JPH0344145B2 - - Google Patents
Info
- Publication number
- JPH0344145B2 JPH0344145B2 JP23992383A JP23992383A JPH0344145B2 JP H0344145 B2 JPH0344145 B2 JP H0344145B2 JP 23992383 A JP23992383 A JP 23992383A JP 23992383 A JP23992383 A JP 23992383A JP H0344145 B2 JPH0344145 B2 JP H0344145B2
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- tellurium
- sintering
- powder
- target plate
- 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
Links
- 239000000843 powder Substances 0.000 claims description 12
- 238000004544 sputter deposition Methods 0.000 claims description 10
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052714 tellurium Inorganic materials 0.000 claims description 7
- 229910001215 Te alloy Inorganic materials 0.000 claims description 6
- 238000005245 sintering Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000005452 bending Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Description
この発明は、スパツタリング用ターゲツト板に
関する。
電子工業、電気工業等の分野で用いられるBi，
Se、Te、Sb、In、Sn等の金属または半金属ある
いはこれらの合金の薄膜は、一般に真空蒸着法ま
たはスパツタリング法によつて基板上へ形成され
る。ところで、上記スパツタリングに用いられる
テルルもしくはテルル合金等のターゲツト板は、
従来前記金属等を真空中や不活性ガス中で溶融
し、鋳型に鋳造する鋳造法や前記金属等の粉末を
押型で高い成形圧下で加圧成形後、加熱して焼結
する、コールドプレス法で製造されている。
しかし、鋳造法では、上記金属等の蒸気圧が高
いため製造中、蒸発量が多く歩留りが低下する問
題、及び、これら蒸気は有毒なので、除害や安全
上に問題がある。また、鋳造した金属等は、ガラ
ス質のため製造時の冷却やスパツタリング時の発
熱に伴つて割れやガス発生が生じ易い問題があ
る。
さらに、コールドプレス法は、高密度焼結体を
得るには高い成形圧が必要であり圧縮性の悪い粉
体に対しては押型より取り出す際に圧縮割れやス
プリングバツグによつて割れる危険性が高い。そ
して、蒸気圧の高い金属等を焼結させるには、表
面積が大きいので蒸発ロスが多いなどの問題があ
る。
この発明は、以上の点に鑑みてなされたもので
あつて、すなわちテルル粉末あるいはテルル合金
粉末を加圧下で成形焼結し、密度比を70〜90％に
調整することにより強い曲げ強さを有して割れに
くいテルルもしくはテルル合金よりなるスパツタ
リング用ターゲツト板を提供するものである。
ここで、密度比とは、金属の真比重に対する焼
結体の見掛密度の百方比をいう。
加圧成形および焼結は通常行われる粉末冶金的
方法で良いが、比較的低い成形圧で粉体を加圧成
形したのちに、加圧下で焼結する方が一般に好結
果が得られる。
加圧下焼結のためには、圧縮焼結法あるいはホ
ツトプレス法があるが、粉体を充填した押型を加
熱する際の熱膨脹や熱歪みを利用して加圧下焼結
を実施する方法も簡便な方法である。
焼結温度は原料の融点の0.75〜0.95倍、好まし
くは0.9倍がよく、テルルターゲツト板製造の際
の焼結温度は340〜430℃、好ましくは410℃とす
る。
焼結時の雰囲気は水素あるいはアルゴン雰囲気
とすることが望ましい。
以下、実施例に基づいてこの発明を説明する。
市販されているテルルシヨツトを−60meshで
あり、かつ−325meshの比率が40％程度となるよ
うに粉砕したテルル粉末を、所定の形状たとえば
薄肉厚の円盤状に成形圧力10〜500Kg／cm2好まし
くは150〜250Kg／cm2において加圧成形したのち、
加圧下で焼結することにより密度比70〜90％の焼
結体とした。密度比を70〜90％とする理由は、密
度比70％以下では曲げ強さが弱く、90％以上では
気孔が少なくなるのでクラツクが発生し易く、且
つ気孔が閉鎖されたものとなり通気孔とならない
のでスパツタリング時に割れやガスが発生しやす
くなるからである。本発明に係るターゲツト板
は、強い曲げ強さを有し、割れにくいものとなつ
ているので、スパツタリング時に急熱されても割
れやガスの発生がなく、ターゲツト板として良好
な性状を有している。
次に、本発明に係るスパツタリング用ターゲツ
トと、高圧圧縮成形常圧焼結したターゲツト板の
物性値の測定比較を表−１に示す。
本発明に係るターゲツト板においては、押型に
装填された粉末を158Kg／cm2の成形圧で圧縮成形
したのち、水素雰囲気中で410℃において加圧焼
結することによつて製造した。一方、従来法によ
る高圧圧縮成形常圧焼結ターゲツト板において
は、粉末を500Kg／cm2の成形圧で常温において圧
縮して成形体を製造し、水素雰囲気中で410℃に
おいて常圧下で焼結した。
なお、焼結する粉末としては、両者とも−
60meshでかつ−325mhshの比率が40％程度とな
るように粉砕されたテルルの粉末を使用した。ま
た、物性値のうち、曲げ強さは、炭素協会規格
JCAS−10−1968−44に従つて測定し、密度比は
JISZ2500−319に準じ測定を行ない評価を行なつ
た。
The present invention relates to a target plate for sputtering. Bi used in fields such as electronic industry and electrical industry,
A thin film of a metal or semimetal such as Se, Te, Sb, In, Sn, or an alloy thereof is generally formed on a substrate by a vacuum evaporation method or a sputtering method. By the way, the target plate made of tellurium or tellurium alloy used in the above sputtering is
Conventionally, there is a casting method in which the metal, etc. is melted in a vacuum or in an inert gas and cast into a mold, and a cold press method, in which the powder of the metal, etc. is pressure-formed in a mold under high molding pressure, and then heated and sintered. Manufactured in However, in the casting method, since the vapor pressure of the above-mentioned metals is high, the amount of evaporation during production is large, resulting in a decrease in yield.Also, since these vapors are toxic, there are problems in terms of abatement and safety. Furthermore, since cast metals are glassy, they tend to crack or generate gas when cooled during production or generated during sputtering. Furthermore, the cold press method requires high compacting pressure to obtain a high-density sintered body, and there is a risk that powders with poor compressibility may break due to compression cracks or spring bags when removed from the mold. expensive. When sintering metals with high vapor pressure, there are problems such as a large amount of evaporation loss due to the large surface area. This invention has been made in view of the above points. Specifically, tellurium powder or tellurium alloy powder is molded and sintered under pressure, and the density ratio is adjusted to 70 to 90%, thereby achieving strong bending strength. To provide a target plate for sputtering made of tellurium or a tellurium alloy, which is hard to break. Here, the density ratio refers to the 100/100 ratio of the apparent density of the sintered body to the true specific gravity of the metal. Pressure forming and sintering may be carried out by conventional powder metallurgical methods, but better results are generally obtained by press forming the powder at a relatively low compacting pressure and then sintering under pressure. There are compression sintering methods and hot press methods for sintering under pressure, but a simple method of performing sintering under pressure is one that utilizes thermal expansion and thermal distortion when heating a mold filled with powder. It's a method. The sintering temperature is preferably 0.75 to 0.95 times, preferably 0.9 times, the melting point of the raw material, and the sintering temperature during production of the tellurium target plate is 340 to 430°C, preferably 410°C. The atmosphere during sintering is preferably a hydrogen or argon atmosphere. The present invention will be explained below based on examples. Tellurium powder obtained by pulverizing a commercially available tellurium shot so that the mesh size is -60mesh and the ratio of -325mesh is about 40% is molded into a predetermined shape, such as a thin disk shape, under a pressure of 10 to 500 kg/ cm2 , preferably. After pressure forming at 150-250Kg/ cm2 ,
By sintering under pressure, a sintered body with a density ratio of 70 to 90% was obtained. The reason why the density ratio is set to 70-90% is that if the density ratio is less than 70%, the bending strength will be weak, and if it is more than 90%, the number of pores will decrease, making cracks more likely to occur. This is because cracks and gas are likely to be generated during sputtering. The target plate according to the present invention has strong bending strength and is not easily cracked, so even if it is rapidly heated during sputtering, it does not crack or generate gas, and has good properties as a target plate. There is. Next, Table 1 shows a comparison of the measured physical properties of the sputtering target according to the present invention and a target plate formed by high-pressure compression molding and pressureless sintering. The target plate according to the present invention was produced by compression molding the powder loaded into a mold at a molding pressure of 158 kg/cm 2 and then pressure sintering it at 410° C. in a hydrogen atmosphere. On the other hand, in the conventional method of high-pressure compression molding and pressureless sintering target plates, the powder is compressed at room temperature with a compacting pressure of 500 kg/cm 2 to produce a compact, which is then sintered at 410°C under normal pressure in a hydrogen atmosphere. did. In addition, the powder to be sintered is -
Tellurium powder was used which was pulverized to have a mesh size of 60mesh and a -325mhsh ratio of approximately 40%. In addition, among the physical property values, bending strength is based on the Carbon Society standards.
Measured according to JCAS-10-1968-44, density ratio is
Measurements and evaluations were made in accordance with JISZ2500-319.
【表】
表−１から判るように、この発明に係るターゲ
ツト板は、従来の方法により焼結したターゲツト
板に比べて、成形圧で１／３と低いにもかかわら
ず曲げ強さは20倍以上となつており、かつ密度比
においても同等以上の値が得られている。
なおターゲツト板の原料としては、テルル粉末
に限らずテルル合金の粉末も用いられる。
以上説明したように、本発明に係るスパツタリ
ング用ターゲツト板は、テルルもしくはテルル合
金の粉末の加圧成形焼結によつて製造され、密度
比70〜90％で強い曲げ強さを有し、スパツタリン
グ時に急熱しても割れやガスの発生がなくスパツ
タリング作業を確実に行なえる効果がある。ま
た、焼結法であるので、溶製法に比して揮発ロス
が少なくてすむ利点がある。[Table] As can be seen from Table 1, the bending strength of the target plate according to the present invention is 20 times that of the target plate sintered by the conventional method, even though the molding pressure is 1/3 lower. In addition, the same or higher density ratio was obtained. Note that the raw material for the target plate is not limited to tellurium powder, but also tellurium alloy powder. As explained above, the sputtering target plate according to the present invention is manufactured by pressure molding and sintering of tellurium or tellurium alloy powder, has a density ratio of 70 to 90%, has high bending strength, and is suitable for sputtering. Even when heated rapidly, there is no cracking or generation of gas, making it possible to perform sputtering operations reliably. Furthermore, since it is a sintering method, it has the advantage of less volatilization loss compared to the melting method.
Claims (1)
したのち、加圧焼結して密度比を70〜90％の間に
調整したことを特徴とするスパツタリング用ター
ゲツト板。1. A target plate for sputtering, characterized in that tellurium or tellurium alloy powder is pressure-molded and then pressure-sintered to adjust the density ratio between 70 and 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23992383A JPS60131963A (en) | 1983-12-21 | 1983-12-21 | Target plate for sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23992383A JPS60131963A (en) | 1983-12-21 | 1983-12-21 | Target plate for sputtering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60131963A JPS60131963A (en) | 1985-07-13 |
| JPH0344145B2 true JPH0344145B2 (en) | 1991-07-05 |
Family
ID=17051853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23992383A Granted JPS60131963A (en) | 1983-12-21 | 1983-12-21 | Target plate for sputtering |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60131963A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6213569A (en) * | 1985-07-10 | 1987-01-22 | Mitsubishi Metal Corp | Sintered te or te alloy target for sputtering |
| JPS62148362A (en) * | 1985-12-24 | 1987-07-02 | 三菱マテリアル株式会社 | Manufacture of target material for sputtering |
| JPH0752527B2 (en) * | 1986-08-18 | 1995-06-05 | 松下電器産業株式会社 | Optical information recording / reproducing disk manufacturing method |
| JPS63143258A (en) * | 1986-12-05 | 1988-06-15 | Mitsubishi Metal Corp | Sputtering target |
| JP2725331B2 (en) * | 1988-12-23 | 1998-03-11 | 三菱マテリアル株式会社 | Target material manufacturing method |
-
1983
- 1983-12-21 JP JP23992383A patent/JPS60131963A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60131963A (en) | 1985-07-13 |
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