JPH03199380A - Method for forming organometallic compound into metallic film - Google Patents
Method for forming organometallic compound into metallic filmInfo
- Publication number
- JPH03199380A JPH03199380A JP33946189A JP33946189A JPH03199380A JP H03199380 A JPH03199380 A JP H03199380A JP 33946189 A JP33946189 A JP 33946189A JP 33946189 A JP33946189 A JP 33946189A JP H03199380 A JPH03199380 A JP H03199380A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- organometallic compound
- plasma
- compd
- metal film
- 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
- 238000000034 method Methods 0.000 title claims description 19
- 150000002902 organometallic compounds Chemical class 0.000 title claims description 17
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000009832 plasma treatment Methods 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 9
- 239000010953 base metal Substances 0.000 claims abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- 238000010304 firing Methods 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000003085 diluting agent Substances 0.000 abstract description 2
- 125000002524 organometallic group Chemical group 0.000 abstract 4
- 238000000354 decomposition reaction Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910052737 gold Inorganic materials 0.000 description 14
- 239000010931 gold Substances 0.000 description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 12
- 239000005416 organic matter Substances 0.000 description 9
- 229910052697 platinum Inorganic materials 0.000 description 7
- 150000002894 organic compounds Chemical class 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- -1 gold organic compound Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
Landscapes
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は、有機金属化合物から金属膜を生成させる方法
に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Application Field) The present invention relates to a method of producing a metal film from an organometallic compound.
（従来の技術）
有機金属化合物から金属膜を生成させるためには、金属
と有機物との結合を断ち、さらに有機物を除去する必要
がある。(Prior Art) In order to generate a metal film from an organometallic compound, it is necessary to break the bond between the metal and the organic substance and further remove the organic substance.
このため、それに応じて必要なエネルギーを与えてやら
ねばならない。このエネルギーとしては、熱が利用され
ており、金属膜を生成させるためには高温環境が不可欠
とされている。Therefore, the necessary energy must be given accordingly. Heat is used as this energy, and a high-temperature environment is considered essential for producing a metal film.
たとえば、金、あるいは白金の有機化合物から金膜ある
いは白金膜を得るには、空気中、あるいは酸素雰囲気中
で［ｉ００〜８００℃で焼成する。For example, in order to obtain a gold film or a platinum film from gold or an organic compound of platinum, the film is fired at a temperature of 00 to 800° C. in air or in an oxygen atmosphere.
また、チタン、タンタル、シリコンあるいはアルミニウ
ムの有機化合物から、それぞれの金属膜を得るには、酸
素を含む窒素雰囲気中で、８ｏｏ〜１０００℃で焼成す
る。Further, in order to obtain each metal film from an organic compound of titanium, tantalum, silicon, or aluminum, firing is performed at 80° C. to 1000° C. in a nitrogen atmosphere containing oxygen.
このような条件下で、金属膜の形成を行っている。The metal film is formed under such conditions.
（発明が角ダ決しようとする課題）
ところで、このような有機金属化合物の金属膜化を、広
く電子デバイスの分野に応用しようとすると、これまで
の温度条件は苛酷であり、様々な欠陥を生じさせる原因
となっている。(Problem to be solved by the invention) By the way, if we try to widely apply the formation of organometallic compounds into metal films in the field of electronic devices, the temperature conditions up until now have been harsh and various defects have occurred. It is the cause of this.
特に、ＩＣ分野における小型、高密度化の進展はめざま
しく、それにつれて高精度、高信頼性が要求されている
。In particular, advances in miniaturization and higher density in the IC field are remarkable, and higher precision and higher reliability are required accordingly.
ところが、８００℃から１０００℃にもなる高温環境下
にＩＣ部品をさらした場合、アルミニウムの融点である
６６０℃を超えてしまうため、アルミニウムを含んだ部
品には金属膜形成が適用できなかったり、金属膜を形成
してもＩＣの耐熱性の域を超えたために品質を劣化させ
てしまうという問題がある。However, when IC parts are exposed to a high temperature environment of 800°C to 1000°C, the melting point of aluminum, 660°C, is exceeded, so metal film formation cannot be applied to parts containing aluminum. Even if a metal film is formed, there is a problem that the heat resistance of the IC is exceeded and the quality deteriorates.
したがって、金属膜を形成しようとする被処理体に損傷
を与えず、より穏やかな条件で金属膜を形成する方法が
望まれている。Therefore, a method of forming a metal film under milder conditions without damaging the object to be processed on which the metal film is to be formed is desired.
本発明はこのような課題を解決するためになされたもの
で、穏やかな低温条件で金属膜を形成することのできる
、有機金属化合物の金属膜化方法を堤供することを１」
的とする。The present invention has been made in order to solve these problems, and aims to provide a method for forming a metal film from an organometallic compound, which can form a metal film under mild, low-temperature conditions.
target
［発明の構成］
（課題を解決するための手段）
本発明の有機金属化合物の金属膜化方法は、基体上に配
置された有機金属化合物を、空気中あるいは酸素雰囲気
中で加熱し、前記有機金属化合物を分解させる焼成工程
と、この焼成工程を経た焼成基体をプラズマにさらし、
前記基体上に金属膜を生成させるプラズマ処理工程とを
有することを特徴としている。[Structure of the Invention] (Means for Solving the Problems) The method of forming a metal film from an organometallic compound of the present invention heats the organometallic compound disposed on a substrate in air or an oxygen atmosphere, and A firing process to decompose the metal compound, and exposing the fired substrate that has undergone this firing process to plasma,
The method is characterized by comprising a plasma treatment step of generating a metal film on the substrate.
本発明において、金、白金等の貴金属の有機化合物から
金膜、白金膜を生成しようとする場合、まず、°金、白
金等の貴金属の有機化合物を必要に応じて稀釈剤で薄め
、基板等に塗布する。In the present invention, when attempting to produce a gold film or a platinum film from an organic compound of a noble metal such as gold or platinum, first dilute the organic compound of a noble metal such as gold or platinum with a diluent as necessary, and then Apply to.
次に、空気中あるいは酸素雰囲気中で、２００〜４００
℃で焼成する。この段階では、有機物は完全に分解除去
されず残存する。Next, in air or oxygen atmosphere, 200 to 400
Bake at ℃. At this stage, organic substances remain without being completely decomposed and removed.
この残存している有機物を分解、除去するために、上記
焼成物を酸素をｏ、ｏｔ−ｔｏ％含有する不活性ガス雰
囲気中のプラズマにさらす。In order to decompose and remove the remaining organic matter, the fired product is exposed to plasma in an inert gas atmosphere containing 0,000% of oxygen.
このとき、酸素含有量が０．０１％より低いと酸素活性
種が少なすぎるために、有機物の分解、除去は効果的に
行われない。１０％より高いと、ｎ°機物の分解、除去
に必要とされている“穏やかな酸化反応”の域を超えて
しまうため、被処理体に損傷を与えるおそれが生じる。At this time, if the oxygen content is lower than 0.01%, there are too few oxygen active species, so that the organic matter cannot be effectively decomposed or removed. If it is higher than 10%, the "mild oxidation reaction" required for decomposing and removing the n°organic material will be exceeded, and there is a risk of damaging the object to be processed.
一方、チタン、タンタル、シリコン、アルミニウム等の
卑金属の有機化合物から、それぞれの卑金属膜を生成し
ようとする場合、空気中あるいは酸素雰囲気中で２００
〜４００℃で焼成を行う工程は貴金属の場合と同様であ
る。On the other hand, when attempting to produce base metal films from organic compounds of base metals such as titanium, tantalum, silicon, and aluminum, it is necessary to
The process of firing at ~400°C is the same as for noble metals.
しかし、卑金属は酸素との親和性が強いことから、この
焼成工程において金属酸化膜が形成されるため、プラズ
マ処理工程における雰囲気は、アンモニア等還元性を有
するガスの１ｇ１、あるいは２８以上の混合ガスとする
。However, since base metals have a strong affinity for oxygen, a metal oxide film is formed during this firing process, so the atmosphere during the plasma treatment process must be 1g1 of a reducing gas such as ammonia, or a mixture of 28 or more gases. shall be.
還１元性ガス活性種の働きで、２００〜４００℃という
低温条件にもかかわらず、金属酸化膜は還元され、よっ
て、所望する卑金属膜を生成させることができる。Due to the action of the reducing gas active species, the metal oxide film is reduced despite the low temperature conditions of 200 to 400°C, and therefore a desired base metal film can be produced.
本発明におけるプラズマ処理は、雰囲気圧力を０．３〜
Ｂ、０Ｔｏｒｒの範囲とすることが好ましい。In the plasma treatment in the present invention, the atmospheric pressure is 0.3~
B, preferably in the range of 0 Torr.
０．３Ｔｏｒｒ以下とすると、不純物ガスの混入の割合
が大きくなり、６．０Ｔｏｒｒを超えると放電が不安定
になりやすい。より好ましいのは、０．３〜４．０Ｔｏ
ｒｒ程度の雰囲気圧力である。When it is 0.3 Torr or less, the proportion of impurity gas mixed in increases, and when it exceeds 6.0 Torr, the discharge tends to become unstable. More preferably 0.3 to 4.0To
The atmospheric pressure is about rr.
プラズマを発生、持続させる高周波放電の失効電力は好
ましくは０．１〜３ＫＷの範囲である。The expiration power of the high frequency discharge for generating and sustaining plasma is preferably in the range of 0.1 to 3 KW.
０．１ＫＷより小さいと金属膜化に要する時間が長くな
りすぎるし、３ＫＷより大きいと高エネルギー荷電粒子
の衝撃によって、膜表面が損傷を受ける場合が生じる。If it is less than 0.1 KW, the time required to form a metal film will be too long, and if it is more than 3 KW, the film surface may be damaged by the impact of high-energy charged particles.
さらに、本発明において、金属膜の批抗値の低減、ある
いは貴金属導電膜を形成する際のコスト低減のために、
銀の粉末を、焼成前の有機金属化合物に、その中の金属
に対して原子量比で０．１〜２０倍混合させることが有
効である。Furthermore, in the present invention, in order to reduce the resistance value of the metal film or reduce the cost when forming the noble metal conductive film,
It is effective to mix silver powder into the organometallic compound before firing in an atomic weight ratio of 0.1 to 20 times the amount of the metal contained therein.
原子量比が、０．１より小さいと、抵抗値、コストとも
に、Ｈ意義な低減効果が得られず、原子量比が２０より
大きいと生成された膜の表面の平滑性、密着性が劣化し
てくる。If the atomic weight ratio is smaller than 0.1, no significant H reduction effect can be obtained in both resistance value and cost, and if the atomic weight ratio is larger than 20, the surface smoothness and adhesion of the produced film will deteriorate. come.
（作 用）
本発明では、プラズマによって活性種を造り出し、その
作用をもって、金属と有機物との結合を断ち、有機物を
除去するためのエネルギーとして利用している。(Function) In the present invention, active species are created by plasma, and this action is used as energy to break the bond between metal and organic matter and remove the organic matter.
このため、エネルギーとして供給すべき熱が低減され、
２００〜４００℃という低温条件にもかかわらず、金、
白金等の有機化合物から、金膜、白金膜が生成されるの
である。Therefore, the amount of heat that should be supplied as energy is reduced,
Despite the low temperature conditions of 200-400℃, gold,
Gold films and platinum films are produced from organic compounds such as platinum.
（実施例） 次に本発明の実施例について説明する。(Example) Next, examples of the present invention will be described.
実施例１
はじめに、金を５重量％含をする金の−ａ機化合物をア
ルミナ基板上にデイツプ法によって塗布した。Example 1 First, a gold -a compound containing 5% by weight of gold was coated onto an alumina substrate by a dip method.
次に、この基板を、空気中、２５０℃で１時間焼成した
。Next, this substrate was baked at 250° C. for 1 hour in air.
この後、焼成したＵ板に対して２．０Ｔｏｒｒのアルゴ
ンガス中、２５０℃、１時間のプラズマ処理を施し、ア
ルミナ基板上に金膜を形成した。このときの高周波出力
は １．２ＫＷとした。Thereafter, the fired U-plate was subjected to plasma treatment at 250° C. for 1 hour in argon gas at 2.0 Torr to form a gold film on the alumina substrate. The high frequency output at this time was 1.2KW.
金膜形成後の有機物の残存量、および金属膜の密着性を
調べた結果、有機物はほぼ除去されており、金膜の密着
性も極めて良好であった。As a result of examining the amount of organic matter remaining after the gold film was formed and the adhesion of the metal film, it was found that almost all the organic matter had been removed, and the adhesion of the gold film was also extremely good.
この結果を、以下に述べる比較例の結果と併せて第１表
に示す。The results are shown in Table 1 together with the results of comparative examples described below.
比較例１〜２
実施例１で使用した金の有機化合物をアルミナ基板上に
デイツプ法によって塗布した。Comparative Examples 1 and 2 The gold organic compound used in Example 1 was applied onto an alumina substrate by a dip method.
次に、この基板を、空気中、２５０℃でｌ特間、および
２時間の条件で、それぞれ焼成した。Next, this substrate was fired in air at 250° C. for 2 hours.
この後、有機物の残存量、および金属膜の形成状態を調
べた。これらの結果を第１表に示す。After this, the amount of remaining organic matter and the state of formation of the metal film were examined. These results are shown in Table 1.
比較例３〜４
実施例１で使用した金の有機化合物をアルミナ基板上に
デイツプ法によって塗布した。Comparative Examples 3 to 4 The gold organic compound used in Example 1 was applied onto an alumina substrate by a dip method.
次に、この址板を、２．０Ｔｏｒｒのアルゴンガス中、
２５０℃、１時間および２時間の条件で、それぞれプラ
ズマ処理を施した。Next, this base plate was placed in argon gas at 2.0 Torr.
Plasma treatment was performed at 250° C. for 1 hour and 2 hours, respectively.
この後、有機物の残存量、および金属膜の形成状態を調
べた。これらの結果を第１表に示す。After this, the amount of remaining organic matter and the state of formation of the metal film were examined. These results are shown in Table 1.
（以下余白）
第 １
表
第１表から明らかなように、焼成処理のみ、またはプラ
ズマ処理のみの比較例では、有機物がかなりの量で残在
しているのに対し、焼成とプラズマ処理とを施した実施
例では、極めて良好に金属膜が形成されていた。(Leaving space below) Table 1 As is clear from Table 1, in the comparative examples with only calcination treatment or only plasma treatment, a considerable amount of organic matter remained, whereas when calcination and plasma treatment were In the examples given, the metal film was formed extremely well.
実施例２
チタンを１０重量％含有するチタンの有機化合物を、ア
ルミナ延板上にデイツプ法によって塗布した。Example 2 A titanium organic compound containing 10% by weight of titanium was applied onto an alumina rolled plate by a dip method.
次いで、空気中、４００℃で１時間焼成し、得られた焼
成基板を、２．０Ｔｏｒｒのアンモニアガス雰囲気中、
２８０℃、１時間の条件でプラズマ中にさらした。Next, the fired substrate was fired at 400° C. for 1 hour in air, and the fired substrate was heated in an ammonia gas atmosphere at 2.0 Torr.
It was exposed to plasma at 280°C for 1 hour.
その結果、焼成直後は白包の絶縁膜であったものが、プ
ラズマ処理後は灰色で光沢性のある導電膜となった。As a result, what was a white insulating film immediately after firing became a gray, glossy conductive film after plasma treatment.
この導電膜のＸ線回折の結果、チタンに相当するシャー
プなピークが認められた。As a result of X-ray diffraction of this conductive film, a sharp peak corresponding to titanium was observed.
このように、プラズマ処理を用いた本発明の方法により
、４００℃以下の低温条件においても、有機金属化合物
の金属膜化を可能にすることができた。As described above, the method of the present invention using plasma treatment made it possible to form an organometallic compound into a metal film even under low temperature conditions of 400° C. or lower.
なお、上述した金属以外の金属についても、本発明によ
るプラズマ処理を適用して活性種を造り出すことにより
、低温条件で有機金属化合物から金属膜を生成させるこ
とができる。Note that even for metals other than the metals mentioned above, by applying the plasma treatment according to the present invention to create active species, a metal film can be generated from an organometallic compound under low-temperature conditions.
［発明の効果］
以上説明したように、本発゛明の有機金属化合物の金属
膜化方法は、不活性ガス雰囲気あるいは、還元性ガス雰
囲気においてプラズマ処理を行うことにより、活性種の
働きを熱エネルギーの替わるエネルギー源として利用し
、低温条件における有機金属化合物の金属膜化を実現さ
せることができる。[Effects of the Invention] As explained above, the method of forming a metal film from an organometallic compound of the present invention heats the action of active species by performing plasma treatment in an inert gas atmosphere or a reducing gas atmosphere. It can be used as an alternative energy source to form metal films from organometallic compounds under low-temperature conditions.
Claims (2)
るいは酸素雰囲気中で加熱し、前記有機金属化合物を分
解させる焼成工程と、 この焼成工程を経た焼成基体をプラズマにさらし、前記
基体上に金属膜を生成させるプラズマ処理工程と を有することを特徴とする有機金属化合物の金属膜化方
法。(1) A firing step in which the organometallic compound placed on the substrate is heated in air or an oxygen atmosphere to decompose the organometallic compound; and the fired substrate that has undergone this baking step is exposed to plasma to 1. A method for forming a metal film from an organometallic compound, comprising: a plasma treatment step for forming a metal film.
る温度は、ともに２００〜４００℃の範囲であり、 前記プラズマ処理における雰囲気は、前記有機金属化合
物が貴金属の場合は不活性ガス雰囲気とし、前記有機金
属化合物が卑金属の場合は還元性ガス雰囲気とする 請求項１記載の有機金属化合物の金属膜化方法。(2) The temperature in the firing step and the plasma treatment step are both in the range of 200 to 400°C, and the atmosphere in the plasma treatment is an inert gas atmosphere when the organometallic compound is a noble metal; 2. The method for forming a metal film from an organometallic compound according to claim 1, wherein when the compound is a base metal, a reducing gas atmosphere is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33946189A JPH03199380A (en) | 1989-12-27 | 1989-12-27 | Method for forming organometallic compound into metallic film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33946189A JPH03199380A (en) | 1989-12-27 | 1989-12-27 | Method for forming organometallic compound into metallic film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03199380A true JPH03199380A (en) | 1991-08-30 |
Family
ID=18327689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33946189A Pending JPH03199380A (en) | 1989-12-27 | 1989-12-27 | Method for forming organometallic compound into metallic film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03199380A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999008803A3 (en) * | 1997-08-18 | 1999-04-15 | Agfa Gevaert Nv | Method for forming a metallic film using non-isothermal plasma |
-
1989
- 1989-12-27 JP JP33946189A patent/JPH03199380A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999008803A3 (en) * | 1997-08-18 | 1999-04-15 | Agfa Gevaert Nv | Method for forming a metallic film using non-isothermal plasma |
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