JP4538259B2 - 層間絶縁膜の表面改質方法及び表面改質装置 - Google Patents
層間絶縁膜の表面改質方法及び表面改質装置 Download PDFInfo
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- 239000011229 interlayer Substances 0.000 title claims description 211
- 230000004048 modification Effects 0.000 title claims description 68
- 238000012986 modification Methods 0.000 title claims description 68
- 238000002715 modification method Methods 0.000 title claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 75
- 239000007789 gas Substances 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 54
- 230000001590 oxidative effect Effects 0.000 claims description 46
- 239000001301 oxygen Substances 0.000 claims description 41
- 229910052760 oxygen Inorganic materials 0.000 claims description 41
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000001257 hydrogen Substances 0.000 claims description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims description 34
- 239000011248 coating agent Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 32
- 238000009413 insulation Methods 0.000 claims description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 18
- -1 polysiloxane Polymers 0.000 claims description 12
- 125000000524 functional group Chemical group 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 10
- 230000010718 Oxidation Activity Effects 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 23
- 239000004065 semiconductor Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 9
- 230000001678 irradiating effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000004528 spin coating Methods 0.000 description 5
- 239000012212 insulator Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
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- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
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- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02214—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen
- H01L21/02216—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane
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Description
また、本発明は、誘電率を維持しつつ、密着性を向上することができる層間絶縁膜の表面改質方法及び表面改質装置を提供することを目的とする。
塗布液を塗布して塗布膜が形成された基板を所定の温度で焼成することにより形成された層間絶縁膜の表面を改質する層間絶縁膜の表面改質方法であって、
前記層間絶縁膜が形成された基板を収容する反応室内を250℃〜400℃に加熱するとともに、前記反応室内に水素及び酸素を別々に供給し、その混合ガスにより生成された活性種によって前記層間絶縁膜の表面エネルギーが大きくなることにより、前記層間絶縁膜の表面を改質する表面改質工程を備える、ことを特徴とする。
塗布液を塗布して塗布膜が形成された基板を所定の温度で焼成することにより形成された層間絶縁膜の表面を改質する層間絶縁膜の表面改質装置であって、
前記層間絶縁膜が形成された基板を収容する反応室内を所定の温度に加熱する加熱手段と、
前記反応室内に酸化活性ガスを供給する酸化活性ガス供給手段と、
前記反応室内を所定の温度に加熱するように前記加熱手段を制御するとともに、前記反応室内に酸化活性ガスを供給するように前記酸化活性ガス供給手段を制御する制御手段と、
を備え、
前記酸化活性ガスは、水素及び酸素であり、
前記制御手段は、前記反応室内を250℃〜400℃に加熱するように前記加熱手段を制御するとともに、前記反応室内に前記水素及び酸素を別々に供給するように前記酸化活性ガス供給手段を制御し、前記反応室内に供給された前記水素及び酸素の混合ガスにより生成された活性種によって前記層間絶縁膜の表面エネルギーが大きくなることにより、前記層間絶縁膜の表面を改質する、ことを特徴とする。
本例では、酸化活性ガス導入管13からのオゾン供給時間を1分、反応管2内の圧力を133Pa(1Torr)、オゾン量を25g/Nm3として、反応管2内の温度を200℃(比較例2)、250℃(参考例1)、及び、300℃(参考例2)に設定し、オゾンによる層間絶縁膜の表面改質を行った場合の層間絶縁膜の純水による接触角を測定した。図3(a)にオゾンによる層間絶縁膜の表面改質の条件を示し、図3(b)に表面改質した層間絶縁膜の純水による接触角を示す。また、表面改質した層間絶縁膜上にハードマスクを成膜してCMPテストを行った。この結果(膜剥がれが発生せず密着性を有する場合を「○」、膜剥がれが発生し密着性を有しない場合を「×」)を図3(a)に示す。さらに、表面改質しない場合(比較例1)についても層間絶縁膜の純水による接触角及びCMPテストを行い、この結果を図3中に示す。
本例では、反応管2内の圧力を常圧として、反応管2内の温度を500℃、酸化活性ガス導入管13からの水蒸気供給時間を30分に設定した場合(参考例3)と、反応管2内の温度を400℃、酸化活性ガス導入管13からの水蒸気供給時間を15分に設定した場合(比較例3)とについて、水蒸気による層間絶縁膜の表面改質を行い、層間絶縁膜の純水による接触角を測定した。図4(a)に水蒸気による層間絶縁膜の表面改質の条件を示し、図4(b)に表面改質した層間絶縁膜の純水による接触角を示す。
本例では、反応管2内の圧力を133Pa(1Torr)として、反応管2内の温度、酸化活性ガス導入管13からの水素及び酸素の供給時間、水素の割合(水素混合比)を変化させた場合(実施例4〜実施例10)について、水素及び酸素による層間絶縁膜の表面改質を行い、層間絶縁膜の純水による接触角を測定した。なお、本例では、別々の酸化活性ガス導入管13から酸素と水素とを供給し、反応管2内で混合した。図5(a)に水素及び酸素による層間絶縁膜の表面改質の条件を示し、図5(b)に表面改質した層間絶縁膜の純水による接触角を示す。
本例では、反応管2内の圧力を常圧、酸化活性ガス導入管13からの酸素供給時間を30分として、反応管2内の温度を300℃(比較例4)、400℃(比較例5)、500℃(参考例11)、及び、600℃(参考例12)に設定し、酸素による層間絶縁膜の表面改質を行った場合の層間絶縁膜の純水による接触角を測定した。図6(a)に酸素による層間絶縁膜の表面改質の条件を示し、図6(b)に表面改質した層間絶縁膜の純水による接触角を示す。
本例では、層間絶縁膜への紫外線照射時間を大気雰囲気中、室温(約25℃)下で10秒(参考例13)、及び、30秒(参考例14)に設定し、紫外線による層間絶縁膜の表面改質を行った場合の層間絶縁膜の純水による接触角を測定した。図7(a)に紫外線による層間絶縁膜の表面改質の条件を示し、図7(b)に表面改質した層間絶縁膜の純水による接触角を示す。
2 反応管
3 内管
4 外管
5 マニホールド
6 支持リング
7 蓋体
8 ボートエレベータ
9 ウエハボート
10 半導体ウエハ
11 断熱体
12 昇温用ヒータ
13 酸化活性ガス導入管
14 排気口
15 パージガス供給管
16 排気管
17 バルブ
18 真空ポンプ
19 制御部
Claims (8)
- 塗布液を塗布して塗布膜が形成された基板を所定の温度で焼成することにより形成された層間絶縁膜の表面を改質する層間絶縁膜の表面改質方法であって、
前記層間絶縁膜が形成された基板を収容する反応室内を250℃〜400℃に加熱するとともに、前記反応室内に水素及び酸素を別々に供給し、その混合ガスにより生成された活性種によって前記層間絶縁膜の表面エネルギーが大きくなることにより、前記層間絶縁膜の表面を改質する表面改質工程を備える、ことを特徴とする層間絶縁膜の表面改質方法。 - 前記層間絶縁膜は、有機官能基を有するポリシロキサンを含む塗布液から形成された低誘電率の層間絶縁膜である、ことを特徴とする請求項1に記載の層間絶縁膜の表面改質方法。
- 前記表面改質工程では、前記層間絶縁膜を、その表面エネルギーが少なくとも80mN/mとなるように改質する、ことを特徴とする請求項1または2に記載の層間絶縁膜の表面改質方法。
- 前記表面改質工程では、前記層間絶縁膜を、その表面における水の表面接触角が40°よりも小さくなるように改質する、ことを特徴とする請求項1乃至3のいずれか1項に記載の層間絶縁膜の表面改質方法。
- 塗布液を塗布して塗布膜が形成された基板を所定の温度で焼成することにより形成された層間絶縁膜の表面を改質する層間絶縁膜の表面改質装置であって、
前記層間絶縁膜が形成された基板を収容する反応室内を所定の温度に加熱する加熱手段と、
前記反応室内に酸化活性ガスを供給する酸化活性ガス供給手段と、
前記反応室内を所定の温度に加熱するように前記加熱手段を制御するとともに、前記反応室内に酸化活性ガスを供給するように前記酸化活性ガス供給手段を制御する制御手段と、
を備え、
前記酸化活性ガスは、水素及び酸素であり、
前記制御手段は、前記反応室内を250℃〜400℃に加熱するように前記加熱手段を制御するとともに、前記反応室内に前記水素及び酸素を別々に供給するように前記酸化活性ガス供給手段を制御し、前記反応室内に供給された前記水素及び酸素の混合ガスにより生成された活性種によって前記層間絶縁膜の表面エネルギーが大きくなることにより、前記層間絶縁膜の表面を改質する、ことを特徴とする層間絶縁膜の表面改質装置。 - 前記層間絶縁膜は、有機官能基を有するポリシロキサンを含む塗布液から形成された低誘電率の層間絶縁膜である、ことを特徴とする請求項5に記載の層間絶縁膜の表面改質装置。
- 前記制御手段は、前記層間絶縁膜を、その表面エネルギーが少なくとも80mN/mとなるように改質する、ことを特徴とする請求項5または6に記載の層間絶縁膜の表面改質装置。
- 前記制御手段は、前記層間絶縁膜を、その表面における水の表面接触角が40°よりも小さくなるように改質する、ことを特徴とする請求項5乃至7のいずれか1項に記載の層間絶縁膜の表面改質装置。
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