JPH0645893B2 - Method of forming thin film - Google Patents
Method of forming thin filmInfo
- Publication number
- JPH0645893B2 JPH0645893B2 JP1036125A JP3612589A JPH0645893B2 JP H0645893 B2 JPH0645893 B2 JP H0645893B2 JP 1036125 A JP1036125 A JP 1036125A JP 3612589 A JP3612589 A JP 3612589A JP H0645893 B2 JPH0645893 B2 JP H0645893B2
- Authority
- JP
- Japan
- Prior art keywords
- forming
- thin film
- light
- film
- substrate
- 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 - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 54
- 239000010409 thin film Substances 0.000 title claims description 32
- 239000010408 film Substances 0.000 claims description 84
- 239000000758 substrate Substances 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 28
- 238000005229 chemical vapour deposition Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000003054 catalyst Substances 0.000 claims description 17
- 238000010884 ion-beam technique Methods 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 230000001678 irradiating effect Effects 0.000 claims description 11
- 230000003197 catalytic effect Effects 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 2
- 239000001257 hydrogen Substances 0.000 claims 2
- 229910052739 hydrogen Inorganic materials 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 28
- 150000002500 ions Chemical class 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000010494 dissociation reaction Methods 0.000 description 8
- 230000005593 dissociations Effects 0.000 description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001182 laser chemical vapour deposition Methods 0.000 description 3
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000006557 surface reaction Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、化学的気相成長法による薄膜の形成方法に関
する。The present invention relates to a method for forming a thin film by a chemical vapor deposition method.
化学的気相成長（ＣＶＤ）法は、原料ガスと基板表面か
らなる系に対して何らかの形でエネルギーを供給するこ
とで化学反応を進行させ、基板上に膜を形成する技術で
あり、各種半導体装置の製造プロセスにおいて、半導体
膜、絶縁膜、金属膜の形成に利用されている。半導体装
置の形造プロセスに多く用いられている減圧ＣＶＤ法で
は、反応律速の温度範囲を用いるのが一般的であり、量
産性に優れており、大口径のウェーハに均一性良く膜を
形成することができる。The chemical vapor deposition (CVD) method is a technique for forming a film on a substrate by causing a chemical reaction to proceed by supplying energy to a system composed of a raw material gas and a substrate surface in some form. It is used to form a semiconductor film, an insulating film, and a metal film in a device manufacturing process. In the low pressure CVD method that is often used in the shaping process of semiconductor devices, a temperature range of reaction rate control is generally used, mass productivity is excellent, and a film is formed on a large-diameter wafer with good uniformity. be able to.
減圧ＣＶＤ法で表面反応が律速となるような場合には基
板の種類による選択性が表れることがある。その代表的
な例が高融点金属材料であるＷをWF6とH2を原料ガスに
用いて形成する場合であり、「ジャーナル オブ エレ
クトロケミカル ソサイアティ ヴォリューム １３
１，ナンバー６（１９８４），第１４２７頁から第１４
３３頁（Journal of Electrochemical Soc.１３１
（６），１４２７（１９８４））」において詳しく論じ
られている。この系ではＨ原子によるWF6の還元反応を
起こす必要があるが、H2分子の解離がＳｉや金属の表面
でしか起こらないため、それらの上にのみ選択的に膜形
成が生じる。この現象は半導体装置のコンタクトやスル
ーホールにのみＷを埋め込む技術として期待されてい
る。In the case where the surface reaction is rate-determining in the low pressure CVD method, the selectivity may appear depending on the type of substrate. A typical example thereof is the case where W, which is a refractory metal material, is formed by using WF 6 and H 2 as source gases. “Journal of Electrochemical Society Volume 13
1, Number 6 (1984), pages 1427 to 14
Page 33 (Journal of Electrochemical Soc. 131
(6), 1427 (1984)) ”. In this system, it is necessary to cause a reduction reaction of WF 6 by H atoms, but since dissociation of H 2 molecules occurs only on the surface of Si or a metal, film formation occurs selectively only on them. This phenomenon is expected as a technique for embedding W only in the contacts and through holes of a semiconductor device.
しかし、この方法ではＷ膜を配線材料としてSiO2やSi3N
4といった絶縁膜上に形成することが困難であるという
欠点がある。温度を７００℃以上にすれば気相中で還元
反応が起こりSiO2上にＷが降り積もって膜が形成される
が、極めて基板との接着性が低く、膜自体のストレスで
簡単に剥がれてしまう。However, in this method, the W film is used as a wiring material for SiO 2 and Si 3 N.
There is a drawback that it is difficult to form on the insulating film such as 4 . If the temperature is set to 700 ° C or higher, a reduction reaction occurs in the gas phase and W accumulates on SiO 2 to form a film, but the adhesiveness to the substrate is extremely low and the film itself easily peels off. .
SiO2上にＷ膜をＣＶＤ法で形成する一手段としてレーザ
ＣＶＤ法があり、「第２０回固体素子材料コンファレン
ス予稿集第８９頁から第９２頁」において報告されてい
る。この方法によれば、気相中でエキシマレーザ光を吸
収したWF6とH2が反応してＷ原子が生成され、Ｓｉ基板
上と同程度の４００℃前後の低い基板温度でSiO2上にス
トレスの小さいＷ膜を形成できる。There is a laser CVD method as one means for forming a W film on SiO 2 by the CVD method, and it is reported in “Twenty-Seventh Solid Element Material Conference Proceedings, pages 89 to 92”. According to this method, WF 6 and H 2 that have absorbed the excimer laser light react in the gas phase to generate W atoms, and W atoms are generated on SiO 2 at a low substrate temperature of about 400 ° C., which is similar to that on Si substrates. A W film with low stress can be formed.
また、SiO2表面にＳｉをイオン打ち込みした後、表面を
エッチングしてＳｉを表面に露出させそのＳｉによりWF
6を還元することでSiO2上にＷ膜を形成可能なことが、
「ジャーナル オブ エレクトロケミカル ソサイアテ
ィ ヴォリューム １３５，ナンバー７（１９８８），
第１７３０頁から第１７３４頁（Journal of Electroch
emical Soc.１３５（７），１７３０（１９８８））」
で報告されている。Also, after Si is ion-implanted on the SiO 2 surface, the surface is etched to expose Si on the surface, and the Si causes WF
It is possible to form a W film on SiO 2 by reducing 6
"Journal of Electrochemical Society Volume 135, No. 7 (1988),
1730 to 1734 (Journal of Electroch
emical Soc. 135 (7), 1730 (1988)) "
Has been reported in.
レーザＣＶＤ法では、気相反応を利用しているため形成
されたＷ膜とSiO2の接着性は低く、高温でのアニールを
行わなくては接着性は改善されないという問題点が残っ
ている。The laser CVD method has a problem that the adhesion between the W film formed and SiO 2 is low because the vapor phase reaction is used, and the adhesion cannot be improved without annealing at a high temperature.
Ｓｉのイオン打ち込みを利用した方法では１０17／cm2
程度のドーズ量を加速電圧２５keVで打ち込む必要があ
り、スループットの向上が難しい。また、一旦打ち込ん
だＳｉをSiO2表面に露出させるためのエッチングが必要
で、工程数が増加する。本発明の目的は、上記のような
問題を解決し、SiO2上にＷ膜を形成する実用的な方法を
提供することにある。10 17 / cm 2 by the method using Si ion implantation
Since it is necessary to drive a dose amount of about 25 keV, it is difficult to improve throughput. Further, etching is required to expose the once-implanted Si to the surface of SiO 2 , which increases the number of steps. An object of the present invention is to solve the above problems and provide a practical method for forming a W film on SiO 2 .
本発明では上記の課題を、触媒反応を利用して解決し
た。触媒物質あるいはその化合物を反応容器内に気体，
液体あるいは固体の形態で導入することができる。また
膜形成前、あるいは膜形成中に基板表面に中性ビーム、
あるいはイオンビームの形態で照射しても良い。場合に
よっては、触媒あるいはその化合物の中性ビーム、ある
いはイオンビームを膜形成中に基板表面に直接照射され
ないように雰囲気中に照射しても良い。ここでは以下、
Ｗ膜をSiO2上に形成するためにH2分子の解離触媒である
Ｔｉを用いた場合について詳細に説明する。The present invention has solved the above-mentioned problems by utilizing a catalytic reaction. The catalytic substance or its compound is put in a gas in the reaction vessel,
It can be introduced in liquid or solid form. In addition, before or during film formation, a neutral beam on the substrate surface,
Alternatively, the irradiation may be performed in the form of an ion beam. In some cases, the neutral beam or the ion beam of the catalyst or its compound may be irradiated in the atmosphere so that the substrate surface is not directly irradiated during the film formation. Here below
The case where Ti, which is a dissociation catalyst for H 2 molecules, is used to form the W film on SiO 2 will be described in detail.
減圧ＣＶＤ法でＷ膜を形成する際の原料ガスはWF6とH2
であり、Ｗ原子を生成するためにＨ原子でWF6を還元す
る必要がある。しかし、H2分子が低温で解離するために
は金属表面が必要である。Ｓｉ上のＷ膜形成の場合、最
初にWF6のＳｉによる還元反応で薄いＷ膜が形成される
ので、引き続いて起こるＷ上でのH2の解離吸着によって
生成した水素原子によってWF6が還元され厚いＷ膜がＳ
ｉ上に形成される。このような反応はSiO2上では起こら
ないために、Ｓｉ上にのみ選択的にＷ膜が形成されるこ
とになる。The source gases for forming the W film by the low pressure CVD method are WF 6 and H 2
Therefore, it is necessary to reduce WF 6 with H atoms in order to generate W atoms. However, a metal surface is required for H 2 molecules to dissociate at low temperatures. In the case of forming a W film on Si, a thin W film is first formed by the reduction reaction of WF 6 with Si. Therefore, WF 6 is reduced by hydrogen atoms generated by the subsequent dissociative adsorption of H 2 on W. Thick W film is S
formed on i. Since such a reaction does not occur on SiO 2 , the W film is selectively formed only on Si.
本発明ではH2分子を解離する触媒を用いてＨ原子を生成
することで、SiO2上にＷ膜を形成する。多くの遷移金属
はH2分子の解離触媒として働くが、その一例としてＴｉ
を用いる。例えば薄いＴｉ膜をSiO2上に薄く形成してお
けば、H2分子がＴｉ表面に解離吸着し生成されたＨ原子
がWF6を還元するのでSiO2上にもＷ膜を形成することが
できる。一旦Ｗ膜が形成されれば、Ｗ膜上でのH2分子の
解離により厚いＷ膜が形成される。Ｔｉは触媒として働
き、H2分子を解離する際に消費されないので、Ｔｉ膜の
厚さは極めて薄くてよく、例えば一原子層程度（ドーズ
量に換算して１０15／cm2程度）でも良い。このため、
Ｔｉ膜の形成手段としてＴｉ、あるいはその化合物の中
性ビームあるいは低エネルギー（１ｋｅＶ以下）イオン
ビームのSiO2表面への照射を用いることができる。In the present invention, a W film is formed on SiO 2 by generating H atoms using a catalyst that dissociates H 2 molecules. Many transition metals act as a dissociation catalyst for H 2 molecules, one example of which is Ti
To use. For example, if a thin Ti film is thinly formed on SiO 2 , H 2 molecules are dissociatively adsorbed on the Ti surface and the generated H atoms reduce WF 6 , so that a W film can be formed on SiO 2. it can. Once the W film is formed, a thick W film is formed by the dissociation of H 2 molecules on the W film. Since Ti acts as a catalyst and is not consumed when dissociating H 2 molecules, the thickness of the Ti film may be extremely thin, for example, about one atomic layer (about 10 15 / cm 2 in terms of dose amount). . For this reason,
Irradiation of a neutral beam of Ti or a compound thereof or a low energy (1 keV or less) ion beam onto the SiO 2 surface can be used as a means for forming the Ti film.
イオンビームを用いることの大きな利点は、マスクを通
して照射することでSiO2上の一部にのみ触媒であるＴｉ
膜を選択形成できる点である。反応容器内の原料ガスの
圧力や基板の温度を、表面反応が優勢に生じる条件にし
ておけば、イオン照射を行った部分にのみ選択的にＷ膜
を形成できる。さらに、液体金属イオン源を用いた収束
イオンビームを利用すれば、サブミクロンの配線パター
ンを本発明の方法で形成することができる。The great advantage of using an ion beam is that irradiation with a mask causes Ti to be a catalyst only on a part of SiO 2.
The point is that the film can be selectively formed. If the pressure of the source gas in the reaction vessel and the temperature of the substrate are set to the conditions in which the surface reaction predominantly occurs, the W film can be selectively formed only in the portion irradiated with ions. Furthermore, by using a focused ion beam using a liquid metal ion source, a submicron wiring pattern can be formed by the method of the present invention.
また、Ｔｉの薄膜を形成する手法として、真空蒸着ある
いはスパッタリング法を用いることもできる。Further, as a method for forming a Ti thin film, vacuum vapor deposition or sputtering can be used.
WF6とH2を原料ガスに用い、Ｔｉの触媒作用を利用してS
iO2上にＷ膜を形成する際、膜形成の初期の段階で基板
に光を照射することが有効である。Ｆ系の原料ガスを用
いているので温度や圧力といったＣＶＤの条件によって
は、膜形成よりもエッチングの方が優勢に起ってしまう
ことがある。そのような場合、気相中あるいは基板表面
に吸着した原料ガス分子に吸収される波長の光を照射す
ることで、膜形成反応を優勢に起こすことができる。WF 6 and H 2 are used as source gases, and the catalytic action of Ti is used to produce S
When forming a W film on iO 2 , it is effective to irradiate the substrate with light at an early stage of film formation. Since the F-based source gas is used, etching may occur more predominantly than film formation depending on the CVD conditions such as temperature and pressure. In such a case, the film forming reaction can be predominantly caused by irradiating with light having a wavelength absorbed by the source gas molecules adsorbed in the gas phase or on the substrate surface.
以上の説明はWF6とH2を原料ガスに用いたＣＶＤ法にお
いて、Ｔｉを用いればSiO2にＷ膜を形成できるというも
のであった。一般的に、低温における半導体や絶縁膜の
形成速度を向上させるためにいろいろな触媒を利用する
ことも考えられる。The above explanation was that in the CVD method using WF 6 and H 2 as source gases, a W film can be formed on SiO 2 by using Ti. In general, it is possible to use various catalysts in order to improve the formation rate of semiconductors and insulating films at low temperatures.
触媒は化学反応の経路を替え活性化エネルギーを低下さ
せることができる。その結果、従来のＣＶＤ法では形成
できなかった基板と膜の組合せを実現できるほか、種々
の半導体や絶縁膜の低温における形成速度を向上させる
ことができる。The catalyst can change the pathway of the chemical reaction and reduce the activation energy. As a result, it is possible to realize a combination of a substrate and a film that cannot be formed by the conventional CVD method, and it is possible to improve the formation rate of various semiconductors and insulating films at low temperatures.
本発明の実施例に用いた装置の概略を第１図に示す。全
体は、反応容器８，光源５，イオン源１２の三つの部分
から構成されている。An outline of the apparatus used in the examples of the present invention is shown in FIG. The whole is composed of three parts of a reaction container 8, a light source 5 and an ion source 12.
〈実施例１〉 本実施例は、SiO2膜上にH2の解離吸着触媒であるＴｉの
薄い層をイオンビーム照射を用いて形成し、その上で形
成されたＨ原子によりWF6を還元することによりＷ膜をS
iO2上に形成させるものである。Example 1 In this example, a thin layer of Ti, which is a dissociative adsorption catalyst for H 2 , is formed on a SiO 2 film by using ion beam irradiation, and WF 6 is reduced by H atoms formed thereon. The W film to S
It is formed on iO 2 .
まず表面に厚さ１００ｎｍのSiO2膜を熱酸化によって形
成したＳｉの基板１０を反応容器８内の試料台を兼ねた
ヒータ９上に設置して１０-5Ｐａまで高真空排気系１４
により排気した後、イオン源１２との間のゲートバルブ
１１を開き、Ｔｉイオンビームを照射して基板１０のSi
O2表面全体に一原子層程度のＴｉ膜を形成した。この
際、Ｔｉイオンビームの原料ガスには原料ガス供給系１
３からのTiCl4を用い、加速電圧は１keV以下とした。低
い加速電圧を用いることにより、ＴｉがSiO2内に打ち込
まれないようにした。First, a Si substrate 10 on the surface of which a 100 nm thick SiO 2 film is formed by thermal oxidation is placed on a heater 9 in the reaction container 8 which also serves as a sample stage, and a high vacuum exhaust system 14 up to 10 −5 Pa is provided.
After evacuating by, the gate valve 11 with the ion source 12 is opened, and the Ti ion beam is irradiated to irradiate the Si of the substrate 10.
A Ti film of about one atomic layer was formed on the entire surface of O 2 . At this time, the raw material gas supply system 1 is used for the raw material gas of the Ti ion beam.
Using TiCl 4 from No. 3, the accelerating voltage was set to 1 keV or less. A low accelerating voltage was used to prevent Ti from being implanted in SiO 2 .
次に、ゲートバルブ１１を閉じて反応容器８側の排気系
を低真空排気系１５に切り替えた後、Ｗ膜形成用の原料
ガスWF6とH2を原料ガス供給系１より反応容器８内に導
入してSiO2表面にＷ膜を形成した。この時の基板温度は
３００℃、WF6とH2の流量比は１：１００で全圧は0.2To
orとした。Next, after closing the gate valve 11 and switching the exhaust system on the side of the reaction vessel 8 to the low vacuum exhaust system 15, the source gases WF 6 and H 2 for forming the W film are supplied from the source gas supply system 1 into the reaction vessel 8. Then, a W film was formed on the surface of SiO 2 . At this time, the substrate temperature is 300 ° C., the flow rate ratio of WF 6 and H 2 is 1: 100, and the total pressure is 0.2To.
or
本実施例におけるＴｉの役割は〔課題を解決するための
手段〕の項で説明したとおりである。形成されたＷ膜を
オージェ電子分光分析法と二次イオン質量分析法で評価
した結果、単位面積あたりに換算して約１０15個／cm2
のＴｉが検出された。これは、一原子層に大体対応して
おり、Ｔｉが膜形成中に失われておらず、触媒として働
いたことが確認された。The role of Ti in this example is as described in the section [Means for solving the problem]. The formed W film was evaluated by Auger electron spectroscopy and secondary ion mass spectrometry, and as a result, it was converted into about 10 15 pieces / cm 2 per unit area.
Ti was detected. This roughly corresponds to one atomic layer, and it was confirmed that Ti was not lost during film formation and worked as a catalyst.
本実施例で明らかになったように、H2分子の解離触媒で
あるＴｉを用いることにより気相反応が生じないような
低温でＷ膜をSiO2上に形成することができた。本方法で
形成した膜は基板との接着性が良好で、厚さ５μｍのＷ
膜を形成しても剥離することがなかった。As is clear from this example, by using Ti, which is a dissociation catalyst for H 2 molecules, it was possible to form a W film on SiO 2 at a low temperature at which a gas phase reaction does not occur. The film formed by this method has good adhesion to the substrate and has a thickness of 5 μm.
Even if a film was formed, it did not peel off.
またイオン照射の後基板８を光源５の方向に回転させて
おいて、ＣＶＤ中に光源５より波長１９３ｎｍのＡｒＦ
エキシマレーザ光６を光学系４によりそのビーム径を拡
大して、このビーム径を拡大されたレーザ光７を基板１
０の表面に垂直に照射したところ、Ｗ膜の形成速度を一
桁程度速くすることができた。尚、レーザ光照射中はパ
ージガス供給系２よりＡｒガスを光導入用窓３の近傍に
導入して、窓内面に反応生成物が付着することを防い
だ。After the ion irradiation, the substrate 8 is rotated in the direction of the light source 5, and during the CVD, the ArF having a wavelength of 193 nm is emitted from the light source 5.
The beam diameter of the excimer laser light 6 is expanded by the optical system 4, and the laser light 7 with the expanded beam diameter is supplied to the substrate 1.
When the surface of No. 0 was irradiated vertically, the formation rate of the W film could be increased by about one digit. During the laser irradiation, the purge gas supply system 2 introduced Ar gas in the vicinity of the light introduction window 3 to prevent the reaction product from adhering to the inner surface of the window.
尚、本実施例においてイオン照射に代えて真空蒸着、あ
るいはスパッタリング法を用いてＴｉの薄膜を形成して
も同様のＷ膜形成が可能である。In the present embodiment, a similar W film can be formed by forming a Ti thin film by using vacuum deposition or sputtering instead of ion irradiation.
〈実施例２〉 本実施例は、ＴｉにかえてＮｉを触媒物質に用いたもの
であり、Ni(CO)4をイオン源１２の原料ガスに用いる。Example 2 In this example, Ni is used as a catalyst substance instead of Ti, and Ni (CO) 4 is used as a source gas of the ion source 12.
まず実施例１と同様、ＮｉイオンをSiO2表面に照射し
た。次に、光源５より波長１９３ｎｍのエキシマレーザ
光６を光学系４によりシート状ビーム（ビーム断面が一
辺が長く他辺が短い矩形状のビーム）７に整形した後基
板面の前方約１cmを基板面と平行に通過するように照射
しながらＣＶＤを行うことで、SiO2上にＷ膜を形成で
き、本発明においてもＮｉとＴｉと同様の作用を示すこ
とが確認された。尚、ＣＶＤの条件は実施例１と同様で
ある。First, as in Example 1, the surface of the SiO 2 was irradiated with Ni ions. Next, the excimer laser light 6 having a wavelength of 193 nm is shaped by the optical system 4 into a sheet-like beam (a rectangular beam having a beam cross section with one side being short and the other side being short) 7 from the light source 5 and then about 1 cm in front of the substrate surface. It was confirmed that a W film can be formed on SiO 2 by performing CVD while irradiating so as to pass in parallel to the surface, and also in the present invention, the same action as Ni and Ti is exhibited. The conditions for CVD are the same as in Example 1.
以上の実施例ではＴｉとＮｉを触媒物質に選んだが、こ
の他、Ｆｅ，Ｃｏ，白金族（Ｒｕ，Ｒｈ，Ｐｄ，Ｏｓ，
Ｉｒ，Ｐｔ）といった遷移金属が同様の効果を呈するも
のとして挙げることができる。In the above examples, Ti and Ni were selected as the catalytic materials, but in addition to these, Fe, Co, platinum group (Ru, Rh, Pd, Os,
Transition metals such as Ir and Pt) can be mentioned as those exhibiting the same effect.
〈実施例３〉 本実施例では、イオンビーム照射をマスクを通して行う
ことでSiO2表面の一部にのみＴｉの薄い膜を形成して、
その部分にのみＷ膜を形成するものである。Example 3 In this example, a thin film of Ti is formed only on a part of the SiO 2 surface by performing ion beam irradiation through a mask,
The W film is formed only on that portion.
まず、反応容器８内に設置された実施例１と同様の基板
１０の前に、第２図に示したようにマスク１６を置いて
おいて、Ｔｉのイオン照射を行った。次に基板１０を光
源５の方向に回転させ波長１９３ｎｍのエキシマレーザ
光を光学系４により拡大して基板１０の表面に垂直に照
射しながら、原料ガス供給系１よりWF6とH2を反応容器
８内に導入してＷ膜形成を１分間行った。この時の基板
温度は３００℃、WF6とH2とＡｒの流量比は１：１０
０：１００で全圧は0.2Torrとした。この条件はＷのＣ
ＶＤが表面反応で生じる条件である。レーザ光の照射を
停止した後基板温度を４００℃にあげ、マスクパターン
のとおりイオン照射部分１７にのみ選択的にＷ膜が形成
された。First, a mask 16 was placed as shown in FIG. 2 in front of a substrate 10 similar to that used in Example 1 placed in the reaction vessel 8, and Ti ion irradiation was performed. Next, the substrate 10 is rotated in the direction of the light source 5 and the excimer laser light with a wavelength of 193 nm is expanded by the optical system 4 and irradiated perpendicularly to the surface of the substrate 10 while reacting WF 6 and H 2 from the source gas supply system 1. After being introduced into the container 8, a W film was formed for 1 minute. At this time, the substrate temperature is 300 ° C., and the flow rate ratio of WF 6 , H 2 and Ar is 1:10.
At 0: 100, the total pressure was 0.2 Torr. This condition is C of W
VD is a condition that occurs in the surface reaction. After the irradiation of the laser beam was stopped, the substrate temperature was raised to 400 ° C., and the W film was selectively formed only on the ion-irradiated portion 17 according to the mask pattern.
尚、エキシマレーザ光の照射の時間を長くするとイオン
照射の行われなかった部分にもＷ膜が形成されることが
あった。しかし、エキシマレーザ光の波長を２４８ｎｍ
（ＫｒＦエキシマレーザ）とすればイオン照射の行われ
なかった部分へのＷ膜の形成は殆ど認められなかった。
これは２４８ｎｍの波長の光がＴｉのイオン照射部分１
７に吸着したWF6にのみ吸収された効果と考えられる。
また、本実施例ではマスクを用いてSiO2表面に部分的に
Ｔｉイオンビームを照射したが、収束イオンビームを用
いればサブミクロンのＷ配線パターンをマスクを用いる
ことなく容易に形成できる。In addition, when the irradiation time of the excimer laser light is lengthened, a W film may be formed in a portion where the ion irradiation is not performed. However, the wavelength of the excimer laser light is 248 nm.
With (KrF excimer laser), almost no W film was formed in the portion where ion irradiation was not performed.
This is the ion-irradiated part 1 where the light of the wavelength of 248 nm is Ti.
This is considered to be the effect of being absorbed only by WF 6 adsorbed on 7.
Further, in this embodiment, the SiO 2 surface was partially irradiated with the Ti ion beam using the mask, but if the focused ion beam is used, a submicron W wiring pattern can be easily formed without using the mask.
〈実施例４〉 本実施例は、H2分子の解離触媒であるＴｉを固体の形態
で反応容器内に設置したものである。用いた装置の概略
は第１図と同じであるが、イオン源は利用しない。Example 4 In this example, Ti, which is a dissociation catalyst for H 2 molecules, is installed in a solid state in a reaction vessel. The outline of the apparatus used is the same as that in FIG. 1, but the ion source is not used.
第３図に示すように、Ｔｉメッシユ１８を実施例１と同
様の基板１０の上方約0.5cmの所に設置しておいて、WF6
をH2を反応容器８内に導入した。この時の基板温度は４
５０℃、WF6とH2とＡｒの流量比は１０：１００：１０
０で全圧は２０Torrとした。この圧力の条件では、Ｔｉ
メッシュ１８上で生成されたＨ原子が気相中でWF6を還
元できるので、基板１０のSiO2上にＷ膜を形成すること
ができる。As shown in FIG. 3, the Ti mesh 18 was placed about 0.5 cm above the substrate 10 similar to that in Example 1, and WF 6
H 2 was introduced into the reaction vessel 8. The substrate temperature at this time is 4
50 ° C, the flow rate ratio of WF 6 , H 2 and Ar is 10: 100: 10.
At 0, the total pressure was 20 Torr. At this pressure condition, Ti
Since the H atoms generated on the mesh 18 can reduce WF 6 in the gas phase, a W film can be formed on the SiO 2 of the substrate 10.
本実施例は実施例１よりも簡便である。気相反応を用い
ているので基板との接着性は多少劣るが、従来の減圧Ｃ
ＶＤ法に比べ低温で膜形成が可能である。This embodiment is simpler than the first embodiment. Adhesion to the substrate is slightly inferior because it uses a gas phase reaction, but the conventional reduced pressure C
The film can be formed at a lower temperature than the VD method.
〈実施例５〉 本実施例は、反応容器内の真空度が１０-3Ｐａと比較的
低くてもＴｉによるH2の解離触媒を利用したＣＶＤを可
能にしたものである。Example 5 In this example, CVD using a dissociation catalyst of H 2 by Ti is possible even if the degree of vacuum in the reaction vessel is relatively low at 10 −3 Pa.
まず、実施例３と同様にＴｉイオンビームをマスク照射
して、一原子層程度の厚さのＴｉ膜のパターンを形成し
た。但し、１０-3Ｐａと低い真空度でイオン照射を行っ
たため、残留している水分やO2によりＴｉ膜が酸化され
てしまい、このままではＴｉ膜がH2の解離吸着触媒とし
て働かなかった。First, the Ti ion beam was mask-irradiated in the same manner as in Example 3 to form a Ti film pattern having a thickness of about one atomic layer. However, since the ion irradiation was performed at a low degree of vacuum of 10 −3 Pa, the Ti film was oxidized by the residual water and O 2 , and the Ti film did not work as a dissociative adsorption catalyst for H 2 as it was.
そこで、H2とＡｒを反応容器８内に0.4Torrまで導入し
て基板の温度を２００℃に保った状態で、波長１９３ｎ
ｍのエキシマレーザ光を光学系４により拡大して基板１
０の表面に３０秒間照射した。その後、WF6を反応容器
８内に追加して１分間レーザＣＶＤを行った。続いて、
基板温度を４５０℃に、全体の圧力を1.6Torrにあげて
熱ＣＶＤを５分間行ったところ、イオン照射パターンど
おりのＷ膜が形成できた。Therefore, with H 2 and Ar introduced into the reaction vessel 8 up to 0.4 Torr and the substrate temperature kept at 200 ° C., the wavelength of 193 n
The excimer laser beam of m is magnified by the optical system 4 and the substrate 1
0 surface was illuminated for 30 seconds. Then, WF 6 was added to the reaction vessel 8 and laser CVD was performed for 1 minute. continue,
When thermal CVD was performed for 5 minutes with the substrate temperature raised to 450 ° C. and the total pressure raised to 1.6 Torr, a W film was formed according to the ion irradiation pattern.
本実施例では、H2雰囲気中で加熱・レーザ照射を行うこ
とで酸化されていたＴｉの表面が還元され、H2解離触媒
として働くようになったものと考えられる。In this example, it is considered that the surface of oxidized Ti was reduced by performing heating and laser irradiation in the H 2 atmosphere, so that it worked as the H 2 dissociation catalyst.
本発明によれば、WF6とH2を用いたＣＶＤ法によりSiO2
上に接着性良くＷ膜を形成できる効果がある。According to the present invention, SiO 2 by a CVD method using WF 6 and H 2
There is an effect that a W film can be formed on the top with good adhesiveness.
【図面の簡単な説明】 第１図は、本発明の実施例に用いた装置の概略を示した
図である。 第２図は、実施例３において基板上にマスクを設置した
様子を示した図である。 第３図は、実施例４において基板上にＴｉメッシュを設
置した様子を示した図である。 １……原料ガス供給系、２……パージガス供給系、３…
…光導入用窓、４……光学系、５……光源、６……レー
ザ光、７……拡大されたレーザ光、８……反応容器、９
……ヒータ、１０……基板、１１……ゲートバルブ、１
２……イオン源、１３……イオン源用原料ガス供給系、
１４……高真空用排気系、１５……低真空用排気系、１
６……マスク、１７……イオン照射部分、１８……Ｔｉ
メッシュ。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a diagram showing an outline of an apparatus used in an embodiment of the present invention. FIG. 2 is a diagram showing a state in which a mask is placed on the substrate in the third embodiment. FIG. 3 is a diagram showing a state in which a Ti mesh is installed on a substrate in Example 4. 1 ... Raw material gas supply system, 2 ... Purge gas supply system, 3 ...
... light introduction window, 4 ... optical system, 5 ... light source, 6 ... laser light, 7 ... enlarged laser light, 8 ... reaction container, 9
...... Heater, 10 …… Substrate, 11 …… Gate valve, 1
2 ... Ion source, 13 ... Ion source material gas supply system,
14 ... High vacuum exhaust system, 15 ... Low vacuum exhaust system, 1
6 ... Mask, 17 ... Ion irradiation part, 18 ... Ti
mesh.
Claims (21)
成する方法において、触媒作用を及ぼす物質あるいはそ
の化合物による第１の膜を予め基板上に形成した後、あ
るいは形成しながら、原料ガスを用いて化学的気相成長
法により上記第１の膜の上に第２の膜を形成することを
特徴とする薄膜の形成方法。1. A method of forming a thin film on a substrate by a chemical vapor deposition method, which comprises forming a first film of a substance having a catalytic action or a compound thereof on a substrate in advance or while forming the first film. A method of forming a thin film, which comprises forming a second film on the first film by a chemical vapor deposition method using a gas.
真空蒸着あるいはスパッタリングによるものであること
を特徴とする特許請求の範囲第１項記載の薄膜の形成方
法。2. A method of forming the first film on a substrate comprises:
The method for forming a thin film according to claim 1, wherein the thin film is formed by vacuum vapor deposition or sputtering.
上記触媒作用を及ぼす物質あるいはその化合物を中性ビ
ームあるいはイオンビームの形態で基板表面に照射する
方法であることを特徴とする特許請求の範囲第１項記載
の薄膜の形成方法。3. A method of forming the first film on a substrate comprises:
The method for forming a thin film according to claim 1, which is a method of irradiating the surface of the substrate with the substance having the catalytic action or a compound thereof in the form of a neutral beam or an ion beam.
て、上記第１の膜に光を照射しながら化学的気相成長法
により第２の膜を形成することを特徴とする特許請求の
範囲第３項記載の薄膜の形成方法。4. A method of forming a second film on the first film, wherein the second film is formed by chemical vapor deposition while irradiating the first film with light. The method for forming a thin film according to claim 3.
なる条件で化学的気相成長法により薄膜を形成すること
を特徴とする特許請求の範囲第４項記載の薄膜の形成方
法。5. The method for forming a thin film according to claim 4, wherein a thin film is formed on the second film by the chemical vapor deposition method under the same conditions or different conditions.
化合物を照射した基板表面に対して照射する光が、化学
的気相成長法に用いる原料ガスに吸収される波長の光で
あることを特徴とする特許請求の範囲第４項または第５
項記載の薄膜の形成方法。6. The light for irradiating the surface of the substrate irradiated with the substance having the catalytic action or the compound thereof is light having a wavelength absorbed by a source gas used in a chemical vapor deposition method. Claims 4 or 5
A method for forming a thin film according to the item.
化合物を照射した基板表面に対して照射する光が、基板
上に吸着した化学的気相成長に用いる原料ガスに選択的
に吸収される波長の光であることを特徴とする特許請求
の範囲第４項または第５項記載の薄膜の形成方法。7. A wavelength at which the light irradiated to the surface of the substrate irradiated with the substance having the catalytic action or the compound thereof is selectively absorbed by the source gas used for chemical vapor deposition adsorbed on the substrate. 6. The method for forming a thin film according to claim 4 or 5, characterized in that the light is a light.
長において、光を基板表面に直接当らないように照射し
ながら化学的気相成長を行わせることを特徴とする特許
請求の範囲第４項〜第６項に記載の薄膜の形成方法。8. The chemical vapor deposition carried out while irradiating the light described above, wherein the chemical vapor deposition is carried out while irradiating the light so as not to directly hit the surface of the substrate. The method for forming a thin film according to any one of items 4 to 6.
に、同一条件あるいは異なる条件で化学的気相成長法に
より薄膜を形成することを特徴とする特許請求の範囲第
８項記載の薄膜の形成方法。9. The method according to claim 8, wherein after the chemical vapor deposition is performed, a thin film is further formed by a chemical vapor deposition method under the same conditions or different conditions. Method for forming thin film.
成長に際して、光を基板表面に直接当らないように照射
する光が、化学的気相成長法に用いる原料ガスに吸収さ
れる波長の光であることを特徴とする特許請求の範囲第
８項及び第９項記載の薄膜の形成方法。10. In the chemical vapor deposition carried out while irradiating the light, the wavelength of the light which is irradiated so that the light does not directly hit the surface of the substrate is absorbed by the source gas used in the chemical vapor deposition method. 10. The method for forming a thin film according to claim 8 or 9, characterized in that the light is a light.
ームあるいはイオンビームの照射時に、マスクを用いて
所定のパターンを選択的に照射して、第１の膜の形成を
行うことを特徴とする特許請求の範囲第３項〜第１０項
の何れかに記載の薄膜の形成方法。11. A first film is formed by selectively irradiating a predetermined pattern with a mask when irradiating the catalyst or its compound with a neutral beam or an ion beam. The method for forming a thin film according to any one of claims 3 to 10.
の化合物のイオンビームの照射を収束イオンビームを用
いて行い、該照射部に選択的に膜形成を行うことを特徴
とする特許請求の範囲第３項〜第１０項の何れかに記載
の薄膜の形成方法。12. The irradiation of an ion beam of the above-mentioned substance exerting a catalytic action or a compound thereof by using a focused ion beam to selectively form a film on the irradiation portion. The method for forming a thin film as described in any one of 3 to 10.
化合物が遷移金属あるいはその化合物であることを特徴
とする特許請求の範囲第１項記載の薄膜の形成方法。13. The method for forming a thin film according to claim 1, wherein the substance having a catalytic action or a compound thereof is a transition metal or a compound thereof.
の化合物がTiあるいはその化合物であることを特徴とす
る特許請求の範囲第１項記載の薄膜の形成方法。14. The method for forming a thin film according to claim 1, wherein the substance having the above-mentioned catalytic action or the compound thereof is Ti or the compound thereof.
ザ光であることを特徴とする特許請求の範囲第４項、第
５項、第６項、第８項、第９項、第１０項の何れかに記
載の薄膜の形成方法。15. The above-mentioned light is ArF excimer laser light having a wavelength of 193 nm. Claims 4, 5, 6, 6, 8, 9 and 10. A method for forming a thin film according to any one of 1.
ザ光であることを特徴とする特許請求の範囲第７項記載
の薄膜の形成方法。16. The method for forming a thin film according to claim 7, wherein the light is KrF excimer laser light having a wavelength of 248 nm.
Ｗであることを特徴とする特許請求の範囲第１項〜第１
６項の何れかに記載の薄膜の形成方法。17. The thin film formed by the chemical vapor deposition method is W, wherein the thin film is W.
7. The method for forming a thin film as described in any one of 6 above.
の残留成分とが反応して形成された化合物を還元する工
程を含むことを特徴とする特許請求の範囲第２項〜第１
２項の何れかに記載の薄膜の形成方法。18. The method according to claim 2, further comprising the step of reducing the compound formed by reacting the first film or the residual component in the reaction vessel with the first film.
The method for forming a thin film as described in any one of 2 above.
基板を加熱する工程であることを特徴とする特許請求の
範囲第１８項記載の薄膜の形成方法。19. The method for forming a thin film according to claim 18, wherein the reducing step is a step of heating the substrate in an atmosphere containing hydrogen.
光を照射しながら基板を加熱する工程であることを特徴
とする特許請求の範囲第１８項記載の薄膜の形成方法。20. The method for forming a thin film according to claim 18, wherein the reducing step is a step of heating the substrate while irradiating light in an atmosphere containing hydrogen.
いはそれと反応容器内の残留成分とが反応して形成され
た化合物に吸収される波長の光を用いることを特徴とす
る特許請求の範囲第２０項記載の薄膜の形成方法。21. As the irradiation light, light having a wavelength absorbed by the first film or a compound formed by the reaction between the first film and the residual component in the reaction vessel is used. 21. A method for forming a thin film as set forth in claim 20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1036125A JPH0645893B2 (en) | 1989-02-17 | 1989-02-17 | Method of forming thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1036125A JPH0645893B2 (en) | 1989-02-17 | 1989-02-17 | Method of forming thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02217469A JPH02217469A (en) | 1990-08-30 |
| JPH0645893B2 true JPH0645893B2 (en) | 1994-06-15 |
Family
ID=12461062
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1036125A Expired - Lifetime JPH0645893B2 (en) | 1989-02-17 | 1989-02-17 | Method of forming thin film |
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| JP (1) | JPH0645893B2 (en) |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4618541A (en) * | 1984-12-21 | 1986-10-21 | Advanced Micro Devices, Inc. | Method of forming a silicon nitride film transparent to ultraviolet radiation and resulting article |
| JPS61247020A (en) * | 1985-04-24 | 1986-11-04 | Canon Inc | Deposition film forming method |
| JPS61276976A (en) * | 1985-05-31 | 1986-12-06 | Res Dev Corp Of Japan | Method and apparatus for producing high quality thin film containing silicon by thermal cvd method using species in intermediate state |
| US4696834A (en) * | 1986-02-28 | 1987-09-29 | Dow Corning Corporation | Silicon-containing coatings and a method for their preparation |
| JPS6425984A (en) * | 1987-03-23 | 1989-01-27 | Canon Kk | Formation of deposited film |
-
1989
- 1989-02-17 JP JP1036125A patent/JPH0645893B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02217469A (en) | 1990-08-30 |
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