成分とする多孔質セラミックスｍ結体を製造
する方法であって、前記無機物１Ｍは、焼結温度以下で
ヒドロキシアパタイトと反応し、その結果生成する反応
生成物が焼結時の温度ではガラス相を形成しない化合物
となり得る無機物質であることを特徴とする多孔質セラ
ミックス焼結体の製造方法に存する。That is, the gist of the present invention is to mix hydroxyapatite powder and other inorganic substances in a weight ratio of hydroxyapatite to other inorganic substances of 0.00/or more and 7 or less, and then mold and fire the mixture. In this method, the inorganic substance 1M reacts with hydroxyapatite at a temperature below the sintering temperature, and the resulting reaction product is sintered. The present invention relates to a method for producing a porous ceramic sintered body characterized by being an inorganic substance that can become a compound that does not form a glass phase at a temperature of
以下、本発明の詳細な説明する罠１本発明で使用するヒ
ドロキシアパタイトとしては。Hereinafter, the present invention will be explained in detail.1 The hydroxyapatite used in the present invention is as follows.
’ ａｇｏ （Ｐ口４ ）＠ （ＯＢ）１の化学式で示
されるヒドロキシアパタイトであって％ １３１０℃以
下で分解せずに緻密に焼結する物質が用いられる。Hydroxyapatite represented by the chemical formula 'ago (P mouth 4) @ (OB) 1 and which is sintered densely without decomposing at temperatures below 1310° C. is used.
池の無機物質としては、ヒドロキシアパタイトの焼結温
度以下でヒドロキシアパタイトと反応し、その結果生成
する反応生成物が焼結時の温度ではガラス相を形成しな
い化合物とな）得る無機物質であればいずれでも用いる
ことができる。具体的には、アル之す、シリカ、ジルコ
ニア、チタニアが例として挙げられる。ヒドロキシアパ
タイトと反応しない物質を用いると。The inorganic substance in the pond is an inorganic substance that reacts with hydroxyapatite at a temperature below the sintering temperature of hydroxyapatite, and the resulting reaction product is a compound that does not form a glass phase at the sintering temperature. Either can be used. Specifically, examples include aluminum, silica, zirconia, and titania. When using a substance that does not react with hydroxyapatite.
ヒドロキシアパタイトが多孔化せずに緻密化しそしまう
。また、ヒドロキシアパタイトと反応した結果生成する
反応生成物が焼結時の温度でガラス相を形成するとヒド
ロキシアパタイトが緻密に焼結してしまう。Hydroxyapatite fails to become densified without becoming porous. Furthermore, if a reaction product produced as a result of the reaction with hydroxyapatite forms a glass phase at the sintering temperature, the hydroxyapatite will be densely sintered.
コレラのヒドロキシアパタイトと他の無機物質は通常粉
体として用い、その粒径は１０３ｍ以下、特には７μｍ
以下が好ましい。Cholera hydroxyapatite and other inorganic substances are usually used as a powder, with a particle size of less than 103 m, especially 7 μm.
The following are preferred.
ヒドロキシアパタイトと他の無機物ＭＯ混合割合は、ヒ
ドロキシアパタイトに対する他の無機物質のＭ量比が０
．００ ／以上、特には０．０７以上で、／以下とする
が、この無機物質が少なすぎると多孔化が難しく、多す
ぎるとヒドロキシアパタイトの特徴を生かすことが困難
となる。The mixing ratio of hydroxyapatite and other inorganic substances is such that the M amount ratio of other inorganic substances to hydroxyapatite is 0.
．． The content of the inorganic substance is preferably 0.00 or more, particularly 0.07 or more and / or less, but if the amount of this inorganic substance is too small, it will be difficult to create porosity, and if it is too large, it will be difficult to take advantage of the characteristics of hydroxyapatite.
ヒドロキシアパタイトと他の無機物質Ｏ混合方法として
は１通常のセラミックス粉体Ｏ混合方法が用いられる。As a method for mixing hydroxyapatite and other inorganic substances, a conventional method for mixing ceramic powder O is used.
乾式混合でも湿式混合でも良いが、よシ均一に混合する
ためにアルコール等の有機溶媒、又はポリビニルアルコ
ール、ポリアクリル製糸のバインダーを含有する水溶液
等管用いた湿式混合を行なうヒとが好ましい。Dry mixing or wet mixing may be used, but wet mixing using a tube containing an organic solvent such as alcohol, or an aqueous solution containing a binder for polyvinyl alcohol or polyacrylic yarn is preferred in order to ensure uniform mixing.
成形方法としては１通常のセラミックスの成形方法が用
いられる。すなわち、加圧成形、テープ成形、鋳込成形
、射出成形などから製品の形状によって選ばれる。As the molding method, a normal ceramic molding method is used. That is, it is selected from pressure molding, tape molding, casting molding, injection molding, etc. depending on the shape of the product.
焼成温度は、使用するヒドロキシアパタイト０粒径など
によって影響を受ける焼結性及びヒドロキシアパタイト
と他Ｏ無機物質と０反応性によ）決められるが１通常１
００℃〜／ＪＪＯ℃の範凹から選ばれる。焼成温度が低
すぎると。The firing temperature is determined by the sinterability, which is influenced by the particle size of the hydroxyapatite used, and the reactivity of the hydroxyapatite with other inorganic substances.
Selected from the range 00°C to /JJO°C. If the firing temperature is too low.
ヒドロキシアパタイトと他の無機物質が反応しないし、
ヒドロキシアパタイト粒子同士も焼結しない。また、焼
成温度が高すぎると、ヒドロキシアパタイトが完全に分
解してしまう。Hydroxyapatite and other inorganic substances do not react,
Hydroxyapatite particles also do not sinter together. Furthermore, if the firing temperature is too high, hydroxyapatite will be completely decomposed.
以上の方法に工〉、多孔性でかつ気孔以外の部分は焼結
度が高い、ヒドロキシアパタイトを主成分とする焼結体
を得ることができる。By using the above method, it is possible to obtain a sintered body mainly composed of hydroxyapatite, which is porous and has a high degree of sintering in areas other than pores.
以下１本発明を実施例によって更に詳細に説明する。 The present invention will be explained in more detail below by way of examples.
実施例／
粒径／ ａｍ Ｏヒドロキシアパタイト（以下同じもの
を使用）１００重ｉｔ部、粒径０．３８ｍのアルミナ１
ｏｏｘ４ｉｋ部及びエチルアルコール−００重量部をボ
ールミル中で混合した。Example / Particle size / am O hydroxyapatite (hereinafter the same is used) 100 parts by weight, alumina 1 with a particle size of 0.38 m
4ik parts oox and 00 parts by weight of ethyl alcohol were mixed in a ball mill.
このスラリーを乾燥後に−Ｏ■φ×コ腸に加圧成形した
。この成形体を７２１０℃で１時間焼成して多孔質ヒド
ロキシアパタイト安結体を得た。この焼結体０６度を測
定したところ。This slurry was dried and then pressure-molded into a shape of -O■φ×coconut. This molded body was fired at 7210° C. for 1 hour to obtain a porous hydroxyapatite aggregate. This sintered body was measured at 06 degrees.
≠３体積方が気孔でおった。≠3 volumes were filled with pores.
実施例コ
ヒドロキシアパタイト／ ００１Ｒ景部１粒径ＯｍＪ
Ｊｌｍのシリカ１００１１ｉｉ部及びエチルアルコール
、２００重社部をボールミル中で混合した。Example cohydroxyapatite/001R Kabe 1 grain size OmJ
100 parts of JLM silica and 200 parts of ethyl alcohol were mixed in a ball mill.
このスラリーを実施例１と同様に処理して多孔質ヒドロ
キシアパタイト焼結体を得た。この焼結体の密度を測定
したところ、３７体積Ｓが気孔であった。This slurry was treated in the same manner as in Example 1 to obtain a porous hydroxyapatite sintered body. When the density of this sintered body was measured, 37 volumes S were pores.
実施例３
ヒドロキシアパタイト１００重量部１粒径０、／ ｔ
Ａｍのジルコニア１００重量部及びエテす
シアルコール２００重量部をボールミル１で混合した。Example 3 Hydroxyapatite 100 parts by weight 1 particle size 0, / t
100 parts by weight of Am zirconia and 200 parts by weight of ethyl alcohol were mixed in a ball mill 1.
このスラリーｔ−実施例／と同様に処理して多孔質ヒド
ロキシアパタイト焼結体を得た。This slurry was treated in the same manner as Example t to obtain a porous hydroxyapatite sintered body.
この焼結体の密度を測定したところ、弘７体積九が気孔
であった。When the density of this sintered body was measured, it was found that 9 by volume of the sintered body were pores.
実施例μ
ヒドロキシアパタイト７００重量部１粒径０．３μｍの
チタニア１００重量部及びエチルアルコール、２００１
１量部をボールミル中で混合した。このスラリーを実施
例１と同様に処理して多孔質ヒドロキシアパタイト焼結
体を得た。この焼結体の密度を測定したところ、≠３体
積九が気孔であった。Example μ 700 parts by weight of hydroxyapatite 100 parts by weight of titania with a particle size of 0.3 μm and ethyl alcohol, 2001
One part was mixed in a ball mill. This slurry was treated in the same manner as in Example 1 to obtain a porous hydroxyapatite sintered body. When the density of this sintered body was measured, it was found that ≠3 volumes were pores.
実施例よ一笑流側１
ヒドロキシアパタイトとジルコニア（実施例３と同じも
の）を表７に示す割合で秤量し、エチルアルコール−ｏ
ｏｘｈ部と共にボールミル中で混合し念、このスラリー
を実施例１と同様に処理して多孔質ヒドロキシアパタイ
ト焼結体を得た。この焼結体の密度から求めた気孔率を
表／に示す。Example 1: Hydroxyapatite and zirconia (same as Example 3) were weighed in the proportions shown in Table 7, and ethyl alcohol-o
After mixing with the oxh part in a ball mill, this slurry was treated in the same manner as in Example 1 to obtain a porous hydroxyapatite sintered body. Table 1 shows the porosity determined from the density of this sintered body.
表 ｌ
比較例／
ヒドロキシアパタイト粉末をλＯ■φ×２膿に加圧成形
した。この成形体ｔ−７λＳＯで１時間焼成して焼結体
を得た。この焼結体の気孔率は３冑積Ｓだった。Table 1 Comparative Example/Hydroxyapatite powder was pressure molded into λO■φ×2 pus. This molded body t-7λSO was fired for 1 hour to obtain a sintered body. The porosity of this sintered body was 3 S.
以上述べたごとく本発明によれば人工骨などの生体材料
用に使用し得る多孔質ヒドロキシアパタイト焼結体を極
めて容易に製造することが出来るので本発明方法は工業
的に優れたものである。As described above, according to the present invention, it is possible to extremely easily produce a porous hydroxyapatite sintered body that can be used for biomaterials such as artificial bones, so the method of the present invention is industrially superior.
Claims (2)
ヒドロキシアパタイトに対する他の無機物質の重量比が
０．００１以上で１以下の割合で混合して成形し焼成す
ることにより、ヒドロキシアパタイトを主成分とする多
孔質セラミックス焼結体を製造する方法であつて、前記
無機物質は、焼結温度以下でヒドロキシアパタイトと反
応し、その結果生成する反応生成物が焼結時の温度では
ガラス相を形成しない化合物となり得る無機物質である
ことを特徴とする多孔質セラミックス焼結体の製造方法
。(1) Hydroxyapatite powder and other inorganic substances,
A method for producing a porous ceramic sintered body containing hydroxyapatite as a main component by mixing hydroxyapatite with another inorganic substance at a weight ratio of 0.001 or more and 1 or less, forming and firing the mixture. The porous material is characterized in that the inorganic substance is an inorganic substance that reacts with hydroxyapatite at a temperature below the sintering temperature, and the resulting reaction product is a compound that does not form a glass phase at the sintering temperature. A method for producing quality ceramic sintered bodies.
びチタニアからなる群から選ばれた１種又は２種以上の
物質であることを特徴とす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 other inorganic substance is one or more substances selected from the group consisting of alumina, silica, zirconia, and titania.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61207288A JPH0757707B2 (en) | 1986-09-03 | 1986-09-03 | Manufacturing method of porous ceramics sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61207288A JPH0757707B2 (en) | 1986-09-03 | 1986-09-03 | Manufacturing method of porous ceramics sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6364954A true JPS6364954A (en) | 1988-03-23 |
| JPH0757707B2 JPH0757707B2 (en) | 1995-06-21 |
Family
ID=16537311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61207288A Expired - Lifetime JPH0757707B2 (en) | 1986-09-03 | 1986-09-03 | Manufacturing method of porous ceramics sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0757707B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04504403A (en) * | 1989-04-10 | 1992-08-06 | スティフテルセン セントルム フエル デンタルテクニク オク ビオマテリアル イ フッディンゲ | Synthetic ceramic materials and their manufacturing methods |
| JPH0532518A (en) * | 1991-07-26 | 1993-02-09 | Sekisui Plastics Co Ltd | Apatite composite particles |
| CN108689699A (en) * | 2018-06-14 | 2018-10-23 | 长沙鹏登生物陶瓷有限公司 | A kind of high-flexibility artificial bone joint ceramic composite and preparation method |
-
1986
- 1986-09-03 JP JP61207288A patent/JPH0757707B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04504403A (en) * | 1989-04-10 | 1992-08-06 | スティフテルセン セントルム フエル デンタルテクニク オク ビオマテリアル イ フッディンゲ | Synthetic ceramic materials and their manufacturing methods |
| JPH0532518A (en) * | 1991-07-26 | 1993-02-09 | Sekisui Plastics Co Ltd | Apatite composite particles |
| CN108689699A (en) * | 2018-06-14 | 2018-10-23 | 长沙鹏登生物陶瓷有限公司 | A kind of high-flexibility artificial bone joint ceramic composite and preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0757707B2 (en) | 1995-06-21 |
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