WO2011049091A1 - 金属微細構造体のパターン倒壊抑制用処理液及びこれを用いた金属微細構造体の製造方法 - Google Patents
金属微細構造体のパターン倒壊抑制用処理液及びこれを用いた金属微細構造体の製造方法 Download PDFInfo
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- fluoroalkyl group
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 70
- 239000002184 metal Substances 0.000 title claims abstract description 70
- 238000011282 treatment Methods 0.000 title claims abstract description 66
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 title abstract description 25
- 125000003709 fluoroalkyl group Chemical group 0.000 claims abstract description 35
- -1 ammonium halide Chemical class 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- 229960003237 betaine Drugs 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 19
- 229910052721 tungsten Inorganic materials 0.000 claims description 19
- 239000010937 tungsten Substances 0.000 claims description 19
- 239000004065 semiconductor Substances 0.000 claims description 14
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 10
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 10
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000001312 dry etching Methods 0.000 claims description 6
- 238000001039 wet etching Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 230000000052 comparative effect Effects 0.000 description 20
- 230000005764 inhibitory process Effects 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 229910052814 silicon oxide Inorganic materials 0.000 description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 230000001629 suppression Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229920002120 photoresistant polymer Polymers 0.000 description 5
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 3
- 238000000206 photolithography Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical class C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910004298 SiO 2 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
- 239000000654 additive Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
- H01L21/0271—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers
- H01L21/0273—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers characterised by the treatment of photoresist layers
- H01L21/0274—Photolithographic processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00841—Cleaning during or after manufacture
- B81C1/00849—Cleaning during or after manufacture during manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2203/00—Basic microelectromechanical structures
- B81B2203/03—Static structures
- B81B2203/0361—Tips, pillars
Definitions
- the present invention relates to a processing solution for suppressing pattern collapse of a metal microstructure and a method for producing a metal microstructure using the same.
- a photolithography technique is used as a method for forming and processing an element having a fine structure used in a wide field such as a semiconductor device or a circuit board.
- a wide field such as a semiconductor device or a circuit board.
- miniaturization, high integration, and high speed of semiconductor devices and the like have advanced remarkably, and the resist pattern used for photolithography has become finer and the aspect ratio has been increasing. I'm following.
- the miniaturization or the like progresses, the collapse of the resist pattern becomes a big problem.
- the collapse of the resist pattern is caused by the surface tension of the processing solution when the processing solution used in the wet processing (mainly rinsing processing for washing away the developing solution) after developing the resist pattern is dried from the resist pattern. It is known that it is generated by the action of stress. Therefore, in order to solve the collapse of the resist pattern, a method of drying by replacing the cleaning liquid with a low surface tension liquid using a nonionic surfactant, an alcohol solvent-soluble compound or the like (for example, Patent Documents 1 and 2). And a method of hydrophobizing the surface of the resist pattern (for example, see Patent Document 3).
- a fine structure made of metal, metal nitride, metal oxide or the like formed by photolithography technology hereinafter referred to as a metal fine structure.
- a metal, metal nitride, or metal oxide is simply included.
- the strength of the metal itself forming the structure is higher than the strength of the resist pattern itself or the bonding strength between the resist pattern and the substrate. Collapse is unlikely to occur.
- semiconductor devices and micromachines are further reduced in size, increased in integration, and speeded up, the pattern of the structure becomes finer, and the collapse of the pattern of the structure due to an increase in aspect ratio becomes a serious problem.
- the resist pattern which is an organic material
- the surface state of the metal microstructure are completely different, unlike the case of the collapse of the resist pattern described above, no effective countermeasures can be found, so semiconductor devices and micromachines are downsized and highly integrated.
- the degree of freedom in pattern design is significantly hindered, such as designing a pattern that does not cause pattern collapse.
- the present invention has been made under such circumstances, and provides a treatment liquid capable of suppressing pattern collapse of a metal microstructure such as a semiconductor device or a micromachine, and a method of manufacturing a metal microstructure using the same. It is the purpose.
- the present inventors have found that at least one of an ammonium halide having a fluoroalkyl group, a betaine compound having a fluoroalkyl group, and an amine oxide compound having a fluoroalkyl group. It has been found that the object can be achieved by a treatment liquid containing The present invention has been completed based on such findings. That is, the gist of the present invention is as follows.
- Pattern collapse suppression treatment for a metal microstructure including at least one selected from the group consisting of an ammonium halide having a fluoroalkyl group, a betaine compound having a fluoroalkyl group, and an amine oxide compound having a fluoroalkyl group liquid.
- the treatment liquid according to [1] wherein the content of the ammonium halide having the fluoroalkyl group, the betaine compound having the fluoroalkyl group, and the amine oxide compound having the fluoroalkyl group is 10 ppm to 50%.
- the metal microstructure according to [5] wherein the metal microstructure is formed using at least one material selected from the group consisting of titanium nitride, tungsten, hafnium oxide, tantalum, and titanium. Production method.
- a treatment liquid capable of suppressing pattern collapse of a metal microstructure such as a semiconductor device or a micromachine, and a method of manufacturing a metal microstructure using the same.
- FIG. 6 is a schematic cross-sectional view for each production stage of metal microstructures produced in Examples 1 to 45 and Comparative Examples 1 to 65.
- the treatment liquid of the present invention is used for suppressing pattern collapse of a metal microstructure, and is at least one selected from an ammonium halide having a fluoroalkyl group, a betaine compound having a fluoroalkyl group, and an amine oxide compound having a fluoroalkyl group. Is included.
- ammonium halide having a fluoroalkyl group, the betaine compound having a fluoroalkyl group, and the amine oxide compound having a fluoroalkyl group used in the treatment liquid of the present invention are adsorbed with the metal material used for the pattern of the metal microstructure, It is considered that the surface of the pattern is hydrophobized. Hydrophobization in this case indicates that the contact angle between the surface of the metal treated with the treatment liquid of the present invention and water is 70 ° or more.
- the fluoroalkyl group shown in the present invention is a perfluoroalkyl group
- the perfluoroalkyl group means a group in which all hydrogen atoms of the alkyl group are substituted with fluorine atoms.
- the fluoroalkyl group preferably has 1 to 6 carbon atoms.
- ammonium halide having a fluoroalkyl group examples include the product name Fluorard FC-135 (manufactured by Sumitomo 3M Co., Ltd.), the product name Aftergent 300 (Neos Corporation), the product name Footgent 310 (Neos Corporation), and the product name Surflon S. -121 (manufactured by AGC Seimi Chemical Co., Ltd.), product name Surflon S-221 (manufactured by AGC Seimi Chemical Co., Ltd.) and the like, and product name Surflon S-221 (manufactured by AGC Seimi Chemical Co., Ltd.) is particularly preferable.
- the product name Footgent 400S (Neos Co., Ltd.), the product name Surflon S-131 (AGC Seimi Chemical Co., Ltd.), the product name Surflon S-132 (AGC Seimi Chemical Co., Ltd.) Product name Surflon S-231 (AGC Seimi Chemical Co., Ltd.) and the like, and Surflon S-231 (AGC Seimi Chemical Co., Ltd.) is particularly preferable.
- the amine oxide compound having a fluoroalkyl group include the product name Surflon S-141 (AGC Seimi Chemical Co., Ltd.) and the product name Surflon S-241 (AGC Seimi Chemical Co., Ltd.).
- the product name Surflon S- 241 (AGC Seimi Chemical Co., Ltd.) is preferable.
- the treatment liquid of the present invention preferably further contains water and is preferably an aqueous solution.
- the water is preferably water from which metal ions, organic impurities, particle particles, and the like have been removed by distillation, ion exchange treatment, filter treatment, various adsorption treatments, and the like, and pure water and ultrapure water are particularly preferred.
- the treatment liquid of the present invention contains at least one of the above-described ammonium halide having a fluoroalkyl group, a betaine compound having a fluoroalkyl group, and an amine oxide compound having a fluoroalkyl group, preferably containing water, It contains various additives usually used in the treatment liquid as long as the effect of the treatment liquid is not impaired.
- the content of the ammonium halide having a fluoroalkyl group, the betaine compound having a fluoroalkyl group, and the amine oxide compound having a fluoroalkyl group in the treatment liquid of the present invention is 10 ppm to 50 % Is preferred. It is preferably 30% or less, more preferably 10% or less, more preferably 5% or less, more preferably 10 to 2000 ppm, particularly preferably 10 to 2000 ppm in consideration of ease of handling, economy and foaming. 1000 ppm.
- an organic solvent such as alcohol may be added, or the solubility may be supplemented by adding an acid or an alkali.
- an organic solvent such as alcohol
- the treatment liquid of the present invention is suitably used for suppressing pattern collapse of a metal microstructure such as a semiconductor device or a micromachine.
- a metal microstructure such as a semiconductor device or a micromachine.
- the pattern of the metal microstructure at least one material selected from TiN (titanium nitride), W (tungsten), HfO 2 (hafnium oxide), Ta (tantalum), and Ti (titanium) is used. Those are preferred.
- the metal microstructure is patterned on an insulating film type such as SiO 2 (silicon oxide film) or TEOS (tetraethoxyorthosilane oxide film), or the insulating film type is formed on a part of the metal microstructure. May be included.
- the treatment liquid of the present invention can exhibit an excellent effect of suppressing pattern collapse on not only a conventional metal microstructure but also a metal microstructure having a finer and higher aspect ratio.
- the aspect ratio is a value calculated by (pattern height / pattern width)
- the treatment liquid of the present invention is an excellent pattern for patterns having a high aspect ratio of 3 or more, and further 7 or more. Has the effect of suppressing collapse.
- the treatment liquid of the present invention has a fine pattern of 1: 1 line and space, even if the pattern size (pattern width) is 300 nm or less, 150 nm or less, 100 nm or less, and even 50 nm or less.
- the fine pattern having a cylindrical or columnar structure having an interval between patterns of 300 nm or less, 150 nm or less, 100 nm or less, or 50 nm or less has an excellent effect of suppressing pattern collapse.
- the metal microstructure manufacturing method of the present invention is characterized by using the above-described treatment liquid of the present invention in a cleaning step after wet etching or dry etching. More specifically, in the cleaning step, preferably, after the metal microstructure pattern and the treatment liquid of the present invention are brought into contact with each other by dipping, spray discharge, spraying, etc., the treatment liquid is replaced with water. dry.
- the immersion time is preferably 10 seconds to 30 minutes, more preferably 15 seconds to 20 minutes, and still more preferably 20 seconds to 15 minutes.
- the temperature condition is preferably 10 to 60 ° C., more preferably 15 to 50 ° C., still more preferably 20 to 40 ° C., and particularly preferably 25 to 40 ° C.
- the surface of the pattern is hydrophobized so that the pattern collapses so that the pattern contacts the adjacent pattern. It becomes possible to suppress.
- the treatment liquid of the present invention includes a wet etching process or a dry etching process in the manufacturing process of the metal microstructure, followed by a wet process (etching or cleaning, rinsing for washing away the cleaning liquid), and then drying. If it has the process to do, it can apply widely irrespective of the kind of metal microstructure. For example, (i) in the manufacture of a DRAM type semiconductor device, after wet etching is performed on an insulating film around a conductive film (see, for example, Japanese Patent Laid-Open Nos.
- a strip After a cleaning step for removing contaminants generated after dry etching or wet etching at the time of processing a gate electrode in the manufacture of a semiconductor device having a transistor having a fin-like shape for example, Japanese Patent Application Laid-Open No.
- treatment liquids 1 to 9 for suppressing pattern collapse of metal microstructures were prepared.
- the balance is water.
- Examples 1 to 9 As shown in FIG. 1A, after silicon nitride 103 (thickness: 100 nm) and silicon oxide 102 (thickness: 1200 nm) are formed on a silicon substrate 104, a photoresist 101 is formed, and then the photo resist is formed. By exposing and developing the resist 101, a circle-ring opening 105 ( ⁇ 125 nm, distance between the circle and the circle: 50 nm) shown in FIG. 1B is formed, and dry etching is performed using the photoresist 101 as a mask. A cylindrical hole 106 shown in FIG. 1C was formed in the silicon oxide 102 by etching up to the silicon nitride 103 layer.
- the photoresist 101 was removed by ashing to obtain a structure in which a cylindrical hole 106 reaching the silicon nitride 103 layer in the silicon oxide 102 shown in FIG. Tungsten is filled and deposited as the metal 107 in the cylindrical hole 106 of the obtained structure (FIG. 1- (e)), and an excess on the silicon oxide 102 is obtained by chemical mechanical polishing (CMP).
- CMP chemical mechanical polishing
- the metal (tungsten) 107 was removed to obtain a structure in which a metal (tungsten) cylinder 108 was embedded in the silicon oxide 102 shown in FIG.
- the silicon oxide 102 of the obtained structure was dissolved and removed with a 0.5% hydrofluoric acid aqueous solution (25 ° C., 1 minute immersion treatment), then rinsed with pure water, treatment liquid 1-18 (30 ° C., 10 minute immersion treatment) , And pure water rinse in that order, followed by drying to obtain a structure shown in FIG.
- the obtained structure is a microstructure having a metal (tungsten) cylinder-chimney pattern ( ⁇ 125 nm, height: 1200 nm (aspect ratio: 9.6), distance between cylinder: 50 nm). Yes, more than 70% of the pattern did not collapse.
- pattern collapse was observed using “FE-SEM S-5500 (model number)” manufactured by Hitachi High-Technologies Corporation, and the collapse suppression rate was calculated as the ratio of the pattern that did not collapse in the total number of patterns. It was determined to be acceptable if the collapse inhibition rate was 50% or more.
- Table 3 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Example 1 the silicon oxide 102 of the structure shown in FIG. 1 (f) was dissolved and removed with hydrofluoric acid, and then treated with pure water only. The structure shown was obtained. 50% or more of the pattern of the obtained structure caused the collapse as shown in FIG. 1 (h) (the collapse suppression rate is less than 50%).
- Table 3 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in Comparative Example 1.
- Example 2 the silicon oxide 102 having the structure shown in FIG. 1 (f) was dissolved and removed with hydrofluoric acid and treated with pure water. Then, instead of the treatment liquid 1, the comparison liquids 1 to 13 shown in Table 2 were used. Except for the treatment, the structure shown in FIG. 1G was obtained in the same manner as in Example 1. More than 50% of the pattern of the obtained structure collapsed as shown in FIG. Table 3 shows the results of the treatment liquid, treatment method, and collapse suppression rate used in Examples 2 to 14.
- Examples 10-18 the structure shown in FIG. 1G was obtained in the same manner as in Examples 1 to 9 except that titanium nitride was used instead of tungsten as the metal 107.
- the obtained structure has a fine pattern ( ⁇ 125 nm, height: 1200 nm (aspect ratio: 9.6), distance between the cylinders: 50 nm) of the cylinder 108 of metal (titanium nitride). It was a structure, and 70% or more of the pattern did not collapse.
- Table 4 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Comparative Examples 15 to 27 In Comparative Examples 1 to 14, the structure shown in FIG. 1G of Comparative Examples 15 to 27 was obtained in the same manner as Comparative Examples 1 to 14, except that titanium nitride was used as the metal 107 instead of tungsten. . More than 50% of the pattern of the obtained structure collapsed as shown in FIG. Table 4 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Examples 19-27 the structure shown in FIG. 1G was obtained in the same manner as in Examples 1 to 9 except that hafnium oxide was used instead of tungsten as the metal 107.
- the obtained structure has a fine pattern ( ⁇ 125 nm, height: 1200 nm (aspect ratio: 9.6), distance between the cylinders: 50 nm) of the cylinder 108 of metal (hafnium oxide). It was a structure, and 70% or more of the pattern did not collapse.
- Table 5 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Comparative Examples 28-40 In Comparative Examples 1 to 14, the structures shown in FIG. 1G of Comparative Examples 28 to 40 were obtained in the same manner as Comparative Examples 1 to 14 except that hafnium oxide was used instead of tungsten as the metal 107. . More than 50% of the pattern of the obtained structure collapsed as shown in FIG. Table 5 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Examples 28-36 In Examples 1 to 9, the structure shown in FIG. 1G was obtained in the same manner as in Examples 1 to 9, except that tantalum was used as the metal 107 instead of tungsten.
- the resulting structure is a microstructure having a cylindrical pattern of metal (tantalum) cylinder 108 ( ⁇ 125 nm, height: 1200 nm (aspect ratio: 9.6), distance between cylinder: 50 nm). And 70% or more of the pattern did not collapse.
- Table 6 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Comparative Examples 41-53 In Comparative Examples 1 to 14, the structure shown in FIG. 1G of Comparative Examples 41 to 53 was obtained in the same manner as Comparative Examples 1 to 14 except that tantalum was used as the metal 107 instead of tungsten. More than 50% of the pattern of the obtained structure collapsed as shown in FIG. Table 6 shows the results of the treatment liquid, the treatment method, and the collapse inhibition rate used in each example.
- Examples 37-45 the structure shown in FIG. 1G was obtained in the same manner as in Examples 1 to 9 except that titanium was used instead of tungsten as the metal 107.
- the resulting structure is a microstructure having a cylindrical pattern of metal (titanium) cylinder 108 ( ⁇ 125 nm, height: 1200 nm (aspect ratio: 9.6), distance between cylinder: 50 nm). And 70% or more of the pattern did not collapse.
- Table 7 shows the results of the treatment liquid, treatment method, and collapse suppression rate used in each example.
- Comparative Examples 53-65 In Comparative Examples 1 to 14, the structure shown in FIG. 1G of Comparative Examples 53 to 65 was obtained in the same manner as Comparative Examples 1 to 14, except that titanium was used as the metal 107 instead of tungsten. More than 50% of the pattern of the obtained structure collapsed as shown in FIG. Table 7 shows the results of the treatment liquid, treatment method, and collapse suppression rate used in each example.
- the treatment liquid of the present invention can be suitably used for suppressing pattern collapse in the production of metal microstructures such as semiconductor devices and micromachines (MEMS).
- MEMS micromachines
- Photoresist 102 Silicon oxide 103. Silicon nitride 104. Silicon substrate 105. Circular opening 106. Cylindrical hole 107. Metal (titanium nitride, tungsten, hafnium oxide, tantalum or titanium) 108. Metal cylinder (titanium nitride, tungsten, hafnium oxide, tantalum or titanium)
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Abstract
Description
本発明は、このような状況下になされたもので、半導体装置やマイクロマシンといった金属微細構造体のパターン倒壊を抑制しうる処理液及びこれを用いた金属微細構造体の製造方法を提供することを目的とするものである。
本発明は、かかる知見に基づいて完成したものである。すなわち、本発明の要旨は下記のとおりである。
[2] 前記フルオロアルキル基を有するアンモニウムハライド、前記フルオロアルキル基を有するベタイン化合物、および前記フルオロアルキル基を有するアミンオキシド化合物の含有量が10ppm~50%である[1]に記載の処理液。
[3] さらに水を含む[1]または[2]に記載の処理液。
[4] 前記金属微細構造体のパターンが、窒化チタン、タングステン、酸化ハフニウム、タンタルおよびチタンからなる群から選択される少なくとも一種の材料を用いてなるものである[1]~[3]のいずれかに記載の処理液。
[5] ウェットエッチングまたはドライエッチングの後の洗浄工程において、[1]~[4]のいずれかに記載の処理液を用いることを特徴とする金属微細構造体の製造方法。
[6] 前記金属微細構造体が、窒化チタン、タングステン、酸化ハフニウム、タンタルおよびチタンからなる群から選択される少なくとも一種の材料を用いてなるものである[5]に記載の金属微細構造体の製造方法。
[7] 前記金属微細構造体が、半導体装置またはマイクロマシンである[5]または[6]に記載の金属微細構造体の製造方法。
また、フルオロアルキル基を有するベタイン化合物としては、製品名フタージェント400S(株式会社ネオス)、製品名サーフロンS-131(AGCセイミケミカル株式会社)、製品名サーフロンS-132(AGCセイミケミカル株式会社)、製品名サーフロンS-231(AGCセイミケミカル株式会社)などが挙げられ、特にサーフロンS-231(AGCセイミケミカル株式会社)が好ましい。
さらに、フルオロアルキル基を有するアミンオキシド化合物としては、製品名サーフロンS-141(AGCセイミケミカル株式会社)、製品名サーフロンS-241(AGCセイミケミカル株式会社)が挙げられ、特に製品名サーフロンS-241(AGCセイミケミカル株式会社)が好ましい。
なお、金属微細構造体は、SiO2(シリコン酸化膜)やTEOS(テトラエトキシオルソシラン酸化膜)などの絶縁膜種の上にパターニングされる場合や、金属微細構造の一部に絶縁膜種が含まれる場合がある。
本発明の金属微細構造体の製造方法は、ウェットエッチング又はドライエッチングの後の洗浄工程において、上記した本発明の処理液を用いることを特徴とするものである。より具体的には、該洗浄工程において、好ましくは金属微細構造体のパターンと本発明の処理液とを浸漬、スプレー吐出、噴霧などにより接触させた後、水で該処理液を置換してから乾燥させる。ここで、金属微細構造体のパターンと本発明の処理液とを浸漬により接触させる場合、浸漬時間は10秒~30分が好ましく、より好ましくは15秒~20分、さらに好ましくは20秒~15分、特に好ましくは30秒~10分であり、温度条件は10~60℃が好ましく、より好ましくは15~50℃、さらに好ましくは20~40℃、特に好ましくは25~40℃である。また、金属微細構造体のパターンと本発明の処理液との接触の前に、あらかじめ水で洗浄を行ってもよい。このように、金属微細構造体のパターンと本発明の処理液とを接触させることにより、該パターンの表面上を疎水化することにより、パターンがその隣のパターンに接触するようなパターンの倒壊を抑制することが可能となる。
第1表に示される配合組成(質量%)に従い、金属微細構造体のパターン倒壊抑制用処理液1~9を調合した。なお、残部は水である。
*2:「サーフロンS-231(商品名)」;AGCセイミケミカル株式会社製パーフルオロアルキルベタイン
*3:「サーフロンS-241(商品名)」;AGCセイミケミカル株式会社製パーフルオロアルキルアミンオキシド
図1(a)に示すように、シリコン基板104上に窒化珪素103(厚さ:100nm)及び酸化珪素102(厚さ:1200nm)を成膜した後、フォトレジスト101を形成した後、該フォトレジスト101を露光、現像することにより、図1(b)に示す円-リング状開口部105(φ125nm、円と円との距離:50nm)を形成し、該フォトレジスト101をマスクとしてドライエッチングにより酸化珪素102に図1(c)に示す円筒状の孔106を、窒化珪素103の層までエッチングして形成した。次いで、フォトレジスト101をアッシングにより除去し、図1(d)に示す酸化珪素102に窒化珪素103の層に達する円筒状孔106が開孔された構造体を得た。得られた構造体の円筒状孔106に、金属107としてタングステンを充填・堆積し(図1-(e))、化学的機械研磨(ケミカルメカニカルポリッシング;CMP)により、酸化珪素102上の余分な金属(タングステン)107を除去し、図1(f)に示す酸化珪素102中に金属(タングステン)の円筒108が埋め込まれた構造体を得た。得られた構造体の酸化珪素102を0.5%フッ酸水溶液により溶解除去(25℃、1分浸漬処理)した後、純水リンス、処理液1~18(30℃、10分浸漬処理)、及び純水リンスの順で接液処理し、乾燥を行い、図1(g)に示す構造体を得た。
ここで、パターンの倒壊は、「FE-SEM S-5500(型番)」:日立ハイテクノロジーズ社製を用いて観察し、倒壊抑制率は、パターン全本数中の倒壊しなかったパターンの割合を算出して求めた数値であり、該倒壊抑制率が50%以上であれば合格と判断した。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第3表に示す。
実施例1において、図1(f)に示される構造体の酸化珪素102をフッ酸により溶解除去した後、純水のみで処理した以外は、実施例1と同様にして図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた(倒壊抑制率は50%未満となる。)。比較例1において使用した処理液、処理方法及び倒壊抑制率の結果を第3表に示す。
実施例1において、図1(f)に示される構造体の酸化珪素102をフッ酸により溶解除去し純水で処理した後、処理液1の代わりに第2表に示す比較液1~13で処理する以外は、実施例1と同様にして図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた。各例2~14において使用した処理液、処理方法及び倒壊抑制率の結果を第3表に示す。
*2:「サーフロンS-111(商品名)」;AGCセイミケミカル(株)製,0.01
%水
*3:「サーフィノール420(商品名)」;日信化学工業株式会社製,0.01%水
*4:「サーフィノール104(商品名)」;日信化学工業株式会社製,0.01%水
*5:「カチオーゲンTML(商品名)」;第一工業製薬株式会社製,0.01%水
*6:「エパン420(商品名)」;第一工業製薬株式会社製,0.01%水
実施例1~9において、金属107としてタングステンの代わりに窒化チタンを用いた以外は実施例1~9と同様にして図1(g)に示す構造体を得た。得られた構造体は、金属(窒化チタン)の円筒108の円筒状のパターン(φ125nm,高さ:1200nm(アスペクト比:9.6),円筒と円筒との間の距離:50nm)を有する微細構造であり、70%以上の該パターンは倒壊することがなかった。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第4表に示す。
比較例1~14において、金属107としてタングステンの代わりに窒化チタンを用いた以外は比較例1~14と同様にして、各々比較例15~27の図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第4表に示す。
実施例1~9において、金属107としてタングステンの代わりに酸化ハフニウムを用いた以外は実施例1~9と同様にして図1(g)に示す構造体を得た。得られた構造体は、金属(酸化ハフニウム)の円筒108の円筒状のパターン(φ125nm,高さ:1200nm(アスペクト比:9.6),円筒と円筒との間の距離:50nm)を有する微細構造であり、70%以上の該パターンは倒壊することがなかった。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第5表に示す。
比較例1~14において、金属107としてタングステンの代わりに酸化ハフニウムを用いた以外は比較例1~14と同様にして、各々比較例28~40の図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第5表に示す。
実施例1~9において、金属107としてタングステンの代わりにタンタルを用いた以外は実施例1~9と同様にして図1(g)に示す構造体を得た。得られた構造体は、金属(タンタル)の円筒108の円筒状のパターン(φ125nm,高さ:1200nm(アスペクト比:9.6),円筒と円筒との間の距離:50nm)を有する微細構造であり、70%以上の該パターンは倒壊することがなかった。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第6表に示す。
比較例1~14において、金属107としてタングステンの代わりにタンタルを用いた以外は比較例1~14と同様にして、各々比較例41~53の図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第6表に示す。
実施例1~9において、金属107としてタングステンの代わりにチタンを用いた以外は実施例1~9と同様にして図1(g)に示す構造体を得た。得られた構造体は、金属(チタン)の円筒108の円筒状のパターン(φ125nm,高さ:1200nm(アスペクト比:9.6),円筒と円筒との間の距離:50nm)を有する微細構造であり、70%以上の該パターンは倒壊することがなかった。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第7表に示す。
比較例1~14において、金属107としてタングステンの代わりにチタンを用いた以外は比較例1~14と同様にして、各々比較例53~65の図1(g)に示す構造体を得た。得られた構造体のパターンの50%以上は、図1(h)に示されるような倒壊をおこしていた。各例において使用した処理液、処理方法及び倒壊抑制率の結果を第7表に示す。
102.酸化珪素
103.窒化珪素
104.シリコン基板
105.円状開口部
106.円筒状孔
107.金属(窒化チタン、タングステン、酸化ハフニウム、タンタルまたはチタン)
108.金属(窒化チタン、タングステン、酸化ハフニウム、タンタルまたはチタン)の円筒
Claims (7)
- フルオロアルキル基を有するアンモニウムハライド、フルオロアルキル基を有するベタイン化合物、およびフルオロアルキル基を有するアミンオキシド化合物からなる群から選択される少なくとも一つを含む金属微細構造体のパターン倒壊抑制用処理液。
- 前記フルオロアルキル基を有するアンモニウムハライド、前記フルオロアルキル基を有するベタイン化合物、および前記フルオロアルキル基を有するアミンオキシド化合物の含有量が10ppm~50%である請求項1に記載の処理液。
- さらに水を含む請求項1または2に記載の処理液。
- 前記金属微細構造体のパターンが、窒化チタン、タングステン、酸化ハフニウム、タンタルおよびチタンからなる群から選択される少なくとも一種の材料を用いてなるものである請求項1~3のいずれかに記載の処理液。
- ウェットエッチングまたはドライエッチングの後の洗浄工程において、請求項1~4のいずれかに記載の処理液を用いることを特徴とする金属微細構造体の製造方法。
- 前記金属微細構造体が、窒化チタン、タングステン、酸化ハフニウム、タンタルおよびチタンからなる群から選択される少なくとも一種の材料を用いてなるものである請求項5に記載の金属微細構造体の製造方法。
- 前記金属微細構造体が、半導体装置またはマイクロマシンである請求項5または6に記載の金属微細構造体の製造方法。
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- 2010-10-19 US US13/502,867 patent/US20120214722A1/en not_active Abandoned
- 2010-10-19 CN CN201080047541.XA patent/CN102598220B/zh active Active
- 2010-10-19 KR KR1020127010125A patent/KR20120116389A/ko active Search and Examination
- 2010-10-19 DE DE112010004602.6T patent/DE112010004602B4/de active Active
- 2010-10-19 JP JP2011537264A patent/JPWO2011049091A1/ja active Pending
- 2010-10-20 TW TW099135765A patent/TWI521314B/zh active
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Publication number | Priority date | Publication date | Assignee | Title |
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US10403491B2 (en) | 2015-07-13 | 2019-09-03 | Fujifilm Corporation | Method for treating pattern structure, method for manufacturing electronic device, and treatment liquid for inhibiting collapse of pattern structure |
WO2017122600A1 (ja) * | 2016-01-13 | 2017-07-20 | 三菱瓦斯化学株式会社 | 半導体基板材料に撥アルコール性を付与する液体組成物および該液体組成物を用いた半導体基板の表面処理方法 |
JPWO2017122600A1 (ja) * | 2016-01-13 | 2018-11-01 | 三菱瓦斯化学株式会社 | 半導体基板材料に撥アルコール性を付与する液体組成物および該液体組成物を用いた半導体基板の表面処理方法 |
US11094526B2 (en) | 2016-01-13 | 2021-08-17 | Mitsubishi Gas Chemical Company, Inc. | Liquid composition for imparting alcohol-repellency to semiconductor substrate material, and method for treating surface of semiconductor substrate using said liquid composition |
Also Published As
Publication number | Publication date |
---|---|
CN102598220B (zh) | 2015-10-07 |
DE112010004602B4 (de) | 2020-01-30 |
KR20120116389A (ko) | 2012-10-22 |
TWI521314B (zh) | 2016-02-11 |
US20120214722A1 (en) | 2012-08-23 |
TW201128326A (en) | 2011-08-16 |
JPWO2011049091A1 (ja) | 2013-03-14 |
CN102598220A (zh) | 2012-07-18 |
DE112010004602T5 (de) | 2013-01-24 |
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