JP2002093804A - Material for forming hafnium-based oxide film - Google Patents
Material for forming hafnium-based oxide filmInfo
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- JP2002093804A JP2002093804A JP2000282198A JP2000282198A JP2002093804A JP 2002093804 A JP2002093804 A JP 2002093804A JP 2000282198 A JP2000282198 A JP 2000282198A JP 2000282198 A JP2000282198 A JP 2000282198A JP 2002093804 A JP2002093804 A JP 2002093804A
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- oxide film
- hafnium
- group
- based oxide
- compound
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、ハフニウム系酸化
膜形成材料に関する。The present invention relates to a hafnium-based oxide film forming material.
【０００２】[0002]
【発明が解決しようとする課題】近年、ＵＬＳＩの進展
に伴い、トランジスタのソース−ドレイン間距離は一層
短くなって来ている。同時に、ゲート酸化膜の厚さも薄
膜化の一途を辿っている。因みに、その膜厚は１０ｎｍ
以下になることが予想されている。In recent years, with the development of ULSI, the distance between the source and the drain of a transistor has been further reduced. At the same time, the thickness of the gate oxide film has been steadily reduced. By the way, the film thickness is 10 nm
It is expected that:
【０００３】ところで、現在、ゲート酸化膜はＳｉＯ２
で出来ているが、このＳｉＯ２製ゲート酸化膜の厚さが
３ｎｍ以下の厚さに至ると、ソースとドレイン間に溜め
られた電荷はゲート酸化膜を通り抜けてしまうようにな
る。At present, the gate oxide film is made of SiO 2
However, when the thickness of the SiO 2 gate oxide film reaches a thickness of 3 nm or less, charges accumulated between the source and the drain pass through the gate oxide film.
【０００４】このような問題を解決する為に金属酸化膜
が提案され始めた。[0004] In order to solve such a problem, a metal oxide film has been proposed.
【０００５】しかし、単に、金属酸化膜であれば良いと
言うものではない。[0005] However, it is not simply sufficient to use a metal oxide film.
【０００６】例えば、下層のシリコンを酸化しないこと
が必要である。For example, it is necessary not to oxidize the underlying silicon.
【０００７】そして、ハフニウムは、シリコンとの界面
に珪酸ハフニウム（ＨｆＳｉＯ４）を形成することか
ら、シリコンを酸化しないと言うことが報告されてい
る。It is reported that hafnium does not oxidize silicon because it forms hafnium silicate (HfSiO 4 ) at the interface with silicon.
【０００８】従って、ハフニウム酸化膜はゲート酸化膜
として好都合なことが判る。Therefore, it can be seen that the hafnium oxide film is favorable as a gate oxide film.
【０００９】ところで、ハフニウム酸化膜の形成方法は
スパッタによっていた。The hafnium oxide film is formed by sputtering.
【００１０】しかし、スパッタ法は、一般的に、成膜に
時間が掛かり過ぎる。However, the sputtering method generally takes too much time for film formation.
【００１１】又、段差被膜性に劣る。例えば、表面が平
坦ではなく、凹凸があるような基板に膜を形成しようと
した場合、凹部の底の面には膜が形成されないようなこ
とがある。膜が形成されても、その膜は均一なものでな
く、斑状のものであったりする。Also, the step coverage is poor. For example, when an attempt is made to form a film on a substrate whose surface is not flat and has irregularities, the film may not be formed on the bottom surface of the concave portion. Even if a film is formed, the film is not uniform and may be patchy.
【００１２】従って、本発明が解決しようとする課題
は、綺麗なハフニウム系酸化膜を効率良く形成できる技
術を提供することである。Therefore, an object of the present invention is to provide a technique capable of efficiently forming a beautiful hafnium-based oxide film.
【００１３】[0013]
【課題を解決するための手段】前記の課題は、（Ｒ１Ｒ
２Ｎ）４Ｈｆ〔但し、Ｒ１，Ｒ２はアルキル基、及びシ
リコン系化合物の基の群の中から選ばれるものであり、
Ｒ１とＲ２とは互いに異なっていても同じであってもよ
い。〕で表される化合物からなることを特徴とするハフ
ニウム系酸化膜形成材料によって解決される。The above object is achieved by (R 1 R
2 N) 4 Hf [where R 1 and R 2 are selected from the group consisting of an alkyl group and a silicon-based compound;
R 1 and R 2 may be different or the same. And a hafnium-based oxide film forming material characterized by comprising the compound represented by the formula:
【００１４】特に、（Ｒ１Ｒ２Ｎ）４Ｈｆ〔但し、
Ｒ１，Ｒ２がメチル基及びエチル基の群の中から選ばれ
るいずれかである。〕で表される化合物からなることを
特徴とするハフニウム系酸化膜形成材料によって解決さ
れる。In particular, (R 1 R 2 N) 4 Hf [provided that
R 1 and R 2 are any one selected from the group consisting of a methyl group and an ethyl group. And a hafnium-based oxide film forming material characterized by comprising the compound represented by the formula:
【００１５】中でも、（Ｍｅ２Ｎ）４Ｈｆ，（Ｅｔ
２Ｎ）４Ｈｆ及び／又は（Ｅｔ（Ｍｅ）Ｎ）４Ｈｆで表
される化合物からなることを特徴とするハフニウム系酸
化膜形成材料によって解決される。Among them, (Me 2 N) 4 Hf, (Et
The problem is solved by a hafnium-based oxide film-forming material characterized by comprising a compound represented by 2N) 4 Hf and / or (Et (Me) N) 4 Hf.
【００１６】上記化合物を用いることによってハフニウ
ム酸化膜を効率良く形成できる。By using the above compound, a hafnium oxide film can be efficiently formed.
【００１７】しかし、（Ｒ１Ｒ２Ｎ）４Ｈｆのみではな
く、（Ｒ１Ｒ２Ｎ）４ＨｆとＳｉ化合物とを併用しても
膜が形成できる。すなわち、（Ｒ１Ｒ２Ｎ）４ＨｆとＳ
ｉ化合物とを併用することによって、シリコンとハフニ
ウムとを主成分として含む酸化膜を形成できる。However, a film can be formed by using not only (R 1 R 2 N) 4 Hf but also a combination of (R 1 R 2 N) 4 Hf and a Si compound. That is, (R 1 R 2 N) 4 Hf and S
By using the i-compound together, an oxide film containing silicon and hafnium as main components can be formed.
【００１８】従って、前記の課題は、（Ｒ１Ｒ２Ｎ）４
Ｈｆ〔但し、Ｒ１，Ｒ２はアルキル基、及びシリコン系
化合物の基の群の中から選ばれるものであり、Ｒ１とＲ
２とは互いに異なっていても同じであってもよい。〕で
表される化合物と、Ｓｉ化合物とを含むことを特徴とす
るハフニウム系酸化膜形成材料によって解決される。Therefore, the above-mentioned problem is solved by (R 1 R 2 N) 4
Hf [However, R 1, R 2 are those selected from the group of radicals of the alkyl group, and silicon-based compounds, R 1 and R
2 may be different from or the same as each other. And a Si compound and a hafnium-based oxide film-forming material.
【００１９】特に、（Ｒ１Ｒ２Ｎ）４Ｈｆ〔但し、
Ｒ１，Ｒ２がメチル基及びエチル基の群の中から選ばれ
るいずれかである。〕で表される化合物と、Ｓｉ化合物
とを含むことを特徴とするハフニウム系酸化膜形成材料
によって解決される。In particular, (R 1 R 2 N) 4 Hf [provided that
R 1 and R 2 are any one selected from the group consisting of a methyl group and an ethyl group. And a Si compound and a hafnium-based oxide film-forming material.
【００２０】中でも、（Ｍｅ２Ｎ）４Ｈｆ，（Ｅｔ
２Ｎ）４Ｈｆ及び／又は（Ｅｔ（Ｍｅ）Ｎ）４Ｈｆで表
される化合物と、Ｓｉ化合物とを含むことを特徴とする
ハフニウム系酸化膜形成材料によって解決される。Among them, (Me 2 N) 4 Hf, (Et
The problem is solved by a hafnium-based oxide film forming material characterized by containing a compound represented by 2N) 4 Hf and / or (Et (Me) N) 4 Hf and a Si compound.
【００２１】上記Ｓｉ化合物としては、好ましくは（Ｒ
１Ｒ２Ｎ）ｎＳｉＨ４−ｎ〔但し、Ｒ１，Ｒ２はアルキ
ル基、及びシリコン系化合物の基の群の中から選ばれる
ものであり、Ｒ１とＲ２とは互いに異なっていても同じ
であってもよい。ｎは１〜４の整数。〕で表される化合
物である。中でも、（Ｅｔ２Ｎ）４Ｓｉ，（Ｅｔ２Ｎ）
３ＳｉＨ，（Ｅｔ２Ｎ）２ＳｉＨ２，（Ｍｅ２Ｎ）４Ｓ
ｉ，（Ｍｅ２Ｎ）３ＳｉＨ，（Ｍｅ２Ｎ）２ＳｉＨ
２〔但し、Ｍｅはメチル基、Ｅｔはエチル基。〕の群の
中から選ばれるいずれかである。The Si compound is preferably (R
1 R 2 N) n SiH 4-n [where R 1 and R 2 are selected from the group consisting of an alkyl group and a group of a silicon compound, and R 1 and R 2 are different from each other. May be the same. n is an integer of 1 to 4. ] It is a compound represented by these. Among them, (Et 2 N) 4 Si, (Et 2 N)
3 SiH, (Et 2 N) 2 SiH 2 , (Me 2 N) 4 S
i, (Me 2 N) 3 SiH, (Me 2 N) 2 SiH
2 [where Me is a methyl group and Et is an ethyl group. ] Is selected from the group consisting of
【００２２】本発明において、（Ｒ１Ｒ２Ｎ）４Ｈｆで
表される化合物とＳｉ化合物とが共に用いられる場合、
Ｓｉ化合物と（Ｒ１Ｒ２Ｎ）４Ｈｆとの割合（重量比）
は、好ましくは、前者：後者＝１：１００〜１０００：
１である。更に好ましくは、１：５０〜１００：１であ
る。In the present invention, when a compound represented by (R 1 R 2 N) 4 Hf and a Si compound are used together,
Ratio (weight ratio) of Si compound and (R 1 R 2 N) 4 Hf
Is preferably the former: the latter = 1: 100-1000:
It is one. More preferably, the ratio is 1:50 to 100: 1.
【００２３】上記のハフニウム系酸化膜形成材料は、溶
媒を更に含む形態のものが好ましい。すなわち、上記の
ハフニウム系酸化膜形成材料は溶媒中に溶解してなる形
態のものが好ましい。The above-mentioned hafnium-based oxide film forming material preferably has a form further containing a solvent. That is, the above-mentioned hafnium-based oxide film forming material is preferably in a form dissolved in a solvent.
【００２４】このような溶媒は、上記ハフニウム系酸化
膜形成材料が溶解されるものであれば良い。中でも好ま
しいものとしては、溶媒が炭素数５〜４０の炭化水素系
化合物及び炭素数２〜４０のアミン系化合物の群の中か
ら選ばれる化合物である。Such a solvent may be any solvent in which the above-mentioned hafnium-based oxide film forming material is dissolved. Among them, a compound whose solvent is selected from the group consisting of a hydrocarbon compound having 5 to 40 carbon atoms and an amine compound having 2 to 40 carbon atoms is preferable.
【００２５】[0025]
【発明の実施の形態】本発明になるハフニウム系酸化膜
形成材料は、（Ｒ１Ｒ２Ｎ）４Ｈｆ〔但し、Ｒ１，Ｒ２
はアルキル基（特に、炭素数1〜１２のアルキル基）、
及びシリコン系化合物の基の群の中から選ばれるもので
あり、Ｒ１とＲ２とは互いに異なっていても同じであっ
てもよい。〕で表される化合物からなる。特に、（Ｒ１
Ｒ２Ｎ）４Ｈｆ〔但し、Ｒ１，Ｒ２がメチル基及びエチ
ル基の群の中から選ばれるいずれかである。〕で表され
る化合物からなる。中でも、（Ｍｅ２Ｎ）４Ｈｆ，（Ｅ
ｔ２Ｎ）４Ｈｆ及び／又は（Ｅｔ（Ｍｅ）Ｎ）４Ｈｆ
（Ｍｅはメチル基、Ｅｔはエチル基）で表される化合物
からなる。BEST MODE FOR CARRYING OUT THE INVENTION The material for forming a hafnium-based oxide film according to the present invention is (R 1 R 2 N) 4 Hf [where R 1 , R 2
Represents an alkyl group (particularly, an alkyl group having 1 to 12 carbon atoms),
And R 1 and R 2 may be different from or the same as each other. ] The compound represented by these. In particular, (R 1
R 2 N) 4 Hf [where R 1 and R 2 are any selected from the group consisting of a methyl group and an ethyl group. ] The compound represented by these. Among them, (Me 2 N) 4 Hf, (E
t 2 N) 4 Hf and / or (Et (Me) N) 4 Hf
(Me is a methyl group, Et is an ethyl group).
【００２６】又、（Ｒ１Ｒ２Ｎ）４Ｈｆのみではなく、
（Ｒ１Ｒ２Ｎ）４Ｈｆ〔上記に同じ。〕で表される化合
物と、Ｓｉ化合物とを含むものである。特に、（Ｒ１Ｒ
２Ｎ）４Ｈｆ〔但し、Ｒ１，Ｒ２がメチル基及びエチル
基の群の中から選ばれるいずれかである。〕で表される
化合物と、Ｓｉ化合物とを含むものである。中でも、
（Ｍｅ２Ｎ）４Ｈｆ，（Ｅｔ２Ｎ）４Ｈｆ及び／又は
（Ｅｔ（Ｍｅ）Ｎ）４Ｈｆで表される化合物と、Ｓｉ化
合物とを含むものである。このＳｉ化合物としては、好
ましくは（Ｒ１Ｒ２Ｎ）ｎＳｉＨ４−ｎ〔但し、Ｒ１，
Ｒ２はアルキル基、及びシリコン系化合物の基の群の中
から選ばれるものであり、Ｒ１とＲ２とは互いに異なっ
ていても同じであってもよい。ｎは１〜４の整数。〕で
表される化合物である。中でも、（Ｅｔ２Ｎ）４Ｓｉ，
（Ｅｔ２Ｎ）３ＳｉＨ，（Ｅｔ２Ｎ） ２ＳｉＨ２，（Ｍ
ｅ２Ｎ）４Ｓｉ，（Ｍｅ２Ｎ）３ＳｉＨ，（Ｍｅ２Ｎ）
２ＳｉＨ２〔但し、Ｍｅはメチル基、Ｅｔはエチル
基。〕の群の中から選ばれるいずれかである。（Ｒ１Ｒ
２Ｎ）４Ｈｆで表される化合物とＳｉ化合物とが共に用
いられる場合、Ｓｉ化合物と（Ｒ１Ｒ２Ｎ）４Ｈｆとの
割合（重量比）は、好ましくは、前者：後者＝１：１０
０〜１０００：１である。更に好ましくは、１：５０〜
１００：１である。Also, (R1R2N)4Not only Hf,
(R1R2N)4Hf [same as above. Compound represented by]
And a Si compound. In particular, (R1R
2N)4Hf [where R1, R2Is a methyl group and ethyl
Any one selected from the group of groups. ]
It contains a compound and a Si compound. Among them,
(Me2N)4Hf, (Et2N)4Hf and / or
(Et (Me) N)4Compound represented by Hf and Si formation
And a compound. As the Si compound,
Preferably (R1R2N)nSiH4-n[However, R1,
R2In the group of alkyl groups and silicon compound groups
R is selected from1And R2Different from each other
Or the same. n is an integer of 1 to 4. 〕so
It is a compound represented. Among them, (Et2N)4Si,
(Et2N)3SiH, (Et2N) 2SiH2, (M
e2N)4Si, (Me2N)3SiH, (Me2N)
2SiH2[However, Me is a methyl group, Et is ethyl.
Base. ] Is selected from the group consisting of (R1R
2N)4Both Hf and Si compounds are used
If it is, the Si compound and (R1R2N)4With Hf
The ratio (weight ratio) is preferably the former: the latter = 1: 10
0 to 1000: 1. More preferably, 1: 50-
100: 1.
【００２７】本発明になるハフニウム系酸化膜形成材料
は、必要に応じて、溶媒を更に含む。すなわち、上記の
ハフニウム系酸化膜形成材料は溶媒中に溶解してなる形
態のものが好ましい。このような溶媒は、上記ハフニウ
ム系酸化膜形成材料が溶解されるものであれば良い。中
でも好ましいものとしては、溶媒が炭素数５〜４０の炭
化水素系化合物及び炭素数２〜４０のアミン系化合物の
群の中から選ばれる化合物である。具体的に挙げると、
炭化水素系の溶媒としては、例えばノルマルデカン、ノ
ルマルヘプタン、テトラデカン、キシレン、トルエンが
挙げられる。アミン系の溶媒としては、例えばトリエチ
ルアミン、ビス（トリメチルシリル）アミン、ジエチル
アミン、ピリジンが挙げられる。溶媒の量は、上記ハフ
ニウム系酸化膜形成材料１００重量部に対して溶媒が１
〜１００００重量部、特に１００〜２０００重量部であ
るのが好ましい。The hafnium-based oxide film forming material according to the present invention may further contain a solvent, if necessary. That is, the above-mentioned hafnium-based oxide film forming material is preferably in a form dissolved in a solvent. Such a solvent may be any as long as the hafnium-based oxide film forming material is dissolved. Among them, a compound whose solvent is selected from the group consisting of a hydrocarbon compound having 5 to 40 carbon atoms and an amine compound having 2 to 40 carbon atoms is preferable. To be specific,
Examples of the hydrocarbon-based solvent include normal decane, normal heptane, tetradecane, xylene, and toluene. Examples of the amine-based solvent include triethylamine, bis (trimethylsilyl) amine, diethylamine, and pyridine. The amount of the solvent is such that 1 part by weight of the solvent is
It is preferably from 1 to 10,000 parts by weight, particularly preferably from 100 to 2000 parts by weight.
【００２８】本発明のハフニウム系酸化膜形成材料によ
って形成される膜は酸化膜タイプのものである。又、本
発明のハフニウム系酸化膜形成材料は、化学気相成長方
法によりハフニウム系酸化膜を形成する為のものであ
る。The film formed by the hafnium-based oxide film forming material of the present invention is of an oxide film type. The hafnium-based oxide film forming material of the present invention is for forming a hafnium-based oxide film by a chemical vapor deposition method.
【００２９】以下、具体的な実施例を挙げて説明する。Hereinafter, a specific embodiment will be described.
【００３０】[0030]
【実施例１】図１は、本発明になる化学気相成長方法が
実施される装置の概略図である。Embodiment 1 FIG. 1 is a schematic view of an apparatus for carrying out a chemical vapor deposition method according to the present invention.
【００３１】尚、図１中、１ａ，１ｂは容器、３は加熱
器、４は分解反応炉、５はＳｉ基板、６はガス流量制御
器である。In FIG. 1, 1a and 1b are containers, 3 is a heater, 4 is a decomposition reactor, 5 is a Si substrate, and 6 is a gas flow controller.
【００３２】そして、図１の装置を用いてＳｉ基板５上
にＨｆ酸化膜を作製した。Then, an Hf oxide film was formed on the Si substrate 5 using the apparatus shown in FIG.
【００３３】すなわち、容器１ａ内に（Ｅｔ２Ｎ）４Ｈ
ｆを入れて１００℃に加熱すると共に、窒素ガス（キャ
リアーガス）を３０ｍｌ／分の割合で供給した。そし
て、気化された（Ｅｔ２Ｎ）４Ｈｆはキャリアーガスと
共に配管を経て分解反応炉４に導かれた。又、同時に、
反応ガスとして酸素が導入された。尚、この時、系内は
真空に排気されている。又、Ｓｉ基板５は５００℃に加
熱されている。That is, (Et 2 N) 4 H is placed in the container 1a.
f and heated to 100 ° C., and nitrogen gas (carrier gas) was supplied at a rate of 30 ml / min. Then, the vaporized (Et 2 N) 4 Hf was led to the decomposition reaction furnace 4 via a pipe together with the carrier gas. Also, at the same time,
Oxygen was introduced as a reaction gas. At this time, the system is evacuated to a vacuum. The Si substrate 5 is heated to 500 ° C.
【００３４】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００３５】この膜を元素分析により調べた処、Ｈｆを
主成分とするものであることが判った。又、X線回折に
よればＨｆの酸化膜であることが判った。Examination of this film by elemental analysis revealed that it was mainly composed of Hf. According to X-ray diffraction, the film was found to be an oxide film of Hf.
【００３６】[0036]
【実施例２】実施例１において、（Ｅｔ２Ｎ）４Ｈｆの
代わりに（Ｍｅ２Ｎ）４Ｈｆを用いた以外は同様に行
い、Ｓｉ基板５上にＨｆの酸化膜を形成した。Example 2 An Hf oxide film was formed on a Si substrate 5 in the same manner as in Example 1 except that (Me 2 N) 4 Hf was used instead of (Et 2 N) 4 Hf.
【００３７】[0037]
【実施例３】実施例１において、（Ｅｔ２Ｎ）４Ｈｆの
代わりに（Ｅｔ（Ｍｅ）Ｎ）４Ｈｆを用いた以外は同様
に行い、Ｓｉ基板５上にＨｆの酸化膜を形成した。Example 3 An Hf oxide film was formed on a Si substrate 5 in the same manner as in Example 1 except that (Et (Me) N) 4 Hf was used instead of (Et 2 N) 4 Hf. .
【００３８】[0038]
【実施例４】図１の装置を用いてＳｉ基板５上にＨｆ系
酸化膜を作製した。Embodiment 4 An Hf-based oxide film was formed on a Si substrate 5 using the apparatus shown in FIG.
【００３９】すなわち、容器１ａ内に（Ｅｔ２Ｎ）４Ｈ
ｆを入れて１００℃に加熱すると共に、窒素ガス（キャ
リアーガス）を３０ｍｌ／分の割合で供給した。That is, (Et 2 N) 4 H is placed in the container 1a.
f and heated to 100 ° C., and nitrogen gas (carrier gas) was supplied at a rate of 30 ml / min.
【００４０】又、容器１ｂ内に（Ｅｔ２Ｎ）３ＳｉＨを
入れて８０℃に加熱すると共に、窒素ガス（キャリアー
ガス）を３０ｍｌ／分の割合で供給した。Further, (Et 2 N) 3 SiH was placed in the vessel 1b, heated to 80 ° C., and a nitrogen gas (carrier gas) was supplied at a rate of 30 ml / min.
【００４１】気化された（Ｅｔ２Ｎ）４Ｈｆと（Ｅｔ２
Ｎ）３ＳｉＨとはキャリアーガスと共に配管を経て分解
反応炉４に導かれた。又、同時に、反応ガスとして酸素
が導入された。尚、この時、系内は真空に排気されてい
る。又、Ｓｉ基板５は５００℃に加熱されている。The vaporized (Et 2 N) 4 Hf and (Et 2
N) 3 SiH was introduced into the decomposition reaction furnace 4 via a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. At this time, the system is evacuated to a vacuum. The Si substrate 5 is heated to 500 ° C.
【００４２】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００４３】この膜を元素分析により調べた結果、Ｈｆ
とＳｉとを主成分とするものであることが判った。又、
X線回折によれば酸化膜であることが判った。The film was analyzed by elemental analysis to find that Hf
And Si as a main component. or,
X-ray diffraction revealed that the film was an oxide film.
【００４４】[0044]
【実施例５】図２の装置を用いてＳｉ基板５上にＨｆ系
酸化膜を作製した。Embodiment 5 An Hf-based oxide film was formed on a Si substrate 5 using the apparatus shown in FIG.
【００４５】すなわち、（Ｅｔ２Ｎ）４Ｈｆと（Ｅｔ２
Ｎ）３ＳｉＨとの等量混合物を容器１ａ内に入れ、液体
流量制御器７を通して気化器２に送った。尚、この気化
器２では１５０℃にして気化させている。That is, (Et 2 N) 4 Hf and (Et 2
An equivalent mixture with N) 3 SiH was placed in the container 1 a and sent to the vaporizer 2 through the liquid flow controller 7. The vaporizer 2 vaporizes at 150 ° C.
【００４６】気化された（Ｅｔ２Ｎ）４Ｈｆと（Ｅｔ２
Ｎ）３ＳｉＨとはキャリアーガスと共に配管を経て分解
反応炉４に導かれた。又、同時に、反応ガスとして酸素
が導入された。尚、この時、系内は真空に排気されてい
る。又、Ｓｉ基板５は５００℃に加熱されている。The vaporized (Et 2 N) 4 Hf and (Et 2
N) 3 SiH was introduced into the decomposition reaction furnace 4 via a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. At this time, the system is evacuated to a vacuum. The Si substrate 5 is heated to 500 ° C.
【００４７】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００４８】この膜を元素分析により調べた処、Ｈｆと
Ｓｉとを主成分とするものであることが判った。又、X
線回折によれば酸化膜であることが判った。When this film was examined by elemental analysis, it was found that the film was mainly composed of Hf and Si. Also X
Line diffraction revealed that the film was an oxide film.
【００４９】[0049]
【実施例６〜１０】実施例５において、（Ｅｔ２Ｎ）３
ＳｉＨの代わりに、（Ｅｔ２Ｎ）４Ｓｉ，（Ｅｔ２Ｎ）
２ＳｉＨ２，（Ｍｅ２Ｎ）４Ｓｉ，（Ｍｅ２Ｎ）３Ｓｉ
Ｈ，（Ｍｅ ２Ｎ）２ＳｉＨ２を用いた以外は同様に行
い、Ｓｉ基板５上にＨｆとＳｉとの酸化膜を形成した。Embodiments 6 to 10 In Embodiment 5, (Et2N)3
Instead of SiH, (Et2N)4Si, (Et2N)
2SiH2, (Me2N)4Si, (Me2N)3Si
H, (Me 2N)2SiH2Except that
First, an oxide film of Hf and Si was formed on the Si substrate 5.
【００５０】[0050]
【実施例１１】図２の装置を用いてＳｉ基板５上にＨｆ
酸化膜を作製した。Embodiment 11 Using the apparatus shown in FIG.
An oxide film was formed.
【００５１】すなわち、（Ｍｅ２Ｎ）４Ｈｆとノルマル
デカンとの混合物（前者：後者＝１：５）を容器１ａ内
に入れ、液体流量制御器７を通して気化器２に送った。
尚、この気化器２では１５０℃にして気化させている。That is, a mixture of (Me 2 N) 4 Hf and normal decane (the former: the latter = 1: 5) was placed in the container 1 a and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 vaporizes at 150 ° C.
【００５２】気化された（Ｍｅ２Ｎ）４Ｈｆとノルマル
デカンとはキャリアーガスと共に配管を経て分解反応炉
４に導かれた。又、同時に、反応ガスとして酸素が導入
された。尚、Ｓｉ基板５は５００℃に加熱されている。The vaporized (Me 2 N) 4 Hf and normal decane were introduced into the decomposition reactor 4 via a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. Note that the Si substrate 5 is heated to 500 ° C.
【００５３】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００５４】この膜を元素分析により調べた処、Ｈｆを
主成分とするものであることが判った。又、X線回折に
よれば酸化膜であることが判った。When this film was examined by elemental analysis, it was found that the film was mainly composed of Hf. X-ray diffraction revealed that the film was an oxide film.
【００５５】[0055]
【実施例１２】図２の装置を用いてＳｉ基板５上にＨｆ
系酸化膜を作製した。Embodiment 12 Using the apparatus shown in FIG.
A system oxide film was formed.
【００５６】すなわち、（Ｍｅ２Ｎ）４Ｈｆとノルマル
デカンとの混合物（前者：後者＝１：５）を容器１ａ内
に入れ、液体流量制御器７を通して気化器２に送った。
尚、この気化器２では１５０℃にして気化させている。That is, a mixture of (Me 2 N) 4 Hf and normal decane (the former: the latter = 1: 5) was placed in the container 1 a and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 vaporizes at 150 ° C.
【００５７】又、（Ｍｅ２Ｎ）３ＳｉＨとノルマルヘプ
タンとの混合物（前者：後者＝１：５）を容器１ｂ内に
入れ、液体流量制御器７を通して気化器２に送った。
尚、この気化器２では１３０℃にして気化させている。Further, a mixture of (Me 2 N) 3 SiH and normal heptane (the former: the latter = 1: 5) was put in the container 1 b and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 vaporizes at 130 ° C.
【００５８】気化された（Ｍｅ２Ｎ）４Ｈｆ及びノルマ
ルデカン、（Ｍｅ２Ｎ）３ＳｉＨ及びノルマルヘプタン
は、キャリアーガスと共に配管を経て分解反応炉４に導
かれた。又、同時に、反応ガスとして酸素が導入され
た。尚、Ｓｉ基板５は５００℃に加熱されている。The vaporized (Me 2 N) 4 Hf and normal decane, (Me 2 N) 3 SiH and normal heptane were introduced into the decomposition reactor 4 via a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. Note that the Si substrate 5 is heated to 500 ° C.
【００５９】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００６０】この膜を元素分析により調べた処、Ｈｆと
Ｓｉを主成分とするものであることが判った。又、X線
回折によれば酸化膜であることが判った。When this film was examined by elemental analysis, it was found that the film was mainly composed of Hf and Si. X-ray diffraction revealed that the film was an oxide film.
【００６１】[0061]
【実施例１３】図２の装置を用いてＳｉ基板５上にＨｆ
酸化膜を作製した。Embodiment 13 Using the apparatus shown in FIG.
An oxide film was formed.
【００６２】すなわち、（Ｍｅ２Ｎ）４Ｈｆと５％のジ
エチルアミンを含むノルマルデカンとの混合物（前者：
後者＝１：６）を容器１ａ内に入れ、液体流量制御器７
を通して気化器２に送った。尚、この気化器２では１５
０℃にして気化させている。That is, a mixture of (Me 2 N) 4 Hf and normal decane containing 5% of diethylamine (the former:
The latter = 1: 6) is placed in the container 1a and the liquid flow controller 7
And sent to vaporizer 2. In this vaporizer 2, 15
It is vaporized at 0 ° C.
【００６３】気化された（Ｍｅ２Ｎ）４Ｈｆ等はキャリ
アーガスと共に配管を経て分解反応炉４に導かれた。
又、同時に、反応ガスとして酸素が導入された。尚、Ｓ
ｉ基板５は５００℃に加熱されている。The vaporized (Me 2 N) 4 Hf and the like were introduced into the decomposition reaction furnace 4 via a pipe together with the carrier gas.
At the same time, oxygen was introduced as a reaction gas. Note that S
The i-substrate 5 is heated to 500 ° C.
【００６４】その結果、Ｓｉ基板５上に膜が設けられ
た。As a result, a film was provided on the Si substrate 5.
【００６５】この膜を元素分析により調べた処、Ｈｆを
主成分とするものであることが判った。又、X線回折に
よれば酸化膜であることが判った。When this film was examined by elemental analysis, it was found that the film was mainly composed of Hf. X-ray diffraction revealed that the film was an oxide film.
【００６６】[0066]
【発明の効果】ハフニウム系酸化膜が効率良く、かつ、
綺麗に出来る。According to the present invention, a hafnium-based oxide film is efficiently formed, and
I can do it neatly.
【図１】ＣＶＤ装置の概略図FIG. 1 is a schematic view of a CVD apparatus.
【図２】ＣＶＤ装置の概略図FIG. 2 is a schematic view of a CVD apparatus.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4K030 AA06 AA09 AA11 AA18 BA01 BA42 BA44 CA04 FA10 LA15 5F040 DA19 ED03 FC00 5F058 BA20 BC03 BF27 BJ01 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4K030 AA06 AA09 AA11 AA18 BA01 BA42 BA44 CA04 FA10 LA15 5F040 DA19 ED03 FC00 5F058 BA20 BC03 BF27 BJ01
Claims (9)
２はアルキル基、及びシリコン系化合物の基の群の中か
ら選ばれるものであり、Ｒ１とＲ２とは互いに異なって
いても同じであってもよい。〕で表される化合物からな
ることを特徴とするハフニウム系酸化膜形成材料。(1) R 1 R 2 N) 4 Hf [where R 1 , R
2 is selected from the group consisting of an alkyl group and a group of a silicon-based compound, and R 1 and R 2 may be different or the same. ] A hafnium-based oxide film forming material comprising the compound represented by the formula:
の中から選ばれるいずれかであることを特徴とする請求
項１のハフニウム系酸化膜形成材料。2. The hafnium-based oxide film forming material according to claim 1 , wherein R 1 and R 2 are any one selected from the group consisting of a methyl group and an ethyl group.
請求項１又は請求項２のハフニウム系酸化膜形成材料。3. The hafnium-based oxide film forming material according to claim 1, further comprising a Si compound.
割合（重量比）が、前者：後者＝１：１００〜１００
０：１であることを特徴とする請求項３のハフニウム系
酸化膜形成材料。 4. The ratio (weight ratio) of the Si compound to (R 1 R 2 N) 4 Hf is 1: 100-100.
The hafnium-based oxide film forming material according to claim 3, wherein the ratio is 0: 1.
４−ｎ〔但し、Ｒ１，Ｒ２はアルキル基、及びシリコン
系化合物の基の群の中から選ばれるものであり、Ｒ１と
Ｒ２とは互いに異なっていても同じであってもよい。ｎ
は１〜４の整数。〕で表される化合物からなることを特
徴とする請求項３又は請求項４のハフニウム系酸化膜形
成材料。5. The method according to claim 1, wherein the Si compound is (R 1 R 2 N) n SiH.
4-n [where R 1 and R 2 are selected from the group consisting of an alkyl group and a group of a silicon-based compound, and R 1 and R 2 may be different from each other or may be the same. . n
Is an integer of 1 to 4. 5. The material for forming a hafnium-based oxide film according to claim 3, wherein the material is a compound represented by the following formula:
ｔ２Ｎ）３ＳｉＨ，（Ｅｔ２Ｎ）２ＳｉＨ２，（Ｍｅ２
Ｎ）４Ｓｉ，（Ｍｅ２Ｎ）３ＳｉＨ，（Ｍｅ ２Ｎ）２Ｓ
ｉＨ２〔但し、Ｍｅはメチル基、Ｅｔはエチル基。〕の
群の中から選ばれるいずれかであることを特徴とする請
求項３〜請求項５いずれかのハフニウム系酸化膜形成材
料。6. The method according to claim 1, wherein the Si compound is (Et)2N)4Si, (E
t2N)3SiH, (Et2N)2SiH2, (Me2
N)4Si, (Me2N)3SiH, (Me 2N)2S
iH2[However, Me is a methyl group and Et is an ethyl group. 〕of
A signature selected from the group consisting of:
The material for forming a hafnium-based oxide film according to any one of claims 3 to 5.
Fees.
請求項１〜請求項６いずれかのハフニウム系酸化膜形成
材料。7. The material for forming a hafnium-based oxide film according to claim 1, wherein the material is dissolved in a solvent.
物及び炭素数２〜４０のアミン系化合物の群の中から選
ばれる一つ又は二つ以上の化合物であることを特徴とす
る請求項７のハフニウム系酸化膜形成材料。8. The method according to claim 1, wherein the solvent is one or more compounds selected from the group consisting of hydrocarbon compounds having 5 to 40 carbon atoms and amine compounds having 2 to 40 carbon atoms. Item 7. A hafnium-based oxide film forming material according to Item 7.
化膜を形成する為のものであることを特徴とする請求項
１〜請求項８いずれかのハフニウム系酸化膜形成材料。9. The hafnium-based oxide film forming material according to claim 1, which is for forming a hafnium-based oxide film by a chemical vapor deposition method.
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