JP2002275561A - Gold or gold-alloy material for thin film deposition and its manufacturing method, and hearth ingot using the gold or gold alloy and its manufacturing method - Google Patents
Gold or gold-alloy material for thin film deposition and its manufacturing method, and hearth ingot using the gold or gold alloy and its manufacturing methodInfo
- Publication number
- JP2002275561A JP2002275561A JP2001070733A JP2001070733A JP2002275561A JP 2002275561 A JP2002275561 A JP 2002275561A JP 2001070733 A JP2001070733 A JP 2001070733A JP 2001070733 A JP2001070733 A JP 2001070733A JP 2002275561 A JP2002275561 A JP 2002275561A
- Authority
- JP
- Japan
- Prior art keywords
- gold
- hearth
- ingot
- melt
- less
- 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
Links
- 239000010931 gold Substances 0.000 title claims abstract description 122
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 98
- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910001020 Au alloy Inorganic materials 0.000 title claims abstract description 40
- 239000003353 gold alloy Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 238000000427 thin-film deposition Methods 0.000 title abstract 3
- 239000012535 impurity Substances 0.000 claims abstract description 44
- 238000007670 refining Methods 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 28
- 230000008018 melting Effects 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005266 casting Methods 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000010409 thin film Substances 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000000155 melt Substances 0.000 claims description 18
- 238000007738 vacuum evaporation Methods 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012768 molten material Substances 0.000 claims 1
- 238000004857 zone melting Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 18
- 239000010408 film Substances 0.000 description 13
- 238000004544 sputter deposition Methods 0.000 description 11
- 238000001771 vacuum deposition Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000000151 deposition Methods 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 5
- 229910001882 dioxygen Inorganic materials 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 229910052714 tellurium Inorganic materials 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 102100021503 ATP-binding cassette sub-family B member 6 Human genes 0.000 description 1
- 229910015363 Au—Sn Inorganic materials 0.000 description 1
- 101000677883 Homo sapiens ATP-binding cassette sub-family B member 6 Proteins 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、金又は金合金材料
及びその製造方法に関し、特に半導体製造における薄膜
形成プロセスに利用される真空蒸着やスパッタ法等で用
いられる金(Ａｕ)又は金合金材料及びその製造方法、並
びにハースインゴット及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gold or gold alloy material and a method for producing the same, and more particularly to a gold (Au) or gold alloy material used in a vacuum deposition or sputtering method used in a thin film forming process in semiconductor production. And a manufacturing method thereof, and a hearth ingot and a manufacturing method thereof.
【０００２】[0002]
【従来の技術】近年の半導体技術の進歩は目覚しく、光
半導体用デバイスのＡｕ配線幅は、当初１００μｍ程度
あったものが最近では数μｍになり、部分的には０．５
μｍ程度になっているものまである。また、パワートラ
ンジスター等の大電流デバイスにおいても、より効率の
よいデバイスにするため、ウェハーを部分的に研磨して
ウェハー厚みを２００μｍ程度にしているデバイスがあ
る。2. Description of the Related Art Recent advances in semiconductor technology have been remarkable, and the Au wiring width of an optical semiconductor device has been about 100 .mu.m initially, but has recently become several .mu.m.
Some are even down to about μm. In addition, even in a large current device such as a power transistor, there is a device in which a wafer is partially polished to reduce the thickness of the wafer to about 200 μm in order to make the device more efficient.
【０００３】このような状況下で、Ａｕ蒸着において従
来問題とならなかった１〜１０数ミクロンの欠陥、つま
りスプラッシュとか金ボールの発生が問題となってい
る。例えば、蒸着膜に雲形の波ができたり、１μｍ程度
のボール状の金が付着してしまう現象であり、蒸着肌を
悪くする。また、Ａｕスパッタの場合も、Ａｕ蒸着の場
合と同様に、スパッタ膜にボール状の金が付着するとい
う現象がある（この場合、異常放電を起こす）。Ａｕ蒸
着の場合に生じる現象の原因の大部分は、金材料中に含
まれる揮発性金属不純物やガス不純物が蒸着中に噴き出
して、スプラッシュとなったり、噴き出したガス成分と
蒸着中のＡｕ粒子とが衝突を起こし、Ａｕ粒子がエネル
ギーを失って金ボールが形成されるものであると考えら
れる。[0003] Under these circumstances, defects of 1 to several tens of microns, which have not been a problem in Au deposition, such as splashes and gold balls, have been a problem. For example, it is a phenomenon in which a cloud-like wave is formed on a deposited film, or a ball-shaped gold of about 1 μm adheres, and the deposited skin is deteriorated. Also, in the case of Au sputtering, similarly to the case of Au evaporation, there is a phenomenon that ball-shaped gold adheres to the sputtered film (in this case, abnormal discharge occurs). Most of the phenomena that occur in the case of Au deposition are caused by volatile metal impurities and gas impurities contained in the gold material squirting during the deposition, resulting in a splash or a scattered gas component and the Au particles during the deposition. Is considered to cause collision and Au particles lose energy to form a gold ball.
【０００４】なお、従来の金材料は、Ａｕ自体を大気中
で溶解しても酸化という問題が生じないため、大気溶解
品又は１Ｐａ程度の真空溶解品であり、不純物を１重量
ｐｐｍ以上含んでおり、その材料表面は必ずしも平滑で
はなかった。Conventional gold materials do not cause oxidation even if Au itself is dissolved in the atmosphere. Therefore, the gold material is an air-dissolved product or a vacuum-dissolved product of about 1 Pa, and contains impurities of 1 ppm by weight or more. And the material surface was not always smooth.
【０００５】[0005]
【発明が解決しようとする課題】上記したように、蒸着
膜、スパッタ膜の表面におけるスプラッシュ、金ボール
の形成という現象は、金又は金合金材料に含まれる揮発
性金属不純物及びガス不純物により生じると共に、金又
は金合金材料の表面に付着した金属不純物及びガス不純
物によっても生じるものである。As described above, the phenomena of the splash and the formation of the gold ball on the surface of the deposited film and the sputtered film are caused by volatile metal impurities and gas impurities contained in the gold or gold alloy material. And metal impurities and gas impurities attached to the surface of gold or gold alloy materials.
【０００６】本発明は、上記従来技術の問題点を解決す
るものであり、内部に含まれる不純物及び外表面に付着
する不純物を最小限にした金又は金合金材料及びその製
造方法、並びにハースインゴット及びその製造方法を提
供することを課題とする。SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems of the prior art, in which a gold or gold alloy material minimizing impurities contained inside and impurities adhering to an outer surface, a method of manufacturing the same, and a hearth ingot are provided. And a method for manufacturing the same.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、Ａｕ蒸着
やＡｕスパッタ中に発生するスプラッシュや金ボールが
金又は金合金材料中の揮発性金属不純物やガス不純物に
起因することから、これら不純物を減少せしめればよい
ことに気が付き、また、インゴット等の金材料のミクロ
な表面積を小さくすることにより、金又は金合金材料表
面の付着ガスを最小限にすることができることから、例
えばインゴットの中央部を盛り上げる形状にし、かつ機
械加工面の無い平滑な鋳肌とすればよいことに気が付
き、本発明を完成するに至った。SUMMARY OF THE INVENTION The inventors of the present invention have determined that the splash or gold ball generated during Au deposition or Au sputtering is caused by volatile metal impurities or gas impurities in the gold or gold alloy material. It is noticed that impurities should be reduced, and by reducing the microscopic surface area of a gold material such as an ingot, the amount of gas adhering to the gold or gold alloy material surface can be minimized. The present inventors have realized that the shape should be such that the central portion is raised, and that a smooth cast surface having no machined surface is sufficient, and the present invention has been completed.
【０００８】本発明の薄膜形成用金又は金合金材料は、
４Ｎ（９９．９９％）以上の純度を有する金からなり、
金の比率がモル比で５０％を超えているものである。こ
の金又は金合金材料は、揮発性金属不純物の含有量が１
重量ｐｐｍ以下、水素及び窒素の含有量が１重量ｐｐｍ
以下、並びに酸素の含有量が５重量ｐｐｍ以下である。
金又は金合金材料中の揮発性金属不純物及びガス不純物
がこのような範囲を外れると、得られた材料を用いて真
空蒸着やスパッタ法などで薄膜を形成する際にスプラッ
シュや金ボールが発生するが、この範囲内であるとその
ような現象は生じない。[0008] The gold or gold alloy material for forming a thin film of the present invention comprises:
Made of gold having a purity of 4N (99.99%) or more,
The ratio of gold exceeds 50% by mole. This gold or gold alloy material has a volatile metal impurity content of 1
Weight ppm or less, hydrogen and nitrogen content is 1 weight ppm
Or less, and the oxygen content is 5 ppm by weight or less.
If the volatile metal impurities and gas impurities in the gold or gold alloy material are out of such a range, a splash or a gold ball is generated when a thin film is formed using the obtained material by vacuum evaporation or sputtering. However, if it is within this range, such a phenomenon does not occur.
【０００９】本発明の薄膜形成用金又は金合金材料は、
４Ｎ以上の純度を有する金を、ゾーンメルト精製法によ
って溶融精製することにより製造される。この製造方法
において、ゾーンメルト精製法による溶融精製を１×１
０-3Ｐａ以下の高真空中で行い、次いで成形体を作製す
る場合は、該溶融精製により得られた金材料を容器に入
れて加熱溶解し、その後、該容器の底面のみからこの溶
解物を冷却して、成形体を得ることが好ましい。また、
この製造方法において、ゾーンメルト精製法による溶融
精製により得られた金材料を容器に入れて１×１０-3Ｐ
ａ以下の高真空中で加熱溶解し、その後、該容器の底面
のみからこの溶解物を冷却して、成形体を得ることが好
ましい。ゾーンメルト精製法を利用し、かつ高真空中で
加熱溶解して金又は金合金材料を製造することにより、
揮発性金属不純物及びガス不純物の含有量が極めて少な
い金又は金合金材料が得られる。さらに、本発明の薄膜
形成用金合金材料の製造方法において、ゾーンメルト精
製法による溶融精製により得られた金材料と、４Ｎ以上
の純度を有し、１×１０-3Ｐａ以下の高真空中で真空溶
解された合金用材料とを、金の比率がモル比で５０％を
超える割合で容器に入れて１×１０-3Ｐａ以下の高真空
中で加熱溶解し、その後、該容器の底面のみからこの溶
解物を冷却して、成形体を得ることが好ましい。The gold or gold alloy material for forming a thin film of the present invention comprises:
It is produced by melting and refining gold having a purity of 4N or more by a zone melt refining method. In this production method, the melting and refining by the zone melt refining method is performed 1 × 1
In the case of performing in a high vacuum of 0 −3 Pa or less and then producing a molded body, the gold material obtained by the melting and refining is placed in a container and heated and melted. Is cooled to obtain a molded body. Also,
In this production method, a gold material obtained by melt refining by a zone melt refining method is put into a container, and 1 × 10 −3 P
It is preferable to heat and dissolve in a high vacuum of a or less, and then cool the melt from only the bottom of the container to obtain a molded body. By using zone-melt refining method and heating and melting in high vacuum to produce gold or gold alloy material,
A gold or gold alloy material having a very low content of volatile metal impurities and gas impurities is obtained. Further, in the method for producing a gold alloy material for forming a thin film according to the present invention, the gold material obtained by melting and refining by the zone melt refining method may have a purity of 4N or more and a high vacuum of 1 × 10 −3 Pa or less. The alloy material vacuum-melted in the above is put into a container at a molar ratio of gold exceeding 50% and heated and melted in a high vacuum of 1 × 10 −3 Pa or less. It is preferable to cool the melt from only the above to obtain a molded body.
【００１０】また、本発明のハースインゴットは、４Ｎ
以上の純度を有する金からなる金の比率がモル比で５０
％を超える金又は金合金からなり、揮発性金属不純物、
水素及び窒素の含有量が１重量ｐｐｍ以下であり、酸素
の含有量が５重量ｐｐｍ以下である真空蒸着用ハースイ
ンゴットであって、その表面積をできるだけ少なくする
ために、その上表面の鋳肌の少なくとも一部が平滑な溶
解表面からなっている。このハースインゴットはまた、
その上表面の中央部が上表面の端部よりも盛り上がって
いる形状を有しているものであることが好ましい。上記
範囲内の揮発性金属不純物及びガス不純物を含むハース
インゴットの表面形状をこのようにすることにより、イ
ンゴットの表面にガス不純物の付着がなくなると共に、
蒸着やスパッタ中にスプラッシュや金ボールの発生がな
くなる。Further, the Haas ingot of the present invention has a 4N
The ratio of gold consisting of gold having the above purity is 50 by mole ratio.
% Of gold or gold alloy, volatile metal impurities,
A hearth ingot for vacuum evaporation having a hydrogen and nitrogen content of 1 wt ppm or less and an oxygen content of 5 wt ppm or less, and in order to reduce the surface area as much as possible, At least a part consists of a smooth dissolution surface. This Haas ingot also
It is preferable that the central part of the upper surface has a shape that is higher than the end of the upper surface. By making the surface shape of the hearth ingot containing the volatile metal impurities and the gas impurities in the above range in this manner, gas impurities are not attached to the surface of the ingot,
Splashes and gold balls are not generated during vapor deposition or sputtering.
【００１１】本発明によるハースインゴットの製造方法
は、４Ｎ以上の純度を有する金を、ゾーンメルト精製法
によって溶融精製することにより製造される。この製造
方法において、ゾーンメルト精製法による溶融精製を１
×１０-3Ｐａ以下の高真空中で行い、該溶融精製により
得られた金材料をハース形状の容器に入れて加熱溶解
し、その後、該容器の底面のみからこの溶解物を冷却
し、ハース形状のインゴットを得るものである。また、
この製造方法において、前記溶融精製により得られた金
材料をハース形状の容器に入れて１×１０-3Ｐａ以下の
高真空中で加熱溶解し、その後、該容器の底面のみから
この溶解物を冷却し、ハース形状のインゴットを得るこ
とができ、さらに、前記溶融精製により得られた金材料
と、４Ｎ以上の純度を有し、１×１０-3Ｐａ以下の高真
空中で真空溶解された合金用材料とを、金の比率がモル
比で５０％を超える割合でハース形状の容器に入れて１
×１０ -3Ｐａ以下の高真空中で加熱溶解し、その後、該
容器の底面のみからこの溶解物を冷却して、ハース形状
のインゴットを得ることができる。[0011] A method of manufacturing a hearth ingot according to the present invention.
Uses zone melt refining method for gold having a purity of 4N or more.
It is manufactured by melting and refining. This manufacturing
The method comprises the steps of:
× 10-3Performed in a high vacuum of Pa or less,
Put the obtained gold material in a hearth-shaped container and heat and melt
Then, cool the melt only from the bottom of the container.
Then, a hearth-shaped ingot is obtained. Also,
In this production method, the gold obtained by the melt refining is used.
Put the material in a hearth-shaped container-3Pa or less
Heat and dissolve in a high vacuum, then only from the bottom of the container
The melt is cooled to obtain a hearth-shaped ingot.
And the gold material obtained by the above-mentioned melting and refining.
Having a purity of 4N or more and 1 × 10-3High true below Pa
The alloy material vacuum-melted in the air is
In a hearth-shaped container at a ratio exceeding 50%
× 10 -3Heat and dissolve in a high vacuum of Pa or less.
Cool the melt from only the bottom of the container to form a hearth
Can be obtained.
【００１２】このようにして得られたインゴットは、そ
の上表面の鋳肌の少なくとも一部が平滑な溶解表面から
なっており、かつ、該上表面の中央部が上表面の端部よ
りも盛り上がっている形状を有する。ゾーンメルト精製
法を利用し、かつ高真空中で加熱溶解することにより、
揮発性金属不純物及びガス不純物の含有量が極めて少な
いインゴットが得られる。In the ingot thus obtained, at least a part of the casting surface on the upper surface is formed of a smooth dissolution surface, and the central portion of the upper surface rises more than the end of the upper surface. It has a shape. By using zone melt purification method and heating and melting in high vacuum,
An ingot having a very low content of volatile metal impurities and gas impurities is obtained.
【００１３】[0013]
【発明の実施の形態】本発明によれば、金又は金合金材
料中の揮発性金属不純物やガス不純物を減少せしめるこ
とにより、また、インゴット等の金又は金合金材料のミ
クロな表面積を少なくすること、例えばインゴットの中
央を盛り上げる形状で機械加工面の無い平滑な鋳肌とし
て金又は金合金材料表面の付着ガスを最小限にすること
により、このような金材料を用いて、半導体製造におけ
る薄膜形成プロセスに利用される真空蒸着やスパッタ法
を行う場合、蒸着やスパッタ中に薄膜表面上にスプラッ
シュや金ボールが発生することもなく、また、薄膜表面
にガス不純物が付着することもなく、良質なＡｕ薄膜が
得られる。According to the present invention, the volatile metal impurities and gas impurities in a gold or gold alloy material are reduced, and the micro surface area of a gold or gold alloy material such as an ingot is reduced. That, for example, by using such a gold material to minimize the gas adhering to the surface of the gold or gold alloy material as a smooth casting surface without a machined surface in a shape that raises the center of the ingot, thin films in semiconductor manufacturing When performing vacuum deposition or sputtering used in the formation process, there is no splash or gold ball generated on the thin film surface during deposition or sputtering, and no gas impurities adhere to the thin film surface, and high quality An Au thin film can be obtained.
【００１４】本発明の金又は金合金材料中に含まれる不
揮発性金属不純物やガス不純物には、金の原材料として
の金鉱石の種類や精錬方法等に応じてその種類や量は異
なるが、一般に、周期表Iａ族の金属としてＬｉ、Ｎ
ａ、Ｋ、周期表IIａ族の金属としてＢｅ、Ｍｇ、Ｃａ、
周期表Ｖａ族の金属としてＰ、Ａｓ、Ｓｂ、周期表IIａ
族の金属としてＳ、Ｓｅ、Ｔｅ等があり、また、水素ガ
ス、窒素ガス、酸素ガス等がある。The types and amounts of the non-volatile metal impurities and gas impurities contained in the gold or gold alloy material of the present invention vary depending on the type of gold ore as a raw material of gold, the refining method, and the like. Li, N as metals of group Ia of the periodic table
a, K, Be, Mg, Ca, as metals of group IIa of the periodic table;
P, As, Sb, Periodic Table IIa
Group metals include S, Se, Te and the like, and also include hydrogen gas, nitrogen gas, oxygen gas and the like.
【００１５】本発明の金又は金合金材料の形状は特に制
限されるものではないが、例えばインゴット、ペレッ
ト、ショット、ワイヤー、ロッド、ターゲット形状等が
好ましい。Although the shape of the gold or gold alloy material of the present invention is not particularly limited, for example, ingots, pellets, shots, wires, rods, target shapes and the like are preferable.
【００１６】本発明によれば、ゾーンメルト精製法を利
用して棒状の金材料を作製し、この材料中の揮発性金属
不純物やガス不純物の含有量を所定の量以下にし、この
棒状材料をるつぼ等の容器内に入れ、１×１０-3Ｐａ以
下の高真空中で所定の時間加熱溶解し、次いで固化物中
に空洞が生じないようにこの溶解物を冷却し、上記した
ような所望の形状に成形し、これを用いて真空蒸着、ス
パッタを行い、所望の薄膜を形成できる。また、ゾーン
メルト精製法を利用し、かつ１×１０-3Ｐａ以下の高真
空中で加熱溶解して棒状の金材料を製造し、この材料中
の揮発性金属不純物及びガス不純物の含有量を所定の量
以下にし、これを用いて真空蒸着、スパッタを行い、所
望の薄膜を形成できる。あるいはまた、上記のようにし
て作製された棒状の金材料を加熱溶融してインゴット等
を製造し、これを用いて蒸着膜を形成してもよい。According to the present invention, a rod-shaped gold material is prepared by using a zone melt refining method, and the content of volatile metal impurities and gas impurities in the material is reduced to a predetermined amount or less. Put in a container such as a crucible and heat-dissolve in a high vacuum of 1 × 10 −3 Pa or less for a predetermined time, and then cool the melt so that no voids are formed in the solidified product. , And vacuum deposition and sputtering are performed using this to form a desired thin film. Further, using a zone melt refining method, and heating and melting in a high vacuum of 1 × 10 −3 Pa or less to produce a rod-shaped gold material, the content of volatile metal impurities and gas impurities in this material was determined. The amount is set to a predetermined amount or less, and a desired thin film can be formed by performing vacuum deposition and sputtering using the amount. Alternatively, the rod-shaped gold material produced as described above may be heated and melted to produce an ingot or the like, and this may be used to form a deposited film.
【００１７】本発明では、単なる従来の真空溶解方法で
はなく、上記不純物が、完全に揮発するような時間、高
真空中で溶融することが必要である。In the present invention, it is necessary to dissolve the impurities in a high vacuum for such a time as to completely volatilize the impurities, rather than merely a conventional vacuum melting method.
【００１８】このようにして得られた金又は金合金材
料、例えばハースインゴットの場合は、その上表面の鋳
肌の少なくとも一部が平滑な溶解表面からなっており、
かつ該上表面の中央部が上表面の端部よりも盛り上がっ
ている形状を有する。ゾーンメルト精製法を利用し、ま
た、高真空中で加熱溶解して金材料を製造することによ
り、揮発性金属不純物及びガス不純物の含有量が極めて
少ないインゴットが得られる。In the case of the gold or gold alloy material thus obtained, for example, a hearth ingot, at least a part of the casting surface on the upper surface thereof has a smooth melting surface,
In addition, the upper surface has a shape in which the central portion is higher than the end portion of the upper surface. By making use of the zone melt refining method and heating and melting in a high vacuum to produce a gold material, an ingot having extremely low contents of volatile metal impurities and gas impurities can be obtained.
【００１９】本発明によれば、４Ｎ（９９．９９％）以
上の純度を有する金を原材料とし、揮発性の金属である
Ｉａ族、IIａ族、Ｖａ族、及びVIａ族の不純物含有量
が、各々１重量ｐｐｍ以下であり、水素ガス、窒素ガス
の含有量が各々１重量ｐｐｍ以下であり、また酸素ガス
の含有量が５重量ｐｐｍ以下である金又は金合金材料を
作り、溶融状態から固体すなわちインゴット、ペレッ
ト、ショット、ワイヤー、ターゲット形状に成型時に空
洞（いわゆる「ス」）ができないように冷却、成形す
る。According to the present invention, gold having a purity of 4N (99.99%) or more is used as a raw material, and volatile metals Ia, IIa, Va, and VIa have an impurity content of: Each gold or gold alloy material is 1 ppm by weight or less, the content of hydrogen gas and nitrogen gas is 1 ppm by weight or less, and the content of oxygen gas is 5 ppm by weight or less. That is, cooling and molding are performed so that cavities (so-called “s”) are not formed during molding into ingots, pellets, shots, wires, and target shapes.
【００２０】[0020]
【実施例】以下、本発明の実施例を図１を参照して説明
する。 （実施例１）Ｅ／Ｂ蒸着用のハース形状のＡｕインゴッ
トを以下のようにして作製した。An embodiment of the present invention will be described below with reference to FIG. (Example 1) A hearth-shaped Au ingot for E / B evaporation was produced as follows.
【００２１】４Ｎの純度を有する金を使用し、ゾーンメ
ルト精製方法に従って溶融精製を行い、棒状の材料を作
り、次いでこの棒状材料をＥ／Ｂ蒸着用のハース形状の
るつぼに入れ、１×１０-3Ｐａ以下の高真空中にて、５
時間かけて加熱溶解した。溶解後、るつぼの底面のみか
らこの溶解物を冷却し、Ｅ／Ｂ蒸着用のハース形状イン
ゴットを得た。このように、溶解物の底面からのみ冷却
したので、得られた成形体中には空洞が生じていなかっ
た。上記精製方法で精製されたインゴット中の不純物
は、Ｌｉ、Ｎａ、Ｋ、Ｂｅ、Ｍｇ、Ｃａ、Ｐ、Ａｓ、Ｓ
ｂ、Ｓ、Ｓｅ、Ｔｅの各々の含有量が１重量ｐｐｍ以下
であった。また、水素、窒素ガスの含有量が各々１重量
ｐｐｍ以下であり、また、酸素ガスの含有量が５重量ｐ
ｐｍ以下であった。Using gold having a purity of 4N, melting and refining are carried out according to a zone melt refining method to produce a rod-shaped material. 5 in a high vacuum of -3 Pa or less
The mixture was heated and dissolved over time. After melting, the melt was cooled only from the bottom of the crucible to obtain a hearth-shaped ingot for E / B evaporation. As described above, since cooling was performed only from the bottom surface of the melt, no cavity was formed in the obtained molded body. The impurities in the ingot purified by the above-described purification method include Li, Na, K, Be, Mg, Ca, P, As, and S.
The content of each of b, S, Se, and Te was 1 ppm by weight or less. Further, the content of hydrogen and nitrogen gas is 1 wt ppm or less, respectively, and the content of oxygen gas is 5 wt p
pm or less.
【００２２】上記のようにして得られた金材料を使用し
て公知の条件で真空蒸着を行い、Ａｕ薄膜を基板上に形
成したところ、スプラッシュが生じることなく、また、
蒸着膜表面にボール状の金の発生も見いだせなかった。Using the gold material obtained as described above, vacuum deposition was performed under known conditions to form an Au thin film on the substrate.
No generation of ball-shaped gold was found on the surface of the deposited film.
【００２３】また、このハースインゴットの上表面の鋳
肌は平滑な溶解表面からなっており、その表面積は小さ
かった。このハースインゴットは、図１に示すように、
その上表面の中央部１が上表面の端部２よりも盛り上が
っている形状を有していた。 （実施例２）電解精製して得た１０ｍｍφ×１０００ｍ
ｍＬのロッド形状の金材料を、１×１０-3Ｐａ以下の高
真空中で、ゾーンメルト精製方法に従い、８時間かけて
溶融精製した。かくして得られた金材料中の不純物は、
Ｌｉ、Ｎａ、Ｋ、Ｂｅ、Ｍｇ、Ｃａ、Ｐ、Ａｓ、Ｓｂ、
Ｓ、Ｓｅ、Ｔｅの各々の含有量が１重量ｐｐｍ以下であ
った。また、ゾーンメルトという特殊溶解であったの
で、水素、窒素ガスの含有量が各々１重量ｐｐｍ以下、
及び酸素ガスの含有量が５重量ｐｐｍ以下であった。The cast surface on the upper surface of this hearth ingot was a smooth dissolution surface, and its surface area was small. This hearth ingot, as shown in FIG.
The central portion 1 of the upper surface had a shape that was higher than the end 2 of the upper surface. (Example 2) 10 mmφ × 1000 m obtained by electrolytic purification
The mL rod-shaped gold material was melt-refined for 8 hours in a high vacuum of 1 × 10 −3 Pa or less according to a zone melt purification method. The impurities in the gold material thus obtained are:
Li, Na, K, Be, Mg, Ca, P, As, Sb,
The content of each of S, Se, and Te was 1 ppm by weight or less. In addition, since it was a special dissolution called zone melt, the contents of hydrogen and nitrogen gas were 1 ppm by weight or less, respectively.
And the content of oxygen gas was 5 ppm by weight or less.
【００２４】次いで、上記のようにして得られた金材料
を使用して公知の条件で真空蒸着を行い、基板上にＡｕ
薄膜を形成したところ、スプラッシュが生じることな
く、また、蒸着膜表面にボール状の金の発生も見いだせ
なかった。Next, vacuum deposition is carried out under the known conditions using the gold material obtained as described above, and Au is deposited on the substrate.
When a thin film was formed, no splash was generated, and no generation of ball-shaped gold was found on the surface of the deposited film.
【００２５】さらに、上記のようにして得られた金材料
を使用して１×１０-4Ｐａの条件で、ハースインゴット
を作製し、これを用いて同様に真空蒸着を行ったとこ
ろ、上記と同様の結果が得られた。 （実施例３）Ｅ／Ｂ蒸着用のハース形状のＡｕ−Ｓｎイ
ンゴットを以下のように作製した。Further, a hearth ingot was manufactured under the conditions of 1 × 10 −4 Pa using the gold material obtained as described above, and vacuum evaporation was similarly performed using the hearth ingot. Similar results were obtained. (Example 3) A heart-shaped Au-Sn ingot for E / B evaporation was produced as follows.
【００２６】Ｓｎ原料として、４Ｎの純度を有する市販
のＳｎを用いた。この原料は、酸素ガス含有量が非常に
多いため、合金を製造する前に、予め真空溶解によりス
ラグを除去した。この時の真空度を１×１０-4Ｐａとし
た。次いで、同様の真空度で、Ａｕ８０ｇとＳｎ２０ｇ
とを真空誘導加熱で溶解して、実施例１に準じてハース
インゴットを製作した。As a Sn raw material, commercially available Sn having a purity of 4N was used. Since this material has a very high oxygen gas content, slag was previously removed by vacuum melting before producing an alloy. The degree of vacuum at this time was 1 × 10 −4 Pa. Then, at the same degree of vacuum, Au 80 g and Sn 20 g
Were melted by vacuum induction heating to produce a hearth ingot according to Example 1.
【００２７】このようにして製作した金合金インゴット
と、従来技術による大気溶解インゴットとを用いて、公
知の条件で真空蒸着を行い、両者の特性比較を行った。
その結果、大気溶解インゴットを使用した場合は、蒸着
前の溶融状態で、表面にスラグが浮出し、このスラグを
ＥＢで飛ばすだけで３〜４分かかった（約４０ｇ消
失）。また、その後の２分間の蒸着では、蒸着膜に直径
１０μｍ以上のボールが４０ヶ以上付着していた。しか
し、本発明による真空溶解インゴットを使用した場合
は、溶融時に、表面へのスラグの浮出しは無く、直ぐに
２分間の蒸着ができた。得られた蒸着膜の表面にボール
の付着は無かった。Using the gold alloy ingot manufactured as described above and the atmospheric melting ingot according to the prior art, vacuum deposition was performed under known conditions, and the characteristics of the two were compared.
As a result, when the air-melted ingot was used, slag emerged on the surface in a molten state before vapor deposition, and it took 3 to 4 minutes just to fly the slag by EB (approximately 40 g disappeared). In the subsequent two-minute vapor deposition, 40 or more balls having a diameter of 10 μm or more adhered to the vapor-deposited film. However, when the vacuum melting ingot according to the present invention was used, there was no slag floating on the surface at the time of melting, and deposition could be immediately performed for 2 minutes. No ball adhered to the surface of the obtained deposited film.
【００２８】[0028]
【発明の効果】本発明の金又は金合金材料によれば、半
導体製造における薄膜形成プロセスに利用される真空蒸
着及びスパッタによるＡｕ成膜において、スプラッシュ
や金ボールの発生という問題が解決され、良質なＡｕ薄
膜を形成することが出来る。この金又は金合金材料の製
造方法によれば、上記真空蒸着及びスパッタによるＡｕ
成膜において、スプラッシュや金ボールの発生という問
題もなく、良質なＡｕ薄膜を形成することのできる金又
は金合金材料が提供され得る。According to the gold or gold alloy material of the present invention, the problem of generation of splash and gold ball is solved in the Au film formation by vacuum evaporation and sputtering used in the thin film formation process in semiconductor production, and the quality is improved. A thin Au thin film can be formed. According to this method for producing a gold or gold alloy material, Au by vacuum deposition and sputtering is used.
It is possible to provide a gold or gold alloy material capable of forming a high-quality Au thin film without a problem of generation of a splash or a gold ball in film formation.
【００２９】本発明のハースインゴットによれば、これ
を用いて行う上記真空蒸着によるＡｕ成膜において、ス
プラッシュや金ボールの発生という問題が解決され、良
質なＡｕ薄膜を形成することが出来る。このハースイン
ゴットの製造方法によれば、上記真空蒸着によるＡｕ成
膜において、スプラッシュや金ボールの発生という問題
もなく、良質なＡｕ薄膜を形成することのできる金又は
金合金材料が提供され得る。According to the hearth ingot of the present invention, the problem of generation of splash and gold ball is solved in the Au film formation by the above-mentioned vacuum deposition performed using the hearth ingot, and a high quality Au thin film can be formed. According to the method of manufacturing the hearth ingot, it is possible to provide a gold or gold alloy material capable of forming a high-quality Au thin film without a problem of generation of a splash or a gold ball in the Au film formation by the vacuum evaporation.
【図１】 本発明のハースインゴットの外観形状を示す
斜視図。FIG. 1 is a perspective view showing an external shape of a hearth ingot of the present invention.
１ 表面の中央部 ２ 表面の端部 1 Central part of surface 2 Edge of surface
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｂ 11/02 Ｃ２２Ｂ 11/02 Ｃ２２Ｃ 1/02 ５０１ Ｃ２２Ｃ 1/02 ５０１Ｚ ５０３ ５０３Ａ (72)発明者 大場 彰 鹿児島県姶良郡横川町上ノ3313 ユーマッ ト株式会社九州工場内 (72)発明者 南 明 福岡県福岡市博多区東光２−１−13 アル バック九州株式会社内 Ｆターム(参考） 4K001 AA04 BA23 EA02 EA05 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme court ゛ (Reference) C22B 11/02 C22B 11/02 C22C 1/02 501 C22C 1/02 501Z 503 503A (72) Inventor Akira Oba 3313 Kamino, Yokokawa-cho, Aira-gun, Kagoshima Prefecture Inside the Kyushu Plant of Umat Corporation (72) Inventor Minami Akira 2-1-13 Toko, Hakata-ku, Fukuoka City, Fukuoka F-Term (reference) 4K001 AA04 BA23 EA02 EA05
Claims (11)
の比率がモル比で５０％を超える金又は金合金であっ
て、揮発性金属不純物の含有量が１重量ｐｐｍ以下、水
素及び窒素の含有量が１重量ｐｐｍ以下、並びに酸素の
含有量が５重量ｐｐｍ以下であることを特徴とする薄膜
形成用金又は金合金材料。1. A gold or gold alloy comprising gold having a purity of 4N or more and a gold ratio of more than 50% by mole, wherein the content of volatile metal impurities is 1% by weight or less, hydrogen and nitrogen A gold or gold alloy material for forming a thin film, characterized by having a content of 1 ppm by weight or less and a content of oxygen of 5 ppm by weight or less.
ルト精製法によって溶融精製し、請求項１記載の薄膜形
成用金又は金合金材料を得ることを特徴とする薄膜形成
用金又は金合金材料の製造方法。2. A gold or gold alloy for forming a thin film, wherein gold having a purity of 4N or more is melt-refined by a zone melt refining method to obtain the gold or gold alloy material for forming a thin film according to claim 1. Material manufacturing method.
真空中で行い、次いで成形体を作製する場合は、該溶融
精製により得られた金材料を容器に入れて加熱溶解し、
その後、該容器の底面のみからこの溶解物を冷却して、
成形体を得ることを特徴とする請求項２記載の薄膜形成
用金又は金合金材料の製造方法。3. The melting and refining is performed in a high vacuum of 1 × 10 −3 Pa or less, and then, when a molded body is produced, the gold material obtained by the melting and refining is put into a container and heated and melted.
Thereafter, the melt is cooled only from the bottom of the container,
3. The method for producing a gold or gold alloy material for forming a thin film according to claim 2, wherein a molded body is obtained.
器に入れて１×１０ -3Ｐａ以下の高真空中で加熱溶解
し、その後、該容器の底面のみからこの溶解物を冷却し
て、成形体を得ることを特徴とする請求項２記載の薄膜
形成用金又は金合金材料の製造方法。4. The method according to claim 1, wherein the gold material obtained by the melt purification is contained.
1 × 10 in a bowl -3Heat melting in high vacuum below Pa
And then cool the melt only from the bottom of the container.
3. A thin film according to claim 2, wherein
Manufacturing method of forming gold or gold alloy material.
４Ｎ以上の純度を有し、１×１０-3Ｐａ以下の高真空中
で真空溶解された合金用材料とを、金の比率がモル比で
５０％を超える割合で容器に入れて１×１０-3Ｐａ以下
の高真空中で加熱溶解し、その後、該容器の底面のみか
らこの溶解物を冷却して、成形体を得ることを特徴とす
る請求項２記載の薄膜形成用金合金材料の製造方法。5. A gold material obtained by the melting and refining,
An alloy material having a purity of 4N or more and vacuum-melted in a high vacuum of 1 × 10 −3 Pa or less is charged into a container at a ratio of gold exceeding 50% by mole, and 1 × 10 3 The thin film-forming gold alloy material according to claim 2, wherein the molten material is heated and melted in a high vacuum of -3 Pa or less, and then the melt is cooled only from the bottom of the container to obtain a molded body. Production method.
比率がモル比で５０％を超える金又は金合金からなり、
揮発性金属不純物、水素及び窒素の含有量が１重量ｐｐ
ｍ以下であり、酸素の含有量が５重量ｐｐｍ以下である
真空蒸着用ハースインゴットであって、その上表面の鋳
肌の少なくとも一部が平滑な溶解表面からなっているこ
とを特徴とするハースインゴット。6. A gold or gold alloy in which the ratio of gold consisting of gold having a purity of 4N or more exceeds 50% by mole,
Content of volatile metal impurities, hydrogen and nitrogen is 1 weight pp
m or less, and a hearth ingot for vacuum evaporation having an oxygen content of 5 wt ppm or less, wherein at least a part of a casting surface on an upper surface thereof is formed of a smooth dissolution surface. ingot.
中央部が上表面の端部よりも盛り上がっている形状を有
することを特徴とする請求項６記載のハースインゴッ
ト。7. The hearth ingot according to claim 6, wherein the hearth ingot has a shape in which a central portion of an upper surface is raised from an end of the upper surface.
ルト精製法によって溶融精製し、請求項６又は７記載の
ハースインゴットを得ることを特徴とするハースインゴ
ットの製造方法。8. A method for producing a hearth ingot, wherein gold having a purity of 4N or more is melt-refined by a zone melt refining method to obtain a hearth ingot according to claim 6 or 7.
真空中で行い、該溶融精製により得られた金材料をハー
ス形状の容器に入れて加熱溶解し、その後、該容器の底
面のみからこの溶解物を冷却して、ハース形状のインゴ
ットを得ることを特徴とする請求項８記載のハースイン
ゴットの製造方法。9. The melting and refining is performed in a high vacuum of 1 × 10 −3 Pa or less, and the gold material obtained by the melting and refining is put into a hearth-shaped container and melted by heating. 9. The method for producing a hearth ingot according to claim 8, wherein the melt is cooled only from the melt to obtain a hearth-shaped ingot.
ハース形状の容器に入れて１×１０-3Ｐａ以下の高真空
中で加熱溶解し、その後、該容器の底面のみからこの溶
解物を冷却して、ハース形状のインゴットを得ることを
特徴とする請求項８記載のハースインゴットの製造方
法。10. The gold material obtained by the melting and refining is placed in a hearth-shaped container and heated and melted in a high vacuum of 1 × 10 −3 Pa or less, and then the melt is removed only from the bottom of the container. The method for manufacturing a hearth ingot according to claim 8, wherein the hearth-shaped ingot is obtained by cooling.
と、４Ｎ以上の純度を有し、１×１０-3Ｐａ以下の高真
空中で真空溶解された合金用材料とを、金の比率がモル
比で５０％を超える割合でハース形状の容器に入れて１
×１０-3Ｐａ以下の高真空中で加熱溶解し、その後、該
容器の底面のみからこの溶解物を冷却して、ハース形状
のインゴットを得ることを特徴とする請求項８記載のハ
ースインゴットの製造方法。11. The gold material obtained by the melting and refining and an alloy material having a purity of 4N or more and vacuum-melted in a high vacuum of 1 × 10 −3 Pa or less have a gold ratio of Put in a hearth-shaped container at a molar ratio exceeding 50%
The hearth ingot according to claim 8, wherein the melt is heated and melted in a high vacuum of 10-3 Pa or less, and then the melt is cooled only from the bottom of the container to obtain a hearth-shaped ingot. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP2001070733A JP5097890B2 (en) | 2001-03-13 | 2001-03-13 | Method for producing gold or gold alloy for vacuum deposition or sputtering, and method for producing hearth ingot |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001070733A JP5097890B2 (en) | 2001-03-13 | 2001-03-13 | Method for producing gold or gold alloy for vacuum deposition or sputtering, and method for producing hearth ingot |
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| Publication Number | Publication Date |
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| JP2002275561A true JP2002275561A (en) | 2002-09-25 |
| JP5097890B2 JP5097890B2 (en) | 2012-12-12 |
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| JP2021091922A (en) * | 2019-12-06 | 2021-06-17 | 松田産業株式会社 | Vapor deposition material and method for manufacturing the same |
| JP6896966B1 (en) * | 2020-10-01 | 2021-06-30 | 松田産業株式会社 | Gold vapor deposition material |
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| JP7499370B1 (en) | 2023-03-13 | 2024-06-13 | 松田産業株式会社 | Precious metal deposition materials |
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