JP2661815B2 - Flattening film - Google Patents
Flattening filmInfo
- Publication number
- JP2661815B2 JP2661815B2 JP16344991A JP16344991A JP2661815B2 JP 2661815 B2 JP2661815 B2 JP 2661815B2 JP 16344991 A JP16344991 A JP 16344991A JP 16344991 A JP16344991 A JP 16344991A JP 2661815 B2 JP2661815 B2 JP 2661815B2
- Authority
- JP
- Japan
- Prior art keywords
- flattening
- film
- silicon oxide
- oxide film
- sicl
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- -1 ethylenediamine Chemical compound 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 229940022663 acetate Drugs 0.000 description 4
- 150000001346 alkyl aryl ethers Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000008096 xylene Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 2
- OJVAMHKKJGICOG-UHFFFAOYSA-N 2,5-hexanedione Chemical compound CC(=O)CCC(C)=O OJVAMHKKJGICOG-UHFFFAOYSA-N 0.000 description 2
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 2
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 229920001709 polysilazane Polymers 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- UXDDRFCJKNROTO-UHFFFAOYSA-N Glycerol 1,2-diacetate Chemical compound CC(=O)OCC(CO)OC(C)=O UXDDRFCJKNROTO-UHFFFAOYSA-N 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910003925 SiC 1 Inorganic materials 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000001089 [(2R)-oxolan-2-yl]methanol Substances 0.000 description 1
- XMUZQOKACOLCSS-UHFFFAOYSA-N [2-(hydroxymethyl)phenyl]methanol Chemical compound OCC1=CC=CC=C1CO XMUZQOKACOLCSS-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000003974 aralkylamines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229940007550 benzyl acetate Drugs 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- DLAHAXOYRFRPFQ-UHFFFAOYSA-N dodecyl benzoate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1 DLAHAXOYRFRPFQ-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229940117803 phenethylamine Drugs 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- BSYVTEYKTMYBMK-UHFFFAOYSA-N tetrahydrofurfuryl alcohol Chemical compound OCC1CCCO1 BSYVTEYKTMYBMK-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
- Formation Of Insulating Films (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は新規な平坦化膜、さらに
詳しくは、厚膜でもクラックが発生することがなく、特
に段差を有する基板に対し、優れた平坦化作用を示す平
坦化膜に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a novel flattening film, and more particularly, to a flattening film which is free from cracks even in a thick film and exhibits an excellent flattening effect particularly on a substrate having a step. Things.
【０００２】[0002]
【従来の技術】近年、半導体素子においては、回路の高
集積化や微細化の方向に進んでおり、また回路パターン
も多層化の方向にある。そして、多層化に伴い、回路パ
ターンを積層する必要があるため、基板の凹凸を埋め、
平坦化する技術が重要となってきている。2. Description of the Related Art In recent years, semiconductor devices have been moving toward higher integration and miniaturization of circuits, and circuit patterns have also been moving toward multilayering. And, with the increase in the number of layers, it is necessary to stack circuit patterns, so fill in the unevenness of the substrate,
The technology of flattening is becoming important.
【０００３】この平坦化の方法としては、従来アルコキ
シシランやハロゲノシランの加水分解反応生成物から成
る塗布液を、凹凸を有する基板上に塗布、乾燥すること
により、酸化ケイ素膜を形成させる方法が用いられてい
る。As a method of flattening, a method of forming a silicon oxide film by applying a coating solution comprising a hydrolysis reaction product of an alkoxysilane or a halogenosilane on a substrate having irregularities and drying the coating solution is conventionally used. Used.
【０００４】しかしながら、前記塗布液から形成された
酸化ケイ素膜は、厚膜にするとクラックが発生しやすく
て厚膜にできないため平坦化作用に劣り、所望の平坦化
を達成するためには、数回の重ね塗りが必要であって、
作業が煩雑になるのを免れないという欠点を有してい
る。したがって、厚膜でもクラックが発生することがな
く、良好な平坦化作用を示す平坦化膜の開発が強く望ま
れていた。However, a silicon oxide film formed from the above-mentioned coating solution is inferior in flattening effect because cracks are liable to occur in a thick film and cannot be made thick. Need to be repainted several times,
There is a disadvantage that the operation is inevitably complicated. Therefore, there has been a strong demand for the development of a flattening film that does not cause cracks even in a thick film and exhibits good flattening action.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、このような
要望にこたえ、厚膜でもクラックが発生することがな
く、特に段差を有する基板に対して優れた平坦化作用を
有する平坦化膜を提供することを目的としてなされたも
のである。SUMMARY OF THE INVENTION In order to meet such a demand, the present invention provides a flattening film which does not cause cracks even in a thick film and has an excellent flattening effect particularly on a substrate having a step. It was made for the purpose of providing.
【０００６】[0006]
【課題を解決するための手段】本発明者らは、厚膜でも
クラックが発生しない酸化ケイ素膜について鋭意研究を
重ねた結果、非水条件下で形成された酸化ケイ素膜は厚
膜でもクラックを発生することがなく、優れた平坦化作
用を有することを見い出し、この知見に基づいて本発明
を完成するに至った。Means for Solving the Problems The present inventors have conducted intensive studies on a silicon oxide film in which cracks do not occur even in a thick film, and as a result, the silicon oxide film formed under non-aqueous conditions has cracks even in a thick film. It has been found that they do not occur and have an excellent flattening action, and the present invention has been completed based on this finding.
【０００７】すなわち、本発明は、非水条件下で形成さ
れた酸化ケイ素膜から成る平坦化膜を提供するものであ
る。That is, the present invention provides a flattening film made of a silicon oxide film formed under non-aqueous conditions.
【０００８】本発明でいう「非水条件下」とは、水の不
存在下及び水の生成を伴わない条件下を意味する。従来
の平坦化膜として用いられている酸化ケイ素膜は、水の
存在下又は水が生成する条件下で形成されるため、その
赤外吸収スペクトルにおいて、水の存在に起因する波数
３２００〜３６００ｃｍ−１の範囲にピークが存在する
のに対し、本発明の平坦化膜として用いられている酸化
ケイ素膜は、前記波数の範囲に実質上ピークが存在しな
いという点で、両者の間は明らかに組成上の差異が認め
られる。[0008] The term "non-aqueous conditions" as used herein means conditions in the absence of water and without the production of water. Since a silicon oxide film used as a conventional planarization film is formed in the presence of water or under conditions in which water is generated, its infrared absorption spectrum has a wavenumber of 3200 to 3600 cm − due to the presence of water. 1 , whereas the silicon oxide film used as the flattening film of the present invention has a clear composition between the two in that there is substantially no peak in the wave number range. The above differences are observed.
【０００９】このような特徴をもつ酸化ケイ素膜は、例
えば固体表面に、シラザン化合物の有機溶剤溶液を塗布
し、次いでこれを酸化雰囲気中で焼成することによって
得られる。このシラザン化合物は、分子中にＳｉ‐Ｎ結
合を有する化合物の総称であるが、本発明においては、
分子中に酸素原子を含まないシラザン化合物を用いるの
が好ましい。A silicon oxide film having such characteristics can be obtained, for example, by applying an organic solvent solution of a silazane compound to a solid surface and then firing the solution in an oxidizing atmosphere. This silazane compound is a general term for a compound having a Si—N bond in a molecule, but in the present invention,
It is preferable to use a silazane compound containing no oxygen atom in the molecule.
【００１０】このようなシラザン化合物は、ハロゲノシ
ランやオルガノハロゲノシランとアンモニア又はアミン
類とを、有機溶媒中で反応させることによって得られ
る。この際用いられるハロゲノシランとしては、例えば
ＳｉＣｌ４、ＨＳｉＣｌ３、Ｈ2ＳｉＣｌ2、Ｈ3ＳｉＣ
ｌなどを挙げることができるし、また、オルガノハロゲ
ノシランとしては、例えばＣＨ３ＳｉＨＣｌ２、ＣＨ３
ＳｉＨ２Ｃｌ、ＣＨ3ＳｉＣｌ3、(ＣＨ3)２ＳｉＣｌ2、
（ＣＨ3）3ＳｉＣｌ、Ｃ2Ｈ5ＳｉＣｌ３、（Ｃ2Ｈ5）3
ＳｉＣｌ、（Ｃ2Ｈ5）（Ｃ6Ｈ5）ＳｉＣｌ２、（Ｃ
2Ｈ5)(Ｃ6Ｈ5)２ＳｉＣｌ、（ＣＨ３）３ＣＳｉＨＣｌ
２、（ＣＨ３）２ＣＨＳｉＨＣｌ2、（Ｃ6Ｈ5）ＳｉＨ
Ｃｌ２、（Ｃ６Ｈ５）ＳｉＣｌ3、（Ｃ６Ｈ５）２Ｓｉ
Ｃｌ２、（Ｃ6Ｈ5）3ＳｉＣｌ、Ｃ6Ｈ5ＣＨ2ＳｉＣ
ｌ3、（Ｃ6Ｈ５ＣＨ２）２ＳｉＣｌ２、（Ｃ６Ｈ５ＣＨ
２）３ＳｉＣｌなどを挙げることができる。Such a silazane compound is obtained by reacting a halogenosilane or an organohalogenosilane with ammonia or an amine in an organic solvent. The halogenosilane used at this time is, for example, SiCl 4 , HSiCl 3 , H 2 SiCl 2 , H 3 SiC
1 and the like, and examples of the organohalogenosilane include, for example, CH 3 SiHCl 2 and CH 3
SiH 2 Cl, CH 3 SiCl 3 , (CH 3 ) 2 SiCl 2 ,
(CH 3 ) 3 SiCl, C 2 H 5 SiCl 3 , (C 2 H 5 ) 3
SiCl, (C 2 H 5 ) (C 6 H 5 ) SiCl 2 ,
2 H 5) (C 6 H 5) 2 SiCl, (CH 3) 3 CSiHCl
2 , (CH 3 ) 2 CHSiHCl 2 , (C 6 H 5 ) SiH
Cl 2 , (C 6 H 5 ) SiCl 3 , (C 6 H 5 ) 2 Si
Cl 2 , (C 6 H 5 ) 3 SiCl, C 6 H 5 CH 2 SiC
l 3 , (C 6 H 5 CH 2 ) 2 SiCl 2 , (C 6 H 5 CH
2 ) 3 SiCl and the like.
【００１１】一方、これらのハロゲノシランやオルガノ
ハロゲノシランと反応させるアミン類としては、例えば
モノメチルアミン、エチルアミン、プロピルアミン、ブ
チルアミンなどの低級アルキルアミンやエチレンジアミ
ンなどのポリアミン、ベンジルアミン、フェネチルアミ
ンなどのアラルキルアミンなどを挙げることができる。On the other hand, examples of amines to be reacted with these halogenosilanes and organohalogenosilanes include lower alkylamines such as monomethylamine, ethylamine, propylamine and butylamine, polyamines such as ethylenediamine, and aralkylamines such as benzylamine and phenethylamine. And the like.
【００１２】また、これらの反応に用いる有機溶媒とし
ては、例えばトルエン、キシレン、ジエチルエーテル、
ジクロロメタンなどが挙げられる。The organic solvents used in these reactions include, for example, toluene, xylene, diethyl ether,
Dichloromethane and the like.
【００１３】特に好適なシラザン化合物は、前記有機溶
媒中に、ＨＳｉＣｌ３、Ｈ２ＳｉＣｌ２、Ｈ３ＳｉＣｌ
などのハロゲノシランを溶解し、これにアンモニアガス
を吹き込むことによって得られるものである。Particularly preferred silazane compounds include HSiCl 3 , H 2 SiCl 2 , and H 3 SiCl in the organic solvent.
Is obtained by dissolving such halogenosilane and blowing ammonia gas into it.
【００１４】本発明においては、このようにして得られ
たハロゲノシラン又はオルガノハロゲノシランとアンモ
ニア又はアミン類との反応混合物をそのまま塗布液とす
ることもできるし、またこの反応混合物から減圧蒸留な
どにより溶媒を除去して、所望のシラザン化合物を油状
物質又は固体物質として回収したのち、これを適当な有
機溶剤に溶解し塗布液とすることもできる。In the present invention, the reaction mixture of the halogenosilane or organohalogenosilane thus obtained and ammonia or amines can be used as it is as a coating solution, or the reaction mixture can be subjected to distillation under reduced pressure or the like. After removing the solvent and recovering the desired silazane compound as an oily substance or a solid substance, this can be dissolved in a suitable organic solvent to prepare a coating solution.
【００１５】この場合の有機溶剤としては、例えばメタ
ノール、エタノール、プロパノール、ブタノール、シク
ロヘキサノール、ベンジルアルコール、ジメチロールベ
ンゼン、フルフリルアルコール、テトラヒドロフルフリ
ルアルコール、ジアセトンアルコール、エチレングリコ
ールモノアルキルエーテル、ジエチレングリコールモノ
アルキルエーテル、トリエチレングリコールモノアルキ
ルエーテル、プロピレングリコールモノアルキルエーテ
ルなどのアルコール類、酢酸アルキルエステル、ジエチ
レングリコールモノアルキルエーテルアセテート、トリ
エチレングリコールモノアルキルエーテルアセテート、
プロピレングリコールモノアルキルエーテルアセテー
ト、アセト酢酸エチルエステル、乳酸アルキルエステ
ル、安息香酸アルキルエステル、ベンジルアセテート、
グリセリンジアセテートなどのエステル類、アセトン、
メチルエチルケトン、シクロヘキサノン、アセチルアセ
トン、イソホロン、ジエチルケトン、メチルイソブチル
ケトン、メチルｎ‐ブチルケトン、アセトニルアセトン
などのケトン類、ｎ‐ペンタン、ｎ‐ヘキサン、イソヘ
キサン、ｎ‐ヘプタン、ｎ‐オクタン、イソオクタン、
ベンゼン、トンエン、キシレン、エチルベンゼン、ジエ
チルベンゼン、イソプロピルベンゼン、テトラリンなど
の炭化水素類などが挙げられる。これらの有機溶剤は単
独で用いてもよいし、２種以上を混合して用いてもよ
い。Examples of the organic solvent in this case include methanol, ethanol, propanol, butanol, cyclohexanol, benzyl alcohol, dimethylolbenzene, furfuryl alcohol, tetrahydrofurfuryl alcohol, diacetone alcohol, ethylene glycol monoalkyl ether, diethylene glycol. Alcohols such as monoalkyl ether, triethylene glycol monoalkyl ether, propylene glycol monoalkyl ether, alkyl acetate, diethylene glycol monoalkyl ether acetate, triethylene glycol monoalkyl ether acetate,
Propylene glycol monoalkyl ether acetate, ethyl acetoacetate, alkyl lactate, alkyl benzoate, benzyl acetate,
Esters such as glycerin diacetate, acetone,
Ketones such as methyl ethyl ketone, cyclohexanone, acetylacetone, isophorone, diethyl ketone, methyl isobutyl ketone, methyl n-butyl ketone, acetonylacetone, n-pentane, n-hexane, isohexane, n-heptane, n-octane, isooctane,
Examples thereof include hydrocarbons such as benzene, toluene, xylene, ethylbenzene, diethylbenzene, isopropylbenzene, and tetralin. These organic solvents may be used alone or as a mixture of two or more.
【００１６】本発明の平坦化膜の形成に用いられる塗布
液としては、シラザン化合物を１〜６０重量％、好まし
くは１０〜３０重量％の割合で含有し、かつ常温におけ
る粘度が０．５〜５０センチポイズ、好ましくは１〜２
０センチポイズの範囲にあるものが実用上好適である。
該粘度は所望の膜厚などによって、有機溶剤の種類や量
を適宜選択することにより、調整することができる。The coating solution used for forming the flattening film of the present invention contains a silazane compound at a ratio of 1 to 60% by weight, preferably 10 to 30% by weight, and has a viscosity at room temperature of 0.5 to 0.5%. 50 centipoise, preferably 1-2
Those in the range of 0 centipoise are practically suitable.
The viscosity can be adjusted by appropriately selecting the type and amount of the organic solvent depending on the desired film thickness and the like.
【００１７】本発明の平坦化膜は、前記のようにして調
製された塗布液を、例えばアルミニウムの回路パターン
を有するシリコンウエハー上にスピンナー法、スプレー
法、浸せき法など、従来慣用されている手段により塗布
したのち、５０〜２００℃程度の温度で乾燥してポリシ
ラザン系被膜を形成させ、次いで大気中又は酸素雰囲気
中で、通常２００〜８００℃の範囲の温度において、１
５〜６０分間程度焼成し、該ポリシラザン系被膜を酸化
ケイ素膜に転化することにより、形成することができ
る。The flattening film of the present invention can be obtained by coating the coating solution prepared as described above on a silicon wafer having an aluminum circuit pattern, for example, by a spinner method, a spray method, or a dipping method. And then dried at a temperature of about 50 to 200 ° C. to form a polysilazane-based coating, and then in air or an oxygen atmosphere at a temperature usually in the range of 200 to 800 ° C.
It can be formed by baking for about 5 to 60 minutes and converting the polysilazane-based film into a silicon oxide film.
【００１８】このようにして形成された平坦化膜は、膜
厚が０．２〜３．０μｍのクラックのない均質な吸湿性
の低い酸化ケイ素膜から成る連続膜であるが、本発明の
目的がそこなわれない範囲で窒素原子や炭素原子が含有
されていてもよい。The flattening film thus formed is a continuous film made of a crack-free homogeneous silicon oxide film having a low hygroscopicity and having a thickness of 0.2 to 3.0 μm. May be contained to the extent that is not impaired.
【００１９】[0019]
【発明の効果】本発明の平坦化膜は吸湿性が低く、均質
でち密な酸化ケイ素膜から成るものであって、厚膜にし
てもクラックが発生することがなく、平坦化作用に優れ
ており、例えば半導体素子や液晶表示素子などの基板の
平坦化に好適に用いられる。The flattening film of the present invention is made of a uniform and dense silicon oxide film having low hygroscopicity. Even if it is a thick film, no cracks are generated and the flattening effect is excellent. For example, it is suitably used for flattening substrates such as semiconductor elements and liquid crystal display elements.
【００２０】[0020]
【実施例】次に、実施例により本発明をさらに詳細に説
明するが、本発明はこれらの例によってなんら限定され
るものではない。Next, the present invention will be described in more detail by way of examples, but the present invention is not limited to these examples.
【００２１】実施例 ハロゲノシランとアンモニアとの反応生成物の２０重量
％キシレン溶液であるＴＥＦＰ（東燃社製）を、アルミ
ニウムパターンが形成された１．０μｍの段差を有する
シリコンウエハー上に、キシレン雰囲気中５００ｒｐｍ
でスピン塗布し、１５０℃で３０分間乾燥したのち、大
気中で５００℃にて６０分間焼成することにより、酸化
ケイ素膜を形成させた。この酸化ケイ素膜は膜厚が１．
５μｍであり、表面にクラックの発生が認められず、段
差部分の平坦化作用に優れた極めて均質性の高い被膜で
あった。また、得られた被膜の赤外吸収スペクトルから
は水の存在は確認できなかった。EXAMPLE A TEFP (manufactured by Tonen Co., Ltd.), a 20% by weight xylene solution of a reaction product of halogenosilane and ammonia, was placed on a silicon wafer having an aluminum pattern and having a step of 1.0 μm in a xylene atmosphere. Medium 500rpm
And dried at 150 ° C. for 30 minutes, and then baked at 500 ° C. for 60 minutes in the air to form a silicon oxide film. This silicon oxide film has a thickness of 1.
The thickness was 5 μm, no cracks were observed on the surface, and the coating was extremely uniform and excellent in flattening action at the stepped portion. The presence of water could not be confirmed from the infrared absorption spectrum of the obtained coating.
【００２２】比較例 テトラエトキシシランをエチルアルコールの存在下で部
分加水分解して得られたＳｉＯ２換算濃度が１２重量％
の塗布液を用いた以外は、実施例と同様な操作により酸
化ケイ素膜を形成させた。COMPARATIVE EXAMPLE Tetraethoxysilane was partially hydrolyzed in the presence of ethyl alcohol to obtain a concentration of 12% by weight in terms of SiO 2.
A silicon oxide film was formed in the same manner as in the example except that the coating liquid of Example 1 was used.
【００２３】この酸化ケイ素膜は、段差部分にクラック
が発生し、平坦化作用に劣るものであった。また、この
酸化ケイ素膜の赤外吸収スペクトルから、水に起因する
３２００〜３６００ｃｍ−１の範囲に吸収ピークが確認
された。In this silicon oxide film, cracks were generated at the step portions, and the silicon oxide film was poor in flattening action. From the infrared absorption spectrum of this silicon oxide film, an absorption peak was observed in the range of 3200 to 3600 cm −1 due to water.
Claims (1)
ら成る平坦化膜。1. A flattening film comprising a silicon oxide film formed under non-aqueous conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16344991A JP2661815B2 (en) | 1991-06-10 | 1991-06-10 | Flattening film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16344991A JP2661815B2 (en) | 1991-06-10 | 1991-06-10 | Flattening film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0532410A JPH0532410A (en) | 1993-02-09 |
| JP2661815B2 true JP2661815B2 (en) | 1997-10-08 |
Family
ID=15774094
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16344991A Expired - Lifetime JP2661815B2 (en) | 1991-06-10 | 1991-06-10 | Flattening film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2661815B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0611067B1 (en) * | 1993-02-05 | 1999-03-10 | Dow Corning Corporation | Coating electronic substrates with silica derived from silazane polymers |
| JP2790163B2 (en) * | 1993-07-29 | 1998-08-27 | 富士通株式会社 | Method for forming silicon oxide film, method for manufacturing semiconductor device, and method for manufacturing flat display device |
| JP3417464B2 (en) | 1998-06-24 | 2003-06-16 | 東京応化工業株式会社 | Coating liquid for flattening film formation |
| JP5299935B2 (en) * | 2001-05-17 | 2013-09-25 | 三菱レイヨン株式会社 | Nonionic or anionic water-soluble acrylamide polymer and process for producing the same |
| CN100444331C (en) * | 2003-11-11 | 2008-12-17 | 三星电子株式会社 | Spin-on-glass composition and method of forming silicon oxide layer using the spin-on-glass in semiconductor manufacturing process |
-
1991
- 1991-06-10 JP JP16344991A patent/JP2661815B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0532410A (en) | 1993-02-09 |
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