JPH03183670A - Production of porous zirconia ceramics - Google Patents
Production of porous zirconia ceramicsInfo
- Publication number
- JPH03183670A JPH03183670A JP32200589A JP32200589A JPH03183670A JP H03183670 A JPH03183670 A JP H03183670A JP 32200589 A JP32200589 A JP 32200589A JP 32200589 A JP32200589 A JP 32200589A JP H03183670 A JPH03183670 A JP H03183670A
- Authority
- JP
- Japan
- Prior art keywords
- ceramics
- zirconia
- zirconia ceramics
- pasp
- polymer
- 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
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 8
- 238000004898 kneading Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 11
- 239000012620 biological material Substances 0.000 abstract description 8
- 239000011148 porous material Substances 0.000 abstract description 7
- 210000000988 bone and bone Anatomy 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000008016 vaporization Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 1
- 102100035024 Carboxypeptidase B Human genes 0.000 description 19
- 101000946524 Homo sapiens Carboxypeptidase B Proteins 0.000 description 19
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 7
- -1 α-substituted styrene Chemical class 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000178 monomer Chemical class 0.000 description 2
- 150000003440 styrenes Chemical class 0.000 description 2
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- KKFHAJHLJHVUDM-UHFFFAOYSA-N n-vinylcarbazole Chemical compound C1=CC=C2N(C=C)C3=CC=CC=C3C2=C1 KKFHAJHLJHVUDM-UHFFFAOYSA-N 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Materials For Medical Uses (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は多孔質ジルコニアセラミックスの製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] This invention relates to a method for producing porous zirconia ceramics.
ジルコニアセラ旦ツクス材料は硬さ、機械的強度、耐熱
性、化学的安定性等に優れており、ＳｉＣやＳｉ３Ｎ４
等の他のセラミックス材料と比較しても耐熱性に遜色が
なく、しかもとりわけ靭性に優れることから、工業用セ
ラミックス材料として広く用いられている。Zirconia ceramic materials have excellent hardness, mechanical strength, heat resistance, chemical stability, etc.
It is widely used as an industrial ceramic material because it is comparable in heat resistance to other ceramic materials such as, and has particularly excellent toughness.
上記ジルコニアセラミックスは単結晶ファイバーを除き
、粉体を所定形状に成形したのち、焼成するかあるいは
、成形と焼成を同時に行うことによって製造していた。The above-mentioned zirconia ceramics have been manufactured by molding the powder into a predetermined shape, excluding the single crystal fiber, and then firing it, or by performing molding and firing at the same time.
化学的に安定な特性を生かして、セラミックス製品は様
々な分野に応用され、とりわけ医療分野、すなわち各種
医療機器や人工骨などの生体材料に不可欠のものとなっ
ている。Taking advantage of their chemically stable properties, ceramic products are used in a variety of fields, and are indispensable in the medical field, in particular for various medical devices and biomaterials such as artificial bones.
そこで、生体材料として、上記セラミックス製品の中で
も特に靭性に優れるジルコニアセラミックスの利用が考
えられるが、上記ジルコニアセラミックスには人工骨な
どの生体材料として使用するに必要な気孔をほとんど有
しないことから、その応用が遅れている。Therefore, the use of zirconia ceramics, which has particularly excellent toughness among the ceramic products mentioned above, could be considered as a biomaterial, but since the zirconia ceramics described above have almost no pores necessary for use as a biomaterial for artificial bones, etc. Application is delayed.
本発明は上記の事情を勘案して生体材料に好適な気孔を
有する多孔質ジルコニアセラミックスを提供することを
目的としている。The present invention takes the above circumstances into consideration and aims to provide porous zirconia ceramics having pores suitable for biomaterials.
上記の目的を達成するために、本発明は、以下の手段を
とる。すなわち、ジルコニア粉末原料９０〜９９重量％
と、ポリアクリルスチレンポリマー１−１０重量％とを
配合し、混練・成形後、焼成する多孔質ジルコニアセラ
ミックスの製造方法である。In order to achieve the above object, the present invention takes the following measures. That is, zirconia powder raw material 90-99% by weight
This is a method for producing porous zirconia ceramics, in which a mixture of 1 to 10% by weight of a polyacrylic styrene polymer is mixed, kneaded and molded, and then fired.
一般に、３００℃〜５００ ”ｃで気化する性質がある
ポリアクリルスチレンポリマー（以下ＰＡＳＰと称する
）を気孔形成剤として、ジルコニア粉末原料とともに混
練・成形した後、脱脂を行うことによってＰＡＳＰを飛
散させ、焼結時には組織内に気孔を形成した多孔質ジル
コニアセラミックスが得られる。In general, polyacrystyrene polymer (hereinafter referred to as PASP), which has the property of vaporizing at 300°C to 500"c, is used as a pore-forming agent and is kneaded and molded with zirconia powder raw material, and then degreased to disperse PASP. During sintering, porous zirconia ceramics with pores formed within the structure is obtained.
上記ＰＡＳＰの配合量が１重量％未満であると充分な気
孔を有するセラミックスの完成品が得られず、１０重量
％を超えた配合量であると、焼成工程における昇温途中
の３００〜４００ ”Ｃ付近で、多量に組織内に存在す
るＰＡＳＰの気化が急速にすすみ、破壊がおこる。また
成形時において脱型が困難となる等の事態を生じ、好ま
しくない。If the blending amount of PASP is less than 1% by weight, a finished ceramic product with sufficient pores will not be obtained, and if the blending amount exceeds 10% by weight, the temperature will rise to 300 to 400 % during the heating process in the firing process. In the vicinity of C, a large amount of PASP present in the structure rapidly evaporates, leading to destruction. In addition, it may become difficult to remove the mold during molding, which is undesirable.
また、気孔形成剤としての上記ＰＡＳＰは、具体的には
例えば、スチレン系樹脂としてのスチレン、ならびにα
−メチルスチレンの如きα−置換スチレン、ビニルトル
エン、０−クロロスチレンの如き核置換スチレン等、ス
チレン誘導体の重合体、これら単量体を主とし、これに
共重合可能な単量体、例えばアクリロニトリル、ならび
にメタアクリル酸、それらのメチルあるいはエチルエス
テルの如きビニル化合物、ビニルピリジン、ビニルカル
バゾールの如きビニル複素環化合物、ブタジェン、イソ
プレンの如き共役ジエン化合物の１種または２種以上を
混合した単量体混合物から得られる相互重合体、および
上記重合体を実質的に主成分とする熱可塑性樹脂組成物
が使用できる。In addition, the above-mentioned PASP as a pore-forming agent is specifically used, for example, with styrene as a styrene resin, and α
- Polymers of styrene derivatives such as α-substituted styrene such as methylstyrene, vinyltoluene, and nuclear-substituted styrene such as 0-chlorostyrene, and monomers copolymerizable with these monomers, such as acrylonitrile. and methacrylic acid, vinyl compounds such as their methyl or ethyl esters, vinyl heterocyclic compounds such as vinyl pyridine and vinyl carbazole, and conjugated diene compounds such as butadiene and isoprene. Interpolymers obtained from mixtures and thermoplastic resin compositions containing the above-mentioned polymers as a substantial component can be used.
粉末状のＰＡＳＰを得るためには、上記樹脂の成形体を
粉砕するか、或いは液状の上記樹脂重合体ラスプレート
ライヤーで噴霧・乾燥するなどの手段を用いることがで
きる。In order to obtain PASP in powder form, methods such as pulverizing the molded resin, or spraying and drying the resin polymer in liquid form with a lath plate dryer can be used.
以下、実施例をもとにさらに説明を加える。 Further explanation will be given below based on examples.
ジルコニア粉末原料としての市販のイツトリアを添加し
た部分安定化ジルコニア粉末原料とＰＡｓｐとを第１表
に示す割合で比較例１〜３および実施例１．２のように
混合した。A commercially available ittria-added partially stabilized zirconia powder raw material as a zirconia powder raw material and PAsp were mixed in the proportions shown in Table 1 as in Comparative Examples 1 to 3 and Example 1.2.
上記のそれぞれの配合物をアムスラー成形機で成形圧２
００ｋｇｆ／ａ＋！で一軸成形を行い、さらに上記−軸
成形体をＣＩＰ装置を用いて成形圧９゜Ｏｋｇ ｆ ／
ｃａｌで成形した。上記成形段階においては、比較例
２．３では成形後の脱型が極めて困難であった。Each of the above formulations was molded using an Amsler molding machine under a molding pressure of 2
00kgf/a+! uniaxial molding is carried out, and the above-mentioned -axial molded body is further molded using a CIP device at a molding pressure of 9°Okg f/
Molded with cal. In the above molding stage, in Comparative Example 2.3, demolding after molding was extremely difficult.
前述の成形体を炭化珪素炉を用いて大気雰囲気中で焼成
した。昇温速度は２℃／ｍｉｎであり、１４５０℃で２
時間保持した。この段階において昇温途中の３００〜４
００℃付近でＰＡＳＰの気化により、組織内周辺に悪影
響を及ぼすわけであるが、３００〜４００℃及びＳＯＯ
℃付近の２点あるＰＡＳＰの昇華点に数時間保持するか
、あるいは脱脂炉を用いることによりこの問題点を解決
することができる。The above molded body was fired in an air atmosphere using a silicon carbide furnace. The temperature increase rate is 2℃/min, and at 1450℃
Holds time. At this stage, 300 to 4
The vaporization of PASP at around 00℃ has a negative effect on the surrounding tissue, but at 300-400℃ and SOO
This problem can be solved by holding the PASP at two sublimation points near .degree. C. for several hours or by using a degreasing furnace.
上記焼成工程中、比較例２．３は、昇温途中に破壊がお
こり焼結体が得られなかった。During the above firing step, in Comparative Example 2.3, destruction occurred during the temperature rise and no sintered body was obtained.
得られた成形体及び焼結体のかさ比重及び気孔率を第２
表に示す。また、ＰＡＳＰの配合量と気孔率との関係を
第１図に、ＰＡＳＰの配合量と焼結体密度との関係を第
２図に示す。それによれば、ＰＡＳＰの配合量が多くな
るに従い、気孔率が増大し、密度が低下する傾向がみら
れ、実施例１．２の気孔率は生体材料として使用するの
に満足する値で、ＰＡＳＰの配合量が適量であることを
示している。The bulk specific gravity and porosity of the obtained molded body and sintered body were
Shown in the table. Further, FIG. 1 shows the relationship between the amount of PASP blended and the porosity, and FIG. 2 shows the relationship between the amount of PASP blended and the density of the sintered body. According to this, as the amount of PASP added increases, the porosity tends to increase and the density tends to decrease.The porosity of Example 1.2 is a value that is satisfactory for use as a biomaterial, and PASP This shows that the blended amount is appropriate.
なお、本発明は上記実施例に限られるものではなく、混
練・成形手段や焼成条件など本発明の趣旨を逸脱しない
範囲で適宜応用して実施すればよいことはいうまでもな
い。It goes without saying that the present invention is not limited to the above-mentioned embodiments, and may be implemented by appropriately applying kneading/molding means, firing conditions, etc. without departing from the spirit of the present invention.
また、本発明による多孔質ジルコニアセラミックスを複
雑形状の人工骨として用いるには、−旦１０００〜１２
００℃で仮焼し、仮焼体加工を行って必要な機械的強度
を得た後に、本焼成を実施するのが好ましい。In addition, in order to use the porous zirconia ceramic according to the present invention as an artificial bone having a complex shape, it is necessary to
It is preferable to perform main firing after calcining at 00°C and processing the calcined body to obtain the necessary mechanical strength.
〈以下余白〉
第
表
ＰＡＳＰ配合表唾量χ）
〔本発明の効果〕
本発明による多孔質ジルコニアセラミックスは、製造方
法が簡易であるばかりでなく、ジルコニアセラミックス
本来のもつ性質である機械的強度、耐摩耗性が高いとい
う特長をも有し、種々の分野に応用可能で、特に人工骨
などの生体材料の分野に最適な多孔質ジルコニアセラミ
ックスが得られる。<Space below> Table PASP blended saliva amount χ) [Effects of the present invention] The porous zirconia ceramics according to the present invention not only have a simple manufacturing method, but also have excellent mechanical strength, which is the inherent property of zirconia ceramics. Porous zirconia ceramics, which also have the feature of high wear resistance and can be applied to various fields, are particularly suitable for the field of biomaterials such as artificial bones.
第１図はこの発明によってできた多孔質セラミックスの
ＰＡＳＰ配合量と気孔率の関係を示す図である。第２図
は同じ＜ＰＡＳＰ配合量と焼結体密度の関係を示す図で
ある。
！
ＰＡＳＰ配合量（重量８）
ＰＡＳＰ配合量と気孔率の関係図
第１図
ＰＡＳＰ配含量（重量％）
ＰＡＳＰ配合Ｉと焼結体密度との関係間第 ２ 図FIG. 1 is a diagram showing the relationship between the PASP content and porosity of porous ceramics made according to the present invention. FIG. 2 is a diagram showing the relationship between the PASP blending amount and the sintered body density. ! PASP blending amount (weight 8) Relationship between PASP blending amount and porosity Figure 1 PASP blending amount (weight %) Relationship between PASP blending I and sintered compact density Figure 2
Claims (1)
クリルスチレンポリマー１〜１０重量％とを配合し、混
練・成形後、焼成することを特徴とする多孔質ジルコニ
アセラミックスの製造方法。(1) A method for producing porous zirconia ceramics, which comprises blending 90 to 99% by weight of a zirconia powder raw material and 1 to 10% by weight of a polyacrystyrene polymer, kneading and shaping, and then firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32200589A JPH03183670A (en) | 1989-12-11 | 1989-12-11 | Production of porous zirconia ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32200589A JPH03183670A (en) | 1989-12-11 | 1989-12-11 | Production of porous zirconia ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03183670A true JPH03183670A (en) | 1991-08-09 |
Family
ID=18138859
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32200589A Pending JPH03183670A (en) | 1989-12-11 | 1989-12-11 | Production of porous zirconia ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03183670A (en) |
-
1989
- 1989-12-11 JP JP32200589A patent/JPH03183670A/en active Pending
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