JPH0757707B2 - Manufacturing method of porous ceramics sintered body - Google Patents
Manufacturing method of porous ceramics sintered bodyInfo
- Publication number
- JPH0757707B2 JPH0757707B2 JP61207288A JP20728886A JPH0757707B2 JP H0757707 B2 JPH0757707 B2 JP H0757707B2 JP 61207288 A JP61207288 A JP 61207288A JP 20728886 A JP20728886 A JP 20728886A JP H0757707 B2 JPH0757707 B2 JP H0757707B2
- Authority
- JP
- Japan
- Prior art keywords
- hydroxyapatite
- sintered body
- inorganic substance
- porous
- porous ceramics
- 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 - Lifetime
Links
- 239000000919 ceramic Substances 0.000 title claims description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 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 40
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 39
- 239000000126 substance Substances 0.000 claims description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 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
- 238000000465 moulding Methods 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 239000000203 mixture Substances 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 5
- 239000012620 biological material Substances 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 3
- 238000005187 foaming Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910014497 Ca10(PO4)6(OH)2 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 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
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 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
- 238000011835 investigation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004584 polyacrylic acid 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)
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の製造方
法に関する。TECHNICAL FIELD The present invention relates to a method for producing a porous hydroxyapatite sintered body.
多孔質ヒドロキシアパタイト焼結体は、人工骨などの生
体材料用として有望視されており、通常発泡法により多
孔化された成形体を焼成することにより製造されてき
た。BACKGROUND ART Porous hydroxyapatite sintered compacts are regarded as promising for biomaterials such as artificial bones, and have usually been produced by firing a molded body that has been made porous by a foaming method.
しかし、発泡操作が煩雑であるため、多孔質ヒドロキシ
アパタイト焼結体の製造は困難であつた。そのため、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 a porous hydroxyapatite sintered body. Therefore, a new method capable of producing a porous hydroxyapatite sintered body that can be used for biomaterials such as artificial bone has been desired.
〔問題点を解決するための手段〕 本発明者等は上記の点に鑑み種々検討した結果、以外に
も、特定の性質を有する無機化合物を混合することによ
つて、極めて容易に多孔質な焼結体を得られることを知
得して本発明に到達した。[Means for Solving Problems] As a result of various investigations made by the present inventors in view of the above points, in addition to the above, by mixing an inorganic compound having specific properties, it is extremely easy to form a porous material. The present invention has been achieved by knowing that a sintered body can be obtained.
すなわち、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0.001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ツ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ツクス
焼結体の製造方法に存する。That is, the gist of the present invention is that hydroxyapatite powder and another inorganic substance are mixed at a weight ratio of the other inorganic substance to hydroxyapatite of 0.001 or more and less than 1 and molded and fired to form hydroxyapatite. A method for producing a porous ceramics sintered body containing as a main component, wherein the inorganic substance reacts with hydroxyapatite at a sintering temperature or lower, and a reaction product generated as a result is glass at a temperature at the time of sintering. A method for producing a porous ceramics sintered body is characterized by being an inorganic substance that can be a compound that does not form a phase.
以下、本発明を詳細に説明するに、本発明で使用するヒ
ドロキシアパタイトとしては、Ca10（PO4）６（OH）２
の化学式で示されるヒドロキシアパタイトであつて、13
50℃以下で分解せずに緻密に焼結する物質が用いられ
る。Hereinafter, the present invention will be described in detail. As the hydroxyapatite used in the present invention, Ca 10 (PO 4 ) 6 (OH) 2 is used.
The hydroxyapatite represented by the chemical formula:
A substance that is densely sintered at a temperature of 50 ° C or less without being decomposed is used.
他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
い化合物となり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、アルミナ、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、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。As the other inorganic substance, any inorganic substance that reacts with hydroxyapatite at a sintering temperature of hydroxyapatite or lower and the reaction product formed as a result can be a compound that does not form a glass phase at the temperature at the time of sintering Can be used. Specific examples include alumina, silica, zirconia, and titania. If a substance that does not react with hydroxyapatite is used, the hydroxyapatite does not become porous but becomes dense. Further, if the reaction product formed as a result of reacting with hydroxyapatite forms a glass phase at the temperature at the time of sintering, hydroxyapatite will sinter densely.
これら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10μｍ以下、特には１μｍ以
下が好ましい。These hydroxyapatite and other inorganic substances are usually used as a powder, and the particle size is preferably 10 μm or less, particularly preferably 1 μm or less.
ヒドロキシアパタイトと他の無機物質の混合割合は、ヒ
ドロキシアパタイトに対する他の無機物質の重量比が0.
001以上、特には0.01以上で、１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 weight ratio of other inorganic substances to hydroxyapatite is 0.
It is 001 or more, particularly 0.01 or more and 1 or less, but if the amount of this inorganic substance is too small, it becomes difficult to make it porous, and if it is too large, it becomes 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の混合方法として
は、通常のセラミツクス粉体の混合方法が用いられる。
乾式混合でも湿式混合でも良いが、より均一に混合する
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、ポリアクリル酸系のバインダーを含有する水溶液
等を用いた湿式混合を行なうことが好ましい。As a method of mixing the hydroxyapatite and the other inorganic substance, an ordinary method of mixing ceramic powder is used.
Either dry mixing or wet mixing may be used, but for more uniform mixing, it is preferable to perform wet mixing using an organic solvent such as alcohol, or an aqueous solution containing polyvinyl alcohol or a polyacrylic acid binder.
成形方法としては、通常のセラミツ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つて選ばれる。As a molding method, a usual ceramic molding method is used. That is, it is selected according to the shape of the product from pressure molding, tape molding, cast molding, injection molding and the like.
焼成温度は、使用するヒドロキシアパタイトの粒径など
によつて影響を受ける焼結性及びヒドロキシアパタイト
と他の無機物質との反応性により決められるが、通常60
0℃〜1350℃の範囲から選ばれる。焼成温度が低すぎる
と、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。The firing temperature is determined by the sinterability which is affected by the particle size of hydroxyapatite used and the reactivity of hydroxyapatite with other inorganic substances, but usually 60
It is selected from the range of 0 ° C to 1350 ° C. If the firing temperature is too low, hydroxyapatite does not react with other inorganic substances, and hydroxyapatite particles do not sinter. If the firing temperature is too high, the hydroxyapatite will be completely decomposed.
以上の方法により、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 the above method, it is possible to obtain a sintered body containing hydroxyapatite as a main component, which is porous and has a high degree of sintering except for the pores.
以下、本発明を実施例によつて更に詳細に説明する。 Hereinafter, the present invention will be described in more detail with reference to Examples.
実施例１ 粒径１μｍのヒドロキシアパタイト（以下同じものを使
用）100重量部、粒径0.3μｍのアルミナ100重量部及び
エチルアルコール200重量部をボールミル鋳で混合し
た。Example 1 100 parts by weight of hydroxyapatite having a particle size of 1 μm (the same ones will be used hereinafter), 100 parts by weight of alumina having a particle size of 0.3 μm and 200 parts by weight of ethyl alcohol were mixed by ball mill casting.
このスラリーを乾燥後に20mmφ×2mmに加圧成形した。
この成形体を1250℃で１時間焼成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、43体積％が気孔であつた。After this slurry was dried, it was pressure-molded to 20 mmφ × 2 mm.
This compact was fired at 1250 ° C. for 1 hour to obtain a porous hydroxyapatite sintered body. When the density of this sintered body was measured, 43% by volume was found to be pores.
実施例２ ヒドロキシアパタイト100重量部、粒径0.3μｍのシリカ
100重量部及びエチルアルコール200重量部をボールミル
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、37体積％が気孔であつた。Example 2 100 parts by weight of hydroxyapatite, silica having a particle size of 0.3 μm
100 parts by weight and 200 parts by weight of ethyl alcohol were 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, 37% by volume was found to be pores.
実施例３ ヒドロキシアパタイト100重量部、粒径0.16μｍのジル
コニア100重量部及びエチルアルコール200重量部をボー
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、41体積％が気孔であ
つた。Example 3 100 parts by weight of hydroxyapatite, 100 parts by weight of zirconia having a particle size of 0.16 μm and 200 parts by weight of ethyl alcohol were 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, 41% by volume was found to be pores.
実施例４ ヒドロキシアパタイト100重量部、粒径0.3μｍのチタニ
ア100重量部及びエチルアルコール200重量部をボールミ
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、43体積％が気孔であつ
た。Example 4 100 parts by weight of hydroxyapatite, 100 parts by weight of titania having a particle size of 0.3 μm and 200 parts by weight of ethyl alcohol were 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, 43% by volume was found to be pores.
実施例５〜実施例８ 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１に示す割合で秤量し、エチルアルコール300
重量部と共に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。この焼結体の密度から求めた気孔率を表
１に示す。Examples 5 to 8 Hydroxyapatite and zirconia (the same as in Example 3) were weighed in the proportions shown in Table 1 to obtain ethyl alcohol 300.
Mixed in a ball mill with parts by weight. This slurry was treated in the same manner as in Example 1 to obtain a porous hydroxyapatite sintered body. Table 1 shows the porosity obtained from the density of this sintered body.
比較例１ ヒドロキシアパタイト粉末を20mmφ×2mmに加圧成形し
た。この成形体を1250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体積％だつた。 Comparative Example 1 Hydroxyapatite powder was pressure-molded into 20 mmφ × 2 mm. This compact was fired at 1250 for 1 hour to obtain a sintered body.
The porosity of this sintered body was 3% by volume.
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, a porous hydroxyapatite sintered body that can be used for a biomaterial such as an artificial bone can be manufactured very easily, so the method of the present invention is industrially excellent.
Claims (2)
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0.001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
多孔質セラミツ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ツクス焼結体の製造方
法。1. A main component of hydroxyapatite is obtained by mixing hydroxyapatite powder and another inorganic substance in a weight ratio of the other inorganic substance to hydroxyapatite of 0.001 or more and molding and firing the mixture. A method for producing a porous ceramics sintered body, wherein the inorganic substance reacts with hydroxyapatite at a sintering temperature or lower, and the resulting reaction product forms a glass phase at the temperature at the time of sintering. A method for producing a porous ceramics sintered body, which is an inorganic substance capable of becoming a non-compound.
ニア及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 other inorganic substance is one or more substances selected from the group consisting of alumina, silica, zirconia, and titania.
The manufacturing method according to the item.
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 JPS6364954A (en) | 1988-03-23 |
| JPH0757707B2 true 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) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE465571B (en) * | 1989-04-10 | 1991-09-30 | Stiftelsen Ct Foer Dentaltekni | SET TO MAKE A COMPOSITIVE CERAMIC MATERIAL WITH BIOACTIVE PROPERTIES |
| JP2837292B2 (en) * | 1991-07-26 | 1998-12-14 | 積水化成品工業株式会社 | 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
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6364954A (en) | 1988-03-23 |
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