JPS58110465A - Hydroxy apatite target - Google Patents

Hydroxy apatite target

Info

Publication number
JPS58110465A
JPS58110465A JP56208639A JP20863981A JPS58110465A JP S58110465 A JPS58110465 A JP S58110465A JP 56208639 A JP56208639 A JP 56208639A JP 20863981 A JP20863981 A JP 20863981A JP S58110465 A JPS58110465 A JP S58110465A
Authority
JP
Japan
Prior art keywords
target
hydroxyapatite
hydroxy apatite
fluorine
present
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
Application number
JP56208639A
Other languages
Japanese (ja)
Other versions
JPS6127348B2 (en
Inventor
蛯原 正臣
正秀 井上
哲朗 小川
幸子 吉田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pentax Corp
Original Assignee
Asahi Kogaku Kogyo Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Asahi Kogaku Kogyo Co Ltd filed Critical Asahi Kogaku Kogyo Co Ltd
Priority to JP56208639A priority Critical patent/JPS58110465A/en
Publication of JPS58110465A publication Critical patent/JPS58110465A/en
Publication of JPS6127348B2 publication Critical patent/JPS6127348B2/ja
Granted legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Physical Vapour Deposition (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) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 本発明はトナースパッタリングの為のハイドロキシ・ア
パタイト・ターゲットに関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to hydroxyapatite targets for toner sputtering.

従来、リン酸カルシウム系のターゲットに関する研究・
開発レポートは少ない。X線回折パターン・レベルで純
粋なハイドロキシ・アパタイトからなるターゲットはス
パッタリングの際、一部分解してアパタイト、リン酸三
カルシウム、酸化カルシウムとなる。これは、ハイドロ
キシ・アパタイトの結晶構造に帰因するものでOHの欠
陥、 Caの欠陥によるものと思われる。これに対して
フッ素を含有したハイドロキシ・アパタイトは、OHの
欠陥部を補なう様にフッ素が置換されているため、スパ
ッタリングにおいてもより安定に存在するものと推察さ
れる。
Previous research on calcium phosphate targets
There are few development reports. A target made of hydroxyapatite that is pure at the X-ray diffraction pattern level is partially decomposed into apatite, tricalcium phosphate, and calcium oxide during sputtering. This is thought to be due to the crystal structure of hydroxyapatite and is caused by OH defects and Ca defects. On the other hand, in fluorine-containing hydroxyapatite, fluorine is substituted to compensate for OH defects, so it is presumed that it exists more stably even during sputtering.

本発明の目的は純粋なハイドロキシ・アパタイトの上記
欠点を解消する為に、フッ素アパタイトを含むハイドロ
キシ・アパタイトのターゲットを提供する二とである。
The object of the present invention is to provide a hydroxyapatite target containing fluoroapatite in order to overcome the above-mentioned drawbacks of pure hydroxyapatite.

以下、図によって本発明の概要を述へる。Hereinafter, an overview of the present invention will be described with reference to figures.

第1図及び第2図は本発明に係わるハイドロキシ・アパ
タイト・ターゲットの−・例を示すものであり、第1図
はその平面図、第2図はその側面図である。図中1はハ
イドロキシ・アパタイト焼結体、2は冷却用裏板、3は
ターゲット固定用穴である。
1 and 2 show an example of a hydroxyapatite target according to the present invention, with FIG. 1 being a plan view thereof and FIG. 2 being a side view thereof. In the figure, 1 is a hydroxyapatite sintered body, 2 is a cooling back plate, and 3 is a target fixing hole.

本発明に用いるハイドロキシ・アパタイト焼結体1はフ
ッ素を含んだハイドロキシ・アパタイト粉体を成形・焼
成して得られる。以下、焼結体の作製手順を述べる。
The sintered hydroxyapatite body 1 used in the present invention is obtained by molding and firing fluorine-containing hydroxyapatite powder. The procedure for producing the sintered body will be described below.

Ca(OH)□と11.PO4を出発原料とするハイド
ロキシ・アパタイトの湿式合成法において、滴下物であ
るH3PO4溶液に所要のフッ素化合物例えばフッ化ア
ンモニウム、フッ化カリウム、フッ化水素アンモニウム
、フッ化水素酸、フッ化水素ナトリウム。
Ca(OH)□ and 11. In the wet synthesis method of hydroxyapatite using PO4 as a starting material, necessary fluorine compounds such as ammonium fluoride, potassium fluoride, ammonium hydrogen fluoride, hydrofluoric acid, and sodium hydrogen fluoride are added to the H3PO4 solution that is dropped.

フッ化ナトリウム等の一部を添加する。Ca (OH)
Add some sodium fluoride, etc. Ca(OH)
.

の撹拌懸濁液にフッ素を含んだH,PO4溶液を滴下す
る。反応槽のpH値が中性になった時点で滴下を停止す
る。反応生成物である沈澱物をスプレードライヤーによ
り乾燥・造粒する。非晶質のハイドロキシ・アパタイト
粉体を凪焼・成形して焼成する。このようにしてハイド
ロキシ・アパタイト焼結体が得られる。
A fluorine-containing H,PO4 solution is added dropwise to the stirred suspension. The dropping is stopped when the pH value of the reaction tank becomes neutral. The reaction product, the precipitate, is dried and granulated using a spray dryer. Amorphous hydroxyapatite powder is calcined, shaped and fired. In this way, a sintered hydroxyapatite body is obtained.

一方、冷却用裏板2は銅、あるいはステンレスで作られ
ておリスバッタリングによりターゲット部材であるハイ
ドロキシ・アパタイト焼結体の温度が上昇することを抑
制している。
On the other hand, the cooling back plate 2 is made of copper or stainless steel and suppresses the rise in temperature of the hydroxyapatite sintered body, which is the target member, due to squirrel battering.

次に1以上のようにして作られたターゲット部材である
焼結体と冷却用裏板を加熱して、インジウムろうを使っ
てボンディングする。
Next, the sintered body, which is the target member made as described above, and the cooling back plate are heated and bonded using indium solder.

次に、本発明の一実施例をさらに詳しく説明する。0.
25M濃度のCa(0)1)2撹拌懸濁液1201.に
4.5grのフッ化水素アンモニウムNH,FHF (
この場合にはハイドロキシ・アパタイトに対するフッ素
の含有量は0.1%である)を溶解した0、3M濃度の
11.PO。
Next, one embodiment of the present invention will be described in more detail. 0.
Stirred suspension of Ca(0)1)2 at a concentration of 25M 1201. 4.5 gr of ammonium hydrogen fluoride NH, FHF (
In this case, the fluorine content with respect to hydroxyapatite is 0.1%) dissolved in 0.3M concentration of 11. P.O.

希釈液を供給速度3L/hで滴下する。反応槽のpH値
が10に下った時点で−・時H、PO4の滴下を中断す
る。反応槽のph値をlOに保留した状態で一昼夜撹拌
する。保留終了後H,PO,,の滴トを再開する。
The diluted solution is added dropwise at a feed rate of 3 L/h. When the pH value of the reactor drops to 10, the dropping of PO4 is stopped. The reaction vessel was stirred all day and night while maintaining the pH value at 1O. After the hold is completed, the dripping of H, PO, etc. is resumed.

反応槽のpi値が7に下った時点でII P(lの滴ド
髪終rする。生成沈澱物をスプレー・ドライヤーで乾燥
造粒する。こうして得られた粉体を700℃で■焼して
φ5“X5m/mの円板状に成形する。二のディスクを
1000℃、4h焼成して焼結体を得る。
When the pi value of the reaction tank has fallen to 7, a drop of II P (l) is stopped. The resulting precipitate is dried and granulated using a spray dryer. The powder thus obtained is calcined at 700°C. The second disk is then fired at 1000° C. for 4 hours to obtain a sintered body.

二の焼結体(寸法φ4’X4.5)と冷却用裏板Cuを
150℃に加熱した状態でインジウムろうでボンディン
グする。このようにして作製されたターゲットを用いて
Ti基板にコーティングする。コート膜をX線回折9分
元売度計で調べた結果、組成はハイドロキシ・アパタイ
トの非晶質体、膜厚は1.2μであった。
The second sintered body (dimensions φ4'×4.5) and the cooling back plate Cu are bonded with indium solder while heated to 150°C. A Ti substrate is coated using the target thus prepared. As a result of examining the coated film using a 9-minute X-ray diffraction meter, it was found that the composition was an amorphous hydroxyapatite and the film thickness was 1.2 μm.

読上のように′本発明のフッ素を含んだアパタイト・タ
ーゲットはスパッタリングの際、純粋なハイドロキシ・
アパタイト・ターゲットに比べて。
As you can see above, the fluorine-containing apatite target of the present invention is a pure hydroxyl target during sputtering.
compared to the apatite target.

アパタイト構造から低級リン酸カルシウム化合物への分
解が少ないという利点を有する。従って、本発明のター
ゲットを利用してスパッタリングを行えば、所要のコー
ティング素子の実現が可能となり、生体材料、工業材料
としての利用に有用である。
It has the advantage that the apatite structure is less likely to decompose into lower calcium phosphate compounds. Therefore, by performing sputtering using the target of the present invention, it becomes possible to realize a desired coating element, which is useful for use as a biological material or an industrial material.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明のハイドロキシ・アパタイト・ターゲッ
トの一実施例の平面図、第2図はその側面図である。 1:ハイドロキシ・アパタイト焼結体 2:冷却用裏板 3:ターゲット固定用穴 第1図     第2図
FIG. 1 is a plan view of an embodiment of the hydroxyapatite target of the present invention, and FIG. 2 is a side view thereof. 1: Hydroxy apatite sintered body 2: Cooling back plate 3: Target fixing hole Figure 1 Figure 2

Claims (1)

【特許請求の範囲】[Claims] スパッタリングにおけるターゲット部材に0.01〜3
.8%のフッ素を含むことを特徴とするハイドロキシ・
アパタイト・ターゲット。
0.01 to 3 for target member in sputtering
.. Hydroxy, which is characterized by containing 8% fluorine.
Apatite target.
JP56208639A 1981-12-23 1981-12-23 Hydroxy apatite target Granted JPS58110465A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP56208639A JPS58110465A (en) 1981-12-23 1981-12-23 Hydroxy apatite target

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP56208639A JPS58110465A (en) 1981-12-23 1981-12-23 Hydroxy apatite target

Publications (2)

Publication Number Publication Date
JPS58110465A true JPS58110465A (en) 1983-07-01
JPS6127348B2 JPS6127348B2 (en) 1986-06-25

Family

ID=16559564

Family Applications (1)

Application Number Title Priority Date Filing Date
JP56208639A Granted JPS58110465A (en) 1981-12-23 1981-12-23 Hydroxy apatite target

Country Status (1)

Country Link
JP (1) JPS58110465A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0339468A (en) * 1989-07-06 1991-02-20 Mitsui Eng & Shipbuild Co Ltd Hydroxyapatite target
CN1048291C (en) * 1997-12-12 2000-01-12 清华大学 Preparation of reinforced ion beam-deposited hydroxyl apatite coating for medical implant
CN102181840A (en) * 2011-06-22 2011-09-14 苏州晶纯新材料有限公司 Lithium cobalt oxide target material and preparation method thereof
CN102206802A (en) * 2010-03-29 2011-10-05 北京品一材料科技有限责任公司 All-solid-state film lithium ion battery related target material and manufacturing method thereof
CN102249661A (en) * 2011-06-22 2011-11-23 苏州晶纯新材料有限公司 Lithium phosphate target and preparation method thereof
CN102285790A (en) * 2011-06-22 2011-12-21 苏州晶纯新材料有限公司 Lithium iron phosphate target materials and preparation method thereof
GB2452823B (en) * 2007-08-30 2012-08-22 Hoya Corp Method of producing fluoroapatite
CN114956790A (en) * 2022-07-28 2022-08-30 广州市尤特新材料有限公司 Near-infrared high-transmittance TCO (transparent conductive oxide) target material and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0339468A (en) * 1989-07-06 1991-02-20 Mitsui Eng & Shipbuild Co Ltd Hydroxyapatite target
CN1048291C (en) * 1997-12-12 2000-01-12 清华大学 Preparation of reinforced ion beam-deposited hydroxyl apatite coating for medical implant
GB2452823B (en) * 2007-08-30 2012-08-22 Hoya Corp Method of producing fluoroapatite
US8609055B2 (en) 2007-08-30 2013-12-17 Hoya Corporation Method of producing fluoroapatite, fluoroapatite, and adsorption apparatus
CN102206802A (en) * 2010-03-29 2011-10-05 北京品一材料科技有限责任公司 All-solid-state film lithium ion battery related target material and manufacturing method thereof
CN102181840A (en) * 2011-06-22 2011-09-14 苏州晶纯新材料有限公司 Lithium cobalt oxide target material and preparation method thereof
CN102249661A (en) * 2011-06-22 2011-11-23 苏州晶纯新材料有限公司 Lithium phosphate target and preparation method thereof
CN102285790A (en) * 2011-06-22 2011-12-21 苏州晶纯新材料有限公司 Lithium iron phosphate target materials and preparation method thereof
CN114956790A (en) * 2022-07-28 2022-08-30 广州市尤特新材料有限公司 Near-infrared high-transmittance TCO (transparent conductive oxide) target material and preparation method thereof

Also Published As

Publication number Publication date
JPS6127348B2 (en) 1986-06-25

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