JPH0316955A - Preparation of whisker-dispersed calcium phosphate powder and preparation of sintered product - Google Patents
Preparation of whisker-dispersed calcium phosphate powder and preparation of sintered productInfo
- Publication number
- JPH0316955A JPH0316955A JP1149372A JP14937289A JPH0316955A JP H0316955 A JPH0316955 A JP H0316955A JP 1149372 A JP1149372 A JP 1149372A JP 14937289 A JP14937289 A JP 14937289A JP H0316955 A JPH0316955 A JP H0316955A
- Authority
- JP
- Japan
- Prior art keywords
- whisker
- calcium phosphate
- phosphate powder
- powder
- whiskers
- 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
- 239000001506 calcium phosphate Substances 0.000 title claims abstract description 35
- 229910000389 calcium phosphate Inorganic materials 0.000 title claims abstract description 33
- 235000011010 calcium phosphates Nutrition 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 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 title abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- -1 calcium phosphate compound Chemical class 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052586 apatite Inorganic materials 0.000 abstract description 4
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 abstract description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 3
- GBNXLQPMFAUCOI-UHFFFAOYSA-H tetracalcium;oxygen(2-);diphosphate Chemical compound [O-2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GBNXLQPMFAUCOI-UHFFFAOYSA-H 0.000 abstract description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 2
- 210000000988 bone and bone Anatomy 0.000 abstract description 2
- 210000001519 tissue Anatomy 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 7
- 229910052588 hydroxylapatite Inorganic materials 0.000 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 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 2
- 235000019731 tricalcium phosphate Nutrition 0.000 description 2
- 229940078499 tricalcium phosphate Drugs 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052587 fluorapatite Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008241 heterogeneous mixture Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229940085991 phosphate ion Drugs 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 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
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明はウイスカ一が均一に分散されたリン酸カルシウ
ム化合物粉体の製造法及びかようなリン酸カルシウム化
合物粉体を用いた焼結体の製造法に関する。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to a method for producing a calcium phosphate compound powder in which whiskers are uniformly dispersed, and a method for producing a sintered body using such a calcium phosphate compound powder. .
く従来の技術〉
従来よりウイスカ一をリン酸カルシウム化合物粉体に添
加し、機械的に混合撹拌した後、常圧下に焼結又は高圧
下にホットプレス焼結して焼結体を製造する方法は公知
である。ところが、この公知の方法では単にウイスカ一
とリン酸カルシウム化合物粉体とを機械的に混合撹拌す
るのみであるため、ウイスカ一が均一に分散されず、ウ
イスカ一が直接接触して混合物中に混在する個所が多々
存在する。故に、かような不均一混合物を焼結してもウ
イスカ一の直接接触部分が破壊点となり、高耐衝撃性、
高靭性の焼結体が得られないという欠点がある。Conventional technology> There is a known method for producing a sintered body by adding whiskers to calcium phosphate compound powder, mechanically mixing and stirring, and then sintering under normal pressure or hot press sintering under high pressure. It is. However, in this known method, the whiskers and the calcium phosphate compound powder are simply mixed and stirred mechanically, so the whiskers are not uniformly dispersed and there are places where the whiskers come into direct contact and are mixed in the mixture. There are many. Therefore, even if such a heterogeneous mixture is sintered, the point of direct contact between the whiskers will be the breaking point, resulting in high impact resistance and
The disadvantage is that a sintered body with high toughness cannot be obtained.
また、公知方法ではできるだけ高強度を付与するため、
場合によっては２０００気圧にも及ぶ超高圧下に焼結す
る。故に、コス］・高となりまた量産性に欠けるという
欠点がある。In addition, in order to provide as high strength as possible with known methods,
Sintering is carried out under ultra-high pressure of up to 2,000 atmospheres in some cases. Therefore, it has the disadvantage of being high in cost and lacking in mass production.
く発明が解決しようとする課題〉
本発明は、ウイスカ一がリン酸カルシウム化合物粉体中
に均一に分散されたウイスカ一分散リン酸カルシウム化
合物粉体の製造法を提供することを目的とする。また、
本発明は高強度且つ高靭性を有するウイスカー補強リン
酸カルシウム化合物焼結体を比較的温和な条件下にて効
率よく製造する方法を提供することを目的とする。Problems to be Solved by the Invention> An object of the present invention is to provide a method for producing a whisker-dispersed calcium phosphate compound powder in which whiskers are uniformly dispersed in the calcium phosphate compound powder. Also,
An object of the present invention is to provide a method for efficiently producing a whisker-reinforced calcium phosphate compound sintered body having high strength and toughness under relatively mild conditions.
〈課題を解決するための手段〉
本発明によれば、ウイスカーが分散されたリン酸カルシ
ウム化合物粉体のスラリーを撹拌しながら圧力下に水熱
処理し、ウイスカ一をリン酸カルシウム化合物粉体に均
一に分散することを特徴とするウイスカー分散リン酸カ
ルシウム化合物粉体の製造法が提供される。<Means for Solving the Problems> According to the present invention, a slurry of calcium phosphate compound powder in which whiskers are dispersed is hydrothermally treated under pressure while stirring to uniformly disperse the whiskers in the calcium phosphate compound powder. A method for producing whisker-dispersed calcium phosphate compound powder is provided.
また、本発明によれば、前記ウイスカ一分散リン酸カル
シウム化合物粉体を焼結することを特徴とするウイスカ
ー補強リン酸カルシウム化合物焼結体の製造法が提供さ
れる。Further, according to the present invention, there is provided a method for producing a whisker-reinforced calcium phosphate compound sintered body, which comprises sintering the whisker-unidispersed calcium phosphate compound powder.
以下、本発明につき更に詳細に説明する。The present invention will be explained in more detail below.
本発明では、まずウイスカ一が分散されたリン酸カルシ
ウム化合物粉体のスラリーを調製する。In the present invention, first, a slurry of calcium phosphate compound powder in which whiskers are dispersed is prepared.
本発明にて用いることができるウイスカ一としては、珪
素化物、たとえばα−Ｓｉ３Ｎ４等の窒化珪素，炭化珪
素等、並びに炭素、ムライ１・、アルミナ，シリカ、リ
ン酸カルシウム質ガラス等を挙げることができる。これ
らのうち、特に窒化珪素ウイスカ一を好ましく用いるこ
とができる。ウイスカ一の寸度は特に臨界的ではないが
、直径０．０３〜５μｍ、好ましくは約０．１μｍ、長
さ１〜５０μｍ、好ましくは約３μｍ程度が好ましい。Examples of whiskers that can be used in the present invention include silicides, such as silicon nitride such as α-Si3N4, silicon carbide, carbon, Murai 1, alumina, silica, calcium phosphate glass, and the like. Among these, silicon nitride whiskers can be particularly preferably used. Although the dimensions of the whisker are not particularly critical, the diameter is preferably about 0.03 to 5 μm, preferably about 0.1 μm, and the length is about 1 to 50 μm, preferably about 3 μm.
また、リン酸カルシウム化合物としては、水酸アバタイ
１・，炭酸アパタイ１〜、フッ素アパタイト，リン酸四
カルシウム、リン酸三カルシウム又はこれらのうちの２
種以上の混合物を挙げることができる。In addition, as the calcium phosphate compound, hydroxyl apatite 1., carbonate apatite 1~, fluoroapatite, tetracalcium phosphate, tricalcium phosphate, or two of these
Mention may be made of mixtures of more than one species.
これらのうちでは水酸アパタイト、水酸アパタイ１・と
リン酸四カルシウム及び／又はリン酸三カルシウムとの
混合物を特に好ましく用いることができる。スラリーを
調製するにあたっては、カルシウム塩水溶液、たとえば
Ｃａ（Ｎ○３）２水溶液などのカルシウムイオン溶液に
ウイスカ一を加えて懸濁させ、次にｐ Ｈをアルカリ側
へ調整するため、３
−４
たとえばアンモニア水を加えてｐ Ｉ−Ｉ １０にｉｌ
Ｗｌ１し、この懸濁液とリン酸塩水溶液、たとえば同一
ｐ Ｈの（ＮＨ．）２ＨＰ０４水溶液などのリン酸イオ
ン溶液とを反応させて湿式合或法によりウイスカ一とリ
ン酸カルシウム化合物との混合物を沈澱させるのが好ま
しい。次いで沈澱混合物を純水等にて口過洗浄し、不純
物を除いた後に、アンモニア水等の水に加えてウイスカ
一が分散されたリン酸カルシウム化合物粉体のスラリー
を得るのが望ましい。Among these, hydroxyapatite and a mixture of hydroxyapatite 1 and tetracalcium phosphate and/or tricalcium phosphate can be particularly preferably used. To prepare the slurry, whiskers are added and suspended in a calcium salt aqueous solution, for example, a calcium ion solution such as a Ca(N○3)2 aqueous solution, and then the pH is adjusted to the alkaline side by 3-4 For example, add aqueous ammonia to p I-I 10.
This suspension is reacted with an aqueous phosphate solution, for example a phosphate ion solution such as an aqueous (NH.)2HP04 solution of the same pH, to precipitate a mixture of whiskers and a calcium phosphate compound by wet synthesis. It is preferable to let Next, the precipitated mixture is rinsed with pure water or the like to remove impurities, and then added to water such as aqueous ammonia to obtain a slurry of calcium phosphate compound powder in which whiskers are dispersed.
ウイスカーのスラリー中における配合割合は特に臨界的
なものではないが、スラリー中のウイスカ一が１〜５Ｃ
）ｖｏｌ％、好まｂくは約１ ０ｖｏ ｌ％程度となる
ように配合するのが望ましい。The blending ratio of whiskers in the slurry is not particularly critical, but the proportion of whiskers in the slurry is 1 to 5C.
) vol %, preferably about 10 vol %.
本発明では次いでスラリーを圧力下に撹拌しながら水熱
処理する。水熱処理は１００〜３００℃、好ましくは約
２００℃にて、０．１〜２４時間、好ましくは約１０時
間、プロペラ撹拌器付きオー１〜クレープを用いて７０
〜１ ２ Ｑ ｒ．ｐ．ｍにて撹拌しながら圧力０．１
〜５ＭＰａ、好ましくは約２ Ｍ Ｐ ａにて行なうの
が望ましい。かようにして水熱処理した粉体は粒径０．
０２〜５μｍ程度を有し、微結晶のリン酸カルシウム化
合物粉体中に均一にウイスカ一が分散されており、極め
て分散性に優れる。In the present invention, the slurry is then hydrothermally treated while stirring under pressure. The hydrothermal treatment is carried out at 100-300°C, preferably about 200°C, for 0.1-24 hours, preferably about 10 hours, using an O-1-Crepe with a propeller stirrer for 70 minutes.
~1 2 Q r. p. Pressure 0.1 while stirring at
It is desirable to carry out at ~5 MPa, preferably about 2 MPa. The powder thus hydrothermally treated has a particle size of 0.
The whiskers are uniformly dispersed in the microcrystalline calcium phosphate compound powder, and have extremely excellent dispersibility.
かようにして得られたウイスカ一分散リン酸カルシウム
粉体を焼結してウイスカー補強リン酸カルシウム化合物
焼結体を得ることができる。焼結は粉体を或形した後、
８００〜１２００℃，好ましくは８００〜１１００℃に
て０．５〜１０時間、好ましくは約１時間常圧焼結して
も又更に８００〜１２００℃、好ましくは８００〜１１
００℃にて圧力５〜１００ＭＰａ、好ましくは約３ ０
ＭＰａにて０．５〜５０時間、好ましくは約ｌ時間ホッ
トプレス焼結してもよい。かようにして得られる焼結体
にはウイスカー相互の直接接触が認められず、従って破
壊点が存在せず、、耐衝撃強度、靭性に優れる。The whisker-unidispersed calcium phosphate powder thus obtained can be sintered to obtain a whisker-reinforced calcium phosphate compound sintered body. After sintering the powder into a certain shape,
Pressureless sintering at 800-1200°C, preferably 800-1100°C for 0.5-10 hours, preferably about 1 hour, or further sintering at 800-1200°C, preferably 800-11
Pressure 5-100MPa at 00℃, preferably about 30℃
Hot press sintering may be performed at MPa for 0.5 to 50 hours, preferably about 1 hour. In the sintered body thus obtained, no direct contact between the whiskers is observed, so there is no breaking point, and the sintered body has excellent impact resistance and toughness.
〈発明の効果〉
本発明によれば均一にウイスカ一が分散されたリン酸カ
ルシウム化合物粉体が得られるので、この粉体を焼結す
れば機械的強度の優れた焼結体が得られ、人工歯、人工
骨などの硬組織代替生体材料として利用することができ
る。<Effects of the Invention> According to the present invention, a calcium phosphate compound powder in which whiskers are uniformly dispersed can be obtained, so if this powder is sintered, a sintered body with excellent mechanical strength can be obtained, which can be used for artificial teeth. It can be used as a biomaterial to replace hard tissues such as artificial bones.
く実施例〉 次に本発明を実施例につき説明する。Example Next, the invention will be explained with reference to examples.
失亀鼻上
ウイスカーとしてα−Ｓ ］． ３ Ｎ４ （商品名ｒ
ＳＮＷ＃ １０Ｊタテホ化学社製）を０．１６７ｍｏｌ
２７ＱのＣ ａ （Ｎ○３）２水溶液５００ｍＱ中に１
０ｖｏＱ％加え、撹拌器にて３０分間懸濁した。次いで
この水溶液にアンモニア水を加え、ｐ Ｈ １ ０に調
整した後．ＰＨＩＯに調整した０．１ｍｏｌ２／Ｑの（
Ｎ Ｈ，）２Ｈ Ｐ Ｏ．水溶液５００−を常温にて撹
拌滴下し、湿式合或法によるα−Ｓ１３Ｎ４ウイスカ一
分散水酸アパタイトの沈澱物を得た。α-S as a whisker on the nose]. 3 N4 (Product name r
0.167 mol of SNW# 10J (manufactured by Tateho Chemical Co., Ltd.)
1 in 500 mQ of C a (N○3)2 aqueous solution of 27Q
0voQ% was added and suspended for 30 minutes using a stirrer. Next, aqueous ammonia was added to this aqueous solution to adjust the pH to 10. 0.1 mol2/Q adjusted to PHIO (
N H,)2H P O. An aqueous solution of 500 mL was added dropwise at room temperature with stirring to obtain a precipitate of α-S13N4 whisker monodispersed hydroxyapatite by a wet synthesis method.
次いでこの沈澱物を純水にて口過洗浄し、不純物イオン
を除去した後、ｐＨ１０に調整したアンモニア水中に混
合した。Next, the precipitate was rinsed with pure water to remove impurity ions, and then mixed into aqueous ammonia adjusted to pH 10.
この混合物を撹拌器付きオーｌ・クレープに仕込み１
０ ０ ｒ．ｐ．ｍにて撹拌しながら２００℃、２ＭＰ
ａにて１０時間水熱処理した後、乾燥し、水酸アパタイ
ト粉体を得た。Pour this mixture into a crepe with a stirrer 1
0 0 r. p. 200℃, 2MP while stirring at
After hydrothermal treatment in a for 10 hours, the mixture was dried to obtain hydroxyapatite powder.
得られた水酸アパタイト粉体の粉末Ｘｉ回折図（第１図
参照）（２０度ＣｕＫα）を調べたところ、α−Ｓｉ，
Ｎ４のピーグ（第１図中のａ）と水酸アパタイトのピー
ク（第１図中のａ以外のピーク）のみが認められ、その
他の化合物は検知されなかった。また得られた水酸アパ
タイト粉体を透過型電子顕微鏡（加速電圧２００ｋｖ，
倍率１万倍）にて調べたところ、棒状のα−Ｓｉ３Ｎ４
ウイスカー（約０．ＩＸ３μｍ）が六角柱状の水酸アパ
タイト微結晶（約２５Ｘ９Ｑｎｍ）に取り囲まれるよう
均一に分散しており，ウイスカ一が直接接触している個
所は観察されなかった。When examining the powder Xi diffraction pattern (see Figure 1) (20 degrees CuKα) of the obtained hydroxyapatite powder, it was found that α-Si,
Only N4 peaks (a in Figure 1) and hydroxyapatite peaks (peaks other than a in Figure 1) were observed, and no other compounds were detected. In addition, the obtained hydroxyapatite powder was examined using a transmission electron microscope (acceleration voltage 200 kv,
When examined at a magnification of 10,000 times, rod-shaped α-Si3N4
Whiskers (approximately 0.IX 3 μm) were uniformly dispersed so as to be surrounded by hexagonal columnar hydroxyapatite microcrystals (approximately 25×9 Q nm), and no place where the whiskers were in direct contact was observed.
失巖於又
実施例１にて得られた粉体をペレット状に金型成形し、
８００℃、９００℃、１０００℃、１１００℃、１２０
０℃にて各々１時間大気中にて常圧焼結した。得られた
焼結体の嵩密度を測定した結果を表１に示す。The powder obtained in Example 1 was molded into pellets,
800℃, 900℃, 1000℃, 1100℃, 120
Normal pressure sintering was performed in the air at 0° C. for 1 hour each. Table 1 shows the results of measuring the bulk density of the obtained sintered body.
−７
８一
去１μ４走
実施例１にて得られた粉体をペレット状に金型成形し、
１２００℃にて１時間大気中常圧焼結した後、８００〜
１２００℃、３０ＭＰａにて１時間各々ホットプレス焼
結した。-7 8-1 μ4 run The powder obtained in Example 1 was molded into a pellet shape,
After normal pressure sintering in the atmosphere at 1200℃ for 1 hour, 800℃~
Each sample was hot press sintered at 1200° C. and 30 MPa for 1 hour.
１１００℃の温度にて焼結した焼結体につきビッカース
法により硬度を測定したところ４．ＯＧＰａであった。The hardness of the sintered body sintered at a temperature of 1100°C was measured by the Vickers method, and the result was 4. It was OGPa.
また小圧子圧入破壊法により強度（ＫＩｃ）を調べたと
ころ、３ ． ０ＭＰ ａ−ｍ／／２であった。研磨面
のＳＥＭ写真を調べたところ、焼結体中に気孔はほとん
どみられず、ウイスカ一が互いに直接接触している個所
もみられなかった。In addition, when the strength (KIc) was investigated using the small indentation fracture method, it was found to be 3. It was 0MP a-m//2. When examining the SEM photograph of the polished surface, it was found that almost no pores were observed in the sintered body, and no place where the whiskers were in direct contact with each other was observed.
得られた焼結体の嵩密度を測定した結果を表１に示す。Table 1 shows the results of measuring the bulk density of the obtained sintered body.
表１Table 1
第１図は本発明の実施例１により得られた水酸アパタイ
ト粉末Ｘ線回折図である。
ａ・・α−Ｓｉ３Ｎ４のピーク。FIG. 1 is an X-ray diffraction diagram of hydroxyapatite powder obtained in Example 1 of the present invention. a... Peak of α-Si3N4.
Claims (1)
体のスラリーを撹拌しながら圧力下に水熱処理し、ウイ
スカーをリン酸カルシウム化合物粉体に均一に分散する
ことを特徴とするウイスカー分散リン酸カルシウム化合
物粉体の製造法。 ２）請求項１記載のウイスカー分散リン酸カルシウム化
合物粉体を焼結することを特徴とするウイスカー補強リ
ン酸カルシウム化合物焼結体の製造法。[Claims] 1) A whisker-dispersed calcium phosphate compound characterized in that a slurry of calcium phosphate compound powder in which whiskers are dispersed is hydrothermally treated under pressure while stirring to uniformly disperse whiskers in the calcium phosphate compound powder. Powder manufacturing method. 2) A method for producing a whisker-reinforced calcium phosphate compound sintered body, which comprises sintering the whisker-dispersed calcium phosphate compound powder according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1149372A JPH0316955A (en) | 1989-06-14 | 1989-06-14 | Preparation of whisker-dispersed calcium phosphate powder and preparation of sintered product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1149372A JPH0316955A (en) | 1989-06-14 | 1989-06-14 | Preparation of whisker-dispersed calcium phosphate powder and preparation of sintered product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0316955A true JPH0316955A (en) | 1991-01-24 |
Family
ID=15473696
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1149372A Pending JPH0316955A (en) | 1989-06-14 | 1989-06-14 | Preparation of whisker-dispersed calcium phosphate powder and preparation of sintered product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0316955A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2250509A (en) * | 1990-11-20 | 1992-06-10 | Mitsubishi Materials Corp | Apatite whiskers and their preparation |
| KR100473276B1 (en) * | 2001-12-05 | 2005-03-08 | 요업기술원 | Preparation of Si,Mg-containing hydroxyapatite whisker using a hydrothermal method and its application |
| KR100473275B1 (en) * | 2001-12-05 | 2005-03-08 | 요업기술원 | Preparation of Si,Mg-containing hydroxyapatite whisker using a molten salt method and its application |
| JP2008018385A (en) * | 2006-07-14 | 2008-01-31 | Kayaba Ind Co Ltd | Insolubilization treatment apparatus |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53111000A (en) * | 1977-03-11 | 1978-09-28 | Tokyo Ika Shika Daigakuchiyou | Method of making caoop205 base apatite |
| JPS63100006A (en) * | 1986-10-13 | 1988-05-02 | Norio Shimizu | Process for preparation of calcium phosphate and composite body thereof |
| JPS645938A (en) * | 1987-06-30 | 1989-01-10 | Lion Corp | Production of ceramic composite sintered compact |
-
1989
- 1989-06-14 JP JP1149372A patent/JPH0316955A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53111000A (en) * | 1977-03-11 | 1978-09-28 | Tokyo Ika Shika Daigakuchiyou | Method of making caoop205 base apatite |
| JPS63100006A (en) * | 1986-10-13 | 1988-05-02 | Norio Shimizu | Process for preparation of calcium phosphate and composite body thereof |
| JPS645938A (en) * | 1987-06-30 | 1989-01-10 | Lion Corp | Production of ceramic composite sintered compact |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2250509A (en) * | 1990-11-20 | 1992-06-10 | Mitsubishi Materials Corp | Apatite whiskers and their preparation |
| GB2250509B (en) * | 1990-11-20 | 1994-11-02 | Mitsubishi Materials Corp | Hydroxyapatite whiskers and their preparation |
| KR100473276B1 (en) * | 2001-12-05 | 2005-03-08 | 요업기술원 | Preparation of Si,Mg-containing hydroxyapatite whisker using a hydrothermal method and its application |
| KR100473275B1 (en) * | 2001-12-05 | 2005-03-08 | 요업기술원 | Preparation of Si,Mg-containing hydroxyapatite whisker using a molten salt method and its application |
| JP2008018385A (en) * | 2006-07-14 | 2008-01-31 | Kayaba Ind Co Ltd | Insolubilization treatment apparatus |
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