JP3409290B2 - Gate oxide film forming material - Google Patents
Gate oxide film forming materialInfo
- Publication number
- JP3409290B2 JP3409290B2 JP2000282198A JP2000282198A JP3409290B2 JP 3409290 B2 JP3409290 B2 JP 3409290B2 JP 2000282198 A JP2000282198 A JP 2000282198A JP 2000282198 A JP2000282198 A JP 2000282198A JP 3409290 B2 JP3409290 B2 JP 3409290B2
- Authority
- JP
- Japan
- Prior art keywords
- oxide film
- gate oxide
- group
- compound
- sih
- 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 - Fee Related
Links
- 239000000463 material Substances 0.000 title claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 39
- 229910052735 hafnium Inorganic materials 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 9
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- -1 amine compound Chemical class 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000002210 silicon-based material Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 description 23
- 239000006200 vaporizer Substances 0.000 description 10
- 239000012159 carrier gas Substances 0.000 description 9
- 238000000354 decomposition reaction Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 6
- 238000000921 elemental analysis Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 239000012495 reaction gas Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 229910000449 hafnium oxide Inorganic materials 0.000 description 2
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910004129 HfSiO Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Formation Of Insulating Films (AREA)
- Insulated Gate Type Field-Effect Transistor (AREA)
- Chemical Vapour Deposition (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明はゲート酸化膜形成材
料に関する。TECHNICAL FIELD The present invention relates to a gate oxide film forming material.
Regarding fees .
【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 progress of ULSI, the distance between the source and drain of a transistor has become shorter. At the same time, the thickness of the gate oxide film is becoming thinner. By the way, the film thickness is 10 nm
It is expected to be below.
【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。By the way, at present, the gate oxide film is SiO 2
However, when the thickness of the SiO 2 gate oxide film reaches 3 nm or less, the 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。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。However, it is not simply 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 has been reported that since hafnium forms hafnium silicate (HfSiO 4 ) at the interface with silicon, it does not oxidize 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 convenient as the 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。Further, the step coverage is poor. For example, when an attempt is made to form a film on a substrate whose surface is not flat but has irregularities, the film may not be formed on the bottom surface of the recess. 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
ゲート酸化膜を提供することである。Accordingly, the problem to be solved by the present invention is
It is to provide a gate oxide film .
【００１３】[0013]
【課題を解決するための手段】前記の課題は、Ｓｉ層上
に設けられるハフニウム系酸化膜からなるゲート酸化膜
の形成材料であって、（Ｒ１Ｒ２Ｎ）４Ｈｆ〔但し、Ｒ
１，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ゲート酸化膜形成材料によっ
て解決される。[Means for Solving the Problems] The above-mentioned problems are caused on the Si layer.
A material for forming a gate oxide film made of a hafnium-based oxide film, which is (R 1 R 2 N) 4 Hf [however, R
1 and R 2 are selected from the group of alkyl groups and groups of silicon compounds, and R 1 and R 2 may be different from each other or the same. ] A gate oxide film forming material characterized by comprising a compound represented by
【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
特徴とするゲート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 [however,
R 1 and R 2 are any one selected from the group consisting of a methyl group and an ethyl group. ] A gate oxide film forming material characterized by comprising a compound represented by
【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ゲート酸化膜形
成材料によって解決される。Among them, (Me 2 N) 4 Hf, (Et
2 N) 4 Hf and / or (Et (Me) N) 4 gate oxide film type, characterized in that a compound represented by Hf
Solved by synthetic materials .
【００１６】上記化合物を用いることによって優れたゲ
ート酸化膜を効率良く形成できる。By using the above compound, excellent properties can be obtained.
The over gate oxide film can be formed efficiently.
【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ゲート酸化膜を形成できる。However, not only (R 1 R 2 N) 4 Hf, but also (R 1 R 2 N) 4 Hf and a Si compound can be used to form a film. That is, (R 1 R 2 N) 4 Hf and S
By using the i compound together, a gate 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
るゲート酸化膜形成材料によって解決される。Therefore, the above-mentioned problems are (R 1 R 2 N) 4
Hf [wherein 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
2 may be different from each other or may be the same. ] A gate oxide film forming material characterized by containing a compound represented by the above formula and a Si compound.
【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ゲート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 [however,
R 1 and R 2 are any one selected from the group consisting of a methyl group and an ethyl group. ] A gate oxide film forming material characterized by containing a compound represented by the above and a Si compound.
【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
ゲート酸化膜形成材料によって解決される。Among them, (Me 2 N) 4 Hf, (Et
2 N) 4 Hf and / or a compound represented by (Et (Me) N) 4 Hf and a Si compound.
It is solved by the gate oxide film forming material .
【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 above Si compound is preferably (R
1 R 2 N) n SiH 4-n [wherein 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 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 [However, Me is a methyl group, Et is an ethyl group. ] Any one selected from the group.
【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 the compound represented by (R 1 R 2 N) 4 Hf and the Si compound are used together,
Ratio of Si compound and (R 1 R 2 N) 4 Hf (weight ratio)
Is preferably: former: latter = 1: 100 to 1000:
It is 1. More preferably, it is 1:50 to 100: 1.
【００２３】上記のゲート酸化膜形成材料は、溶媒を更
に含む形態のものが好ましい。すなわち、上記のは溶媒
中に溶解してなる形態のものが好ましい。The above-mentioned gate oxide film forming material preferably has a form further containing a solvent. That is, the above-mentioned one is preferably 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。Any solvent may be used as long as it can dissolve the hafnium-based oxide film forming material. Among them, a compound whose solvent is preferably 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.
【００２５】[0025]
【発明の実施の形態】本発明になるゲート酸化膜形成材
料は、Ｓｉ層上に設けられるハフニウム系酸化膜からな
るゲート酸化膜の形成材料であって、（Ｒ１Ｒ２Ｎ）４
Ｈｆ〔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、（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。中でも、
（Ｍｅ２Ｎ）４Ｈｆ，（Ｅｔ２Ｎ）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 A gate oxide film forming material according to the present invention is a material for forming a gate oxide film made of a hafnium-based oxide film provided on a Si layer , which is (R 1 R 2 N) 4
Hf [however, R 1 and R 2 are alkyl groups (especially, carbon number 1
~ 12 alkyl groups) and a group of silicon-based compounds, and R 1 and R 2 may be different or the same. ] It consists of the compound represented by these. In particular, (R 1 R 2 N) 4 Hf [provided that R 1 ,
R 2 is any one selected from the group of methyl group and ethyl group. ] It consists of the compound represented by these. Above all,
It is composed of a compound represented by (Me 2 N) 4 Hf, (Et 2 N) 4 Hf and / or (Et (Me) N) 4 Hf (Me is a methyl group and 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。In addition, (R1RTwoN)FourNot just Hf,
(R1RTwoN)FourHf [Same as above. ] Compound represented by
And a Si compound. In particular, (R1R
TwoN)FourHf [however, R1, RTwoIs methyl and ethyl
It is one selected from the group of groups. ]
It includes a compound and a Si compound. Above all,
(MeTwoN)FourHf, (EtTwoN)FourHf and / or
(Et (Me) N)FourCompound represented by Hf and Si conversion
It includes a compound. As this Si compound,
More preferably (R1RTwoN)nSiH4-n[However, R1，
RTwoIs a group of alkyl groups and groups of silicon compounds
R is selected from1And RTwoDifferent from
Or they may be the same. n is an integer of 1 to 4. 〕so
It is the compound represented. Above all, (EtTwoN)FourSi,
(EtTwoN)ThreeSiH, (EtTwoN) TwoSiHTwo, (M
eTwoN)FourSi, (MeTwoN)ThreeSiH, (MeTwoN)
TwoSiHTwo[However, Me is a methyl group, Et is ethyl
Basis. ] Any one selected from the group. (R1R
TwoN)FourUses both Hf and Si compounds
In case of adding Si compound and (R1RTwoN)FourWith Hf
The ratio (weight ratio) is preferably the former: the latter = 1: 10.
It is 0 to 1000: 1. More preferably, from 1:50
It is 100: 1.
【００２７】本発明になるゲート酸化膜形成材料は、必
要に応じて、溶媒を更に含む。すなわち、上記のゲート
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 material for forming a gate oxide film according to the present invention further contains a solvent, if necessary. Ie the above gate
The oxide film forming material is preferably in the form of being dissolved in a solvent. Such a solvent may be one that can dissolve the above materials. Among them, a compound whose solvent is preferably 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. Specifically, examples of the hydrocarbon 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 1 to 10000 parts by weight, particularly 100 parts by weight, based on 100 parts by weight of the hafnium-based oxide film forming material.
It is preferably ˜2000 parts by weight.
【００２８】本発明の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、本発明の材料は、化学気相
成長方法によりゲート酸化膜を形成する為のものであ
る。The film formed from the material of the present invention is of the oxide film type. The material of the present invention is for forming a gate 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。A specific example will be described below.
【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。EXAMPLE 1 FIG. 1 is a schematic view of an apparatus for carrying out the 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 vessels, 3 is a heater, 4 is a decomposition reaction furnace, 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, in the container 1a, (Et 2 N) 4 H
While f was charged and heated to 100 ° C., nitrogen gas (carrier gas) was supplied at a rate of 30 ml / min. Then, the vaporized (Et 2 N) 4 Hf was introduced into the decomposition reaction furnace 4 through a pipe together with the carrier gas. At the same time,
Oxygen was introduced as the 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。When the film was examined by elemental analysis, it was found that Hf was the main component. Further, it was found by X-ray diffraction that it was an Hf oxide film.
【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 the 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 the 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。Example 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, in the container 1a, (Et 2 N) 4 H
While f was charged and heated to 100 ° C., 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 container 1b and heated to 80 ° C., and 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 through 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。As a result of examining this film by elemental analysis, Hf
It was found that the main components were Si and Si. or,
X-ray diffraction revealed that it 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。Example 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 equal amount of N) 3 SiH mixture was placed in the container 1 a and sent to the vaporizer 2 through the liquid flow controller 7. The vaporizer 2 is vaporized 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。Vaporized (Et 2 N) 4 Hf and (Et 2 N
N) 3 SiH was introduced into the decomposition reaction furnace 4 through 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 it was composed mainly of Hf and Si. Also, X
It was found by line diffraction that it 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, (EtTwoN)Three
Instead of SiH, (EtTwoN)FourSi, (EtTwoN)
TwoSiHTwo, (MeTwoN)FourSi, (MeTwoN)ThreeSi
H, (Me TwoN)TwoSiHTwoThe same line except using
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] Hf is formed on a Si substrate 5 by using the apparatus shown in FIG.
An oxide film was produced.
【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 (former: latter = 1: 5) was placed in the container 1a and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 is vaporized 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 reaction furnace 4 through a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. 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 Hf was the main component. Also, it was found by X-ray diffraction that it 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] Hf is formed on a Si substrate 5 by using the apparatus shown in FIG.
A system oxide film was prepared.
【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 (former: latter = 1: 5) was placed in the container 1a and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 is vaporized 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。A mixture of (Me 2 N) 3 SiH and normal heptane (former: latter = 1: 5) was placed in the container 1b and sent to the vaporizer 2 through the liquid flow controller 7.
The vaporizer 2 is vaporized 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 through a pipe together with a carrier gas. At the same time, oxygen was introduced as a reaction gas. 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 it had Hf and Si as main components. Also, it was found by X-ray diffraction that it 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] Hf is formed on the Si substrate 5 by using the apparatus of FIG.
An oxide film was produced.
【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 put in the container 1a, and the liquid flow rate controller 7
To vaporizer 2. In addition, 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 through a pipe together with the carrier gas.
At the same time, oxygen was introduced as a reaction gas. Incidentally, 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 Hf was the main component. Also, it was found by X-ray diffraction that it was an oxide film.
【００６６】[0066]
【発明の効果】例えば、下層のシリコンを酸化させるこ
とが無いゲート酸化膜を効率良く、かつ、きれいに出来
る。 [Effects of the Invention] For example, it is possible to oxidize lower silicon
Efficient and clean gate oxide film
It
【図１】ＣＶＤ装置の概略図FIG. 1 is a schematic diagram of a CVD apparatus.
【図２】ＣＶＤ装置の概略図FIG. 2 is a schematic diagram of a CVD apparatus.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C23C 16/00 - 16/56 H01L 21/316 ─────────────────────────────────────────────────── ─── Continuation of the front page (58) Fields surveyed (Int.Cl. 7 , DB name) C23C 16/00-16/56 H01L 21/316
Claims (9)
膜からなるゲート酸化膜の形成材料であって、 （Ｒ１Ｒ２Ｎ）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
とするゲート酸化膜形成材料。1. A material for forming a gate oxide film comprising a hafnium-based oxide film provided on a Si layer , wherein (R 1 R 2 N) 4 Hf [wherein R 1 and R 2 are alkyl groups and silicon It is selected from the group of groups of the system compounds, and R 1 and R 2 may be different from each other or the same. ] A gate oxide film-forming material comprising a compound represented by
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のゲート酸化膜形成材料。2. The material for forming a gate oxide film 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のゲート酸化膜形成材料。3. The gate 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のゲート酸化膜
形成材料。 4. The ratio (weight ratio) of the Si compound and (R 1 R 2 N) 4 Hf is such that the former: the latter = 1: 100 to 100.
The gate oxide film forming material according to claim 3, wherein the material 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のゲート酸化膜形成材
料。5. The Si compound is (R 1 R 2 N) n SiH.
4-n [wherein 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 the same or different from each other. . n
Is an integer from 1 to 4. ] The gate oxide film forming material of Claim 3 or Claim 4 which consists of a compound represented by these.
ｔ２Ｎ）３ＳｉＨ，（Ｅｔ２Ｎ）２ＳｉＨ２，（Ｍｅ２
Ｎ）４Ｓｉ，（Ｍｅ２Ｎ）３ＳｉＨ，（Ｍｅ２Ｎ）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いずれかのゲート酸化膜形成材料。6. The Si compound is (Et 2 N) 4 Si, (E
t 2 N) 3 SiH, (Et 2 N) 2 SiH 2 , (Me 2
N) 4 Si, (Me 2 N) 3 SiH, (Me 2 N) 2 S
iH 2 [However, Me is a methyl group, Et is an ethyl group. ] The gate oxide film forming material according to any one of claims 3 to 5, which is any one selected from the group.
請求項１〜請求項６いずれかのゲート酸化膜形成材料。7. The material for forming a gate 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のゲート酸化膜形成材料。8. The solvent is one or more compounds 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. Item 7. A gate oxide film forming material according to item 7.
化膜からなるゲート酸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いずれかのゲート酸
化膜形成材料。9. The material for forming a gate oxide film according to claim 1, which is for forming a gate oxide film made of a hafnium-based oxide film by a chemical vapor deposition method.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7507848B2 (en) | 2000-09-28 | 2009-03-24 | President And Fellows Of Harvard College | Vapor deposition of metal oxides, silicates and phosphates, and silicon dioxide |
| US8536070B2 (en) | 2002-03-28 | 2013-09-17 | President And Fellows Of Harvard College | Vapor deposition of silicon dioxide nanolaminates |
Families Citing this family (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| US7507848B2 (en) | 2000-09-28 | 2009-03-24 | President And Fellows Of Harvard College | Vapor deposition of metal oxides, silicates and phosphates, and silicon dioxide |
| US8334016B2 (en) | 2000-09-28 | 2012-12-18 | President And Fellows Of Harvard College | Vapor deposition of metal oxides, silicates and phosphates, and silicon dioxide |
| US9905414B2 (en) | 2000-09-28 | 2018-02-27 | President And Fellows Of Harvard College | Vapor deposition of metal oxides, silicates and phosphates, and silicon dioxide |
| US8536070B2 (en) | 2002-03-28 | 2013-09-17 | President And Fellows Of Harvard College | Vapor deposition of silicon dioxide nanolaminates |
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