CN1276482C - Low-dielectric constant insulating media monox thin-film and preparing method thereof - Google Patents
Low-dielectric constant insulating media monox thin-film and preparing method thereof Download PDFInfo
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- CN1276482C CN1276482C CN200410044831.5A CN200410044831A CN1276482C CN 1276482 C CN1276482 C CN 1276482C CN 200410044831 A CN200410044831 A CN 200410044831A CN 1276482 C CN1276482 C CN 1276482C
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- dielectric constant
- silicon oxide
- low dielectric
- film
- oxide film
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- 238000000034 method Methods 0.000 title claims description 5
- 239000010409 thin film Substances 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 25
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011148 porous material Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 229910018557 Si O Inorganic materials 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 229910018540 Si C Inorganic materials 0.000 claims abstract description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000009413 insulation Methods 0.000 claims description 23
- -1 siloxanes Chemical class 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 6
- 125000004429 atom Chemical group 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000007639 printing Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract 2
- 239000010408 film Substances 0.000 description 54
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000007171 acid catalysis Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000003071 parasitic effect Effects 0.000 description 3
- 229920000151 polyglycol Polymers 0.000 description 3
- 239000010695 polyglycol Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- BJZYYSAMLOBSDY-QMMMGPOBSA-N (2s)-2-butoxybutan-1-ol Chemical compound CCCCO[C@@H](CC)CO BJZYYSAMLOBSDY-QMMMGPOBSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 208000035126 Facies Diseases 0.000 description 1
- 101000598921 Homo sapiens Orexin Proteins 0.000 description 1
- 101001123245 Homo sapiens Protoporphyrinogen oxidase Proteins 0.000 description 1
- 102100029028 Protoporphyrinogen oxidase Human genes 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- ZMAPKOCENOWQRE-UHFFFAOYSA-N diethoxy(diethyl)silane Chemical compound CCO[Si](CC)(CC)OCC ZMAPKOCENOWQRE-UHFFFAOYSA-N 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention discloses an insulating medium silicon oxide thin membrane with a low dielectric constant, which is made of materials having a general formula of SiO<x>Ry. The insulating medium silicon oxide thin membrane has chemical bonds of Si-O bonds, Si-C bonds and C-H bonds, has nanometer micropores. A preparation method of the present invention comprises: single end group sequin siloxane organics are used as a pore making mould plate which is used for preparing sol in an organic solution with siloxane; the sol is coated on a silicon chip to fabricate a thin membrane; the thin membrane is annealed under the protection of inert gas, which obtains the insulating medium silicon oxide thin membrane with a low dielectric constant, wherein annealing temperature is 200 to 600 DEG C, and a heating rate is 5 to 20 DEG C per minute. The present invention has the advantages of low dielectric constant, uniform nanometer micropore distribution, adjustable micropore dimension, rigidity of the thin membrane, controllable flexibility, stable electrical property of the thin membrane, good adhesiveness with silicon chips, tight combination and small residual stress.
Description
One, technical field
The present invention is a kind of low dielectric constant insulation medium silicon oxide film and preparation method thereof, and this film is used for the integrated circuit manufacturing.
Two, background technology
Along with developing rapidly of large scale integrated circuit, when the characteristic size of integrated circuit is decreased to 180nm or more hour, the parasitic resistance of interconnection, delay that electric capacity causes, crosstalk and energy consumption has become the bottleneck problem that development high speed, high density, low-power consumption and multifunctional integrated circuit need solve.In large scale integrated circuit, medium replaces silicon dioxide with the low dielectric constant insulation dielectric film between interlayer and line, can effectively reduce interconnection parasitic capacitance, thereby reduces delay that electric capacity causes, crosstalk and energy consumption.Therefore, a lot of scientific research personnel are exploring some low dielectric constant insulation dielectric films always.
At present, both at home and abroad the more low dielectric constant insulation dielectric film of research has fluorinated silicon oxide film (SiOF), polyimide film (PI), sesquialter silicon oxide film (SSQ) etc., but these products exist complex manufacturing, heat resistance poor, circuit had shortcomings such as burn into and silicon chip adhesion property difference.Existing many nano-pores silicon oxide film is single because of the pore template, can not participate in crosslinked, thereby cause membrane pore size to be difficult to control, the micropore skewness, mechanical strength is unadjustable, and when annealing thin film mechanical performance seriously descend.
Three, summary of the invention
The purpose of this invention is to provide a kind of low dielectric constant insulation medium silicon oxide film and preparation method thereof, this film can be used for large scale integrated circuit, have electrical properties good, with silicon chip adhesiveness good, nanometer micropore aperture scalable, micropore distribution homogeneous, mechanical property is adjustable.
Low dielectric constant insulation medium silicon oxide film of the present invention is characterized in that this film made by the material with following general formula:
SiO
xR
y
Wherein: 1≤x＜2,0＜y≤2,2x+y=4; R is methyl, ethyl or phenyl; Chemical bond in the film is Si-O key, Si-C key and c h bond; Film contains nanometer micropore.Film is thick to be 50-400nm; Si atom content (weight) 17-47% in the film, C atom content (weight) 0-33%, hydrogen atom content (weight) 0-9%, O atom content (weight) 21-55%; The aperture of nanometer micropore is 5-100nm in the film.
The preparation method of low dielectric constant insulation medium silicon oxide film of the present invention is characterized in that this method may further comprise the steps:
1, in organic solution, prepares colloidal sol with single-ended basic silsesquioxane organic substance as pore template and siloxanes;
2, above-mentioned colloidal sol is coated made film on the silicon chip;
3, above-mentioned film is annealed under inert gas shielding promptly get low dielectric constant insulation medium silicon oxide film, annealing temperature is 200-600 ℃, and heating rate is a 5-20 ℃ of per minute.
Wherein used pore template can be single-ended basic silsesquioxane polymer in (1), particularly single-ended basic silsesquioxane polyethers, as single-ended basic silsesquioxane polyglycol ether, single-ended basic silsesquioxane polypropylene glycol ether, single-ended basic silsesquioxane PTMG etc., and be that the polyethers of 500-4000 is best with the molecular weight, single-ended basic silsesquioxane polyethers can synthesize by certain method, as hydrosilylation etc.
Used organic solution is oxolane or methylformamide solution.
Used siloxanes is at least a in methyl silicate, tetraethoxysilane, alkylalkoxy silane, the alkoxy aryl silane, and adopts different ratios, can obtain the material of different mechanical properties.
Prepared collosol concentration is 0.1-1%.
The pore template of employing different molecular weight can obtain the nanometer micropore in different apertures, adopts different pore templates and siloxanes ratio, can obtain the material of the long-pending ratio in different holes.
Described coating process particularly rotate smearing method, and rotary speed is 1000-7000rpm for printing, spraying.
Because the dielectric constant of silica own is 2.8-4.0, suitably adds organic pore template, just can obtain dielectric constant and be lower than 2.0 ultralow dielectric dielectric film.Because the main film body structure is the Si-O key, and is so the film temperature tolerance is good, good with the silicon chip adhesion property.
The present invention compared with prior art, its remarkable advantage is: 1, dielectric constant is low, can be reduced to about 2.2.2, the nanometer micropore in the film is evenly distributed, pore template one end participates in cross-linking system, organic facies micron-scale phase separation when both having stoped gel to be smeared, the film internal crosslinking is subjected to Web Grafiti when effectively having avoided participating in annealing that cross-linking system causes because of pore template many places again.3, the micropore size dimension in the film is adjustable, by the molecular weight of control pore template, thereby can regulate and control organic segment from the size of twining balling-up, can obtain the nanometer micropore of required size after the annealing.4, the rigidity of film, flexible adjustable by the ratio of positive silicic acid alkane ester and alkylalkoxy silane in the adjusting multicomponent silicone, can be regulated the crosslink density of silica in the film, thereby can control the mechanical strength and the pliability of film.5, film electricity stable in properties, heat decomposition temperature do not absorb moisture substantially more than 500 ℃ in air.6, the adhesiveness with silicon chip is good, and in conjunction with tight, residual stress is little.
Along with the development of very lagre scale integrated circuit (VLSIC), the size of microelectronic circuit is dwindled day by day, and the increase of interconnect delay and parasitic capacitance, the present invention are specially adapted to very lagre scale integrated circuit (VLSIC), CPU substitutes traditional Si O in producing
2And other existing low dielectric films, can reduce heating and delay very effectively.
Four, embodiment
The invention will be further described below by embodiment.
Embodiment 1: the low dielectric constant insulation medium silicon oxide film that the present invention is prepared, make by material with following general formula:
SiO
xR
y
Wherein: x=1.1, y=1.8; R is a methyl; Chemical bond in the film is Si-O key, Si-C key and c h bond; Contain nanometer micropore in the film, the aperture is 50 nanometers, and the volume ratio of micropore and film is 20%; The thickness of film is 200 nanometers; Si atom content (weight) 37% in the film, C atom content (weight) 33%, hydrogen atom content (weight) 7%, O atom content (weight) 23%.
The preparation method of above-mentioned film is:
1,, obtains molecular weight and is 1000 single-ended basic silsesquioxane polyglycol ether, as the pore template with allyl polyglycol ether (molecular weight 900) and the silicon hydrogen addition under chloroplatinic acid-catalysis of trimethoxy silicon hydrogen.
2, be raw material with above-mentioned pore template and dimethyldimethoxysil,ne, methyl silicate; wherein the ratio of dimethyldimethoxysil,ne and methyl silicate is 9: 1; in oxolane, use hydrolysis under the diluted acid catalysis; make 0.2% concentration colloidal sol; spin-coating under room temperature and 5000rpm rotating speed; 450 ℃ of temperature and condition of nitrogen gas protection annealing down, heating rate is 5 ℃ of per minutes.
Embodiment 2: the low dielectric constant insulation medium silicon oxide film that the present invention is prepared, make by material with following general formula:
SiO
xR
y
Wherein: x=1.5, y=1; R is an ethyl; Chemical bond in the film is Si-O key, Si-C key and c h bond; Contain nanometer micropore in the film, the aperture is 20 nanometers, and the volume ratio of micropore and film is 50%; The thickness of film is 300 nanometers; Si atom content (weight) 35% in the film, C atom content (weight) 30%, hydrogen atom content (weight) 5%, O atom content (weight) 30%.
The preparation method of above-mentioned film is: with molecular weight is that 650 single-ended basic silsesquioxane PPOX ether, diethyl diethoxy base silane, tetraethoxysilane are raw material.Wherein the ratio of diethyl diethoxy silane and tetraethoxysilane is 1: 1, hydrolysis under the weak base catalysis in dimethyl formamide makes O.1% concentration colloidal sol, spin-coating under the 4000rpm rotating speed, anneal 10 ℃ of per minutes of heating rate under 500 ℃ of argon gas conditions.
Embodiment 3:
The low dielectric constant insulation medium silicon oxide film that the present invention is prepared, make by material with following general formula:
SiO
xR
y
Wherein: x=1.9, y=0.2; R is a phenyl; Chemical bond in the film is Si-O key, Si-C key and c h bond; Contain nanometer micropore in the film, the aperture is 80 nanometers, and the volume ratio of micropore and film is 80%; The thickness of film is 400 nanometers; Si atom content (weight) 38% in the film, C atom content (weight) 20%, hydrogen atom content (weight) 1%, O atom content (weight) 41%.
The preparation method of above-mentioned film is: with molecular weight is that 650 single-ended basic silsesquioxane PTMG, diphenyl dimethoxy triacetoxy, methyl silicate are raw material.Wherein the ratio of dimethoxydiphenylsilane and methyl silicate is 1: 9, and hydrolysis under the acid catalysis in dimethyl formamide makes 0.5% concentration colloidal sol, and spin-coating under the 2000rpm rotating speed is annealed under 600 ℃ of argon gas conditions, 20 ℃ of per minutes of heating rate.
Claims (10)
1, a kind of low dielectric constant insulation medium silicon oxide film is characterized in that this film made by the material with following general formula:
SiO
xR
y
Wherein: 1≤x＜2,0＜y≤2,2x+y=4; R is methyl, ethyl or phenyl; Chemical bond in the film is Si-O key, Si-C key and c h bond; Film contains nanometer micropore.
2, low dielectric constant insulation medium silicon oxide film according to claim 1 is characterized in that the thick 50-400nm of being of film.
3, low dielectric constant insulation medium silicon oxide film according to claim 1 is characterized in that the Si atom content is weight 17-47% in the film, and the C atom content is weight 0-33%, and the H atom content is weight 0-9%, and the O atom content is weight 21-55%.
4, low dielectric constant insulation medium silicon oxide film according to claim 1, the aperture that it is characterized in that nanometer micropore in the film is 5-100nm.
5, a kind of preparation method of low dielectric constant insulation medium silicon oxide film is characterized in that this method may further comprise the steps:
(1) in organic solution, prepares colloidal sol with single-ended basic silsesquioxane organic substance as pore template and siloxanes;
(2) above-mentioned colloidal sol is coated made film on the silicon chip;
(3) above-mentioned film is annealed under inert gas shielding promptly get low dielectric constant insulation medium silicon oxide film, annealing temperature is 200-600 ℃, and heating rate is a 5-20 ℃ of per minute.
6, the preparation method of low dielectric constant insulation medium silicon oxide film according to claim 5 is characterized in that used pore template is single-ended basic silsesquioxane polymer in (1).
7, the preparation method of low dielectric constant insulation medium silicon oxide film according to claim 6 is characterized in that the pore template is single-ended basic silsesquioxane polyethers, and molecular weight is 500-4000.
8, the preparation method of low dielectric constant insulation medium silicon oxide film according to claim 5 is characterized in that the organic solution in (1) is oxolane or methylformamide.
9, the preparation method of low dielectric constant insulation medium silicon oxide film according to claim 5 is characterized in that coating process is smeared for printing, spraying or rotation in (2).
10, the preparation method of low dielectric constant insulation medium silicon oxide film according to claim 5 is characterized in that used siloxanes in (1) is at least a in methyl silicate, tetraethoxysilane, alkylalkoxy silane, the alkoxy aryl silane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410044831.5A CN1276482C (en) | 2004-06-02 | 2004-06-02 | Low-dielectric constant insulating media monox thin-film and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410044831.5A CN1276482C (en) | 2004-06-02 | 2004-06-02 | Low-dielectric constant insulating media monox thin-film and preparing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1585101A CN1585101A (en) | 2005-02-23 |
| CN1276482C true CN1276482C (en) | 2006-09-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408251B (en) * | 2011-07-25 | 2013-03-27 | 重庆文理学院 | Preparation method of mesoporous silica thin film material with low dielectric constant |
| CN103121856B (en) * | 2011-07-25 | 2014-08-13 | 重庆文理学院 | Preparation method of mesoporous silicon oxide thin film material |
| CN115746380A (en) * | 2022-11-24 | 2023-03-07 | 慧迈材料科技(广东)有限公司 | Preparation method of polyimide porous composite film |
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