TW201625505A - 燒結體 - Google Patents
燒結體 Download PDFInfo
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- TW201625505A TW201625505A TW104138291A TW104138291A TW201625505A TW 201625505 A TW201625505 A TW 201625505A TW 104138291 A TW104138291 A TW 104138291A TW 104138291 A TW104138291 A TW 104138291A TW 201625505 A TW201625505 A TW 201625505A
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- Taiwan
- Prior art keywords
- sintered body
- oxyfluoride
- mpa
- cerium
- less
- Prior art date
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- 238000013001 point bending Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims description 47
- 239000000843 powder Substances 0.000 claims description 46
- 238000004519 manufacturing process Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 24
- 229910052684 Cerium Inorganic materials 0.000 claims description 23
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 23
- XVVDIUTUQBXOGG-UHFFFAOYSA-N [Ce].FOF Chemical compound [Ce].FOF XVVDIUTUQBXOGG-UHFFFAOYSA-N 0.000 claims description 18
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 17
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 17
- CHBIYWIUHAZZNR-UHFFFAOYSA-N [Y].FOF Chemical compound [Y].FOF CHBIYWIUHAZZNR-UHFFFAOYSA-N 0.000 abstract 3
- 238000000034 method Methods 0.000 description 55
- 230000000052 comparative effect Effects 0.000 description 29
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 24
- 229910052731 fluorine Inorganic materials 0.000 description 23
- 239000007789 gas Substances 0.000 description 20
- 239000002245 particle Substances 0.000 description 18
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 17
- 239000011737 fluorine Substances 0.000 description 17
- 238000005259 measurement Methods 0.000 description 16
- 239000000470 constituent Substances 0.000 description 13
- 229910052736 halogen Inorganic materials 0.000 description 13
- 150000002367 halogens Chemical class 0.000 description 13
- 239000004065 semiconductor Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 12
- 238000005530 etching Methods 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000000465 moulding Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 125000001153 fluoro group Chemical group F* 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000003826 uniaxial pressing Methods 0.000 description 6
- 239000012768 molten material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 230000002706 hydrostatic effect Effects 0.000 description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
- 229940105963 yttrium fluoride Drugs 0.000 description 4
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000004451 qualitative analysis Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- -1 alumina Chemical class 0.000 description 1
- HIPVTVNIGFETDW-UHFFFAOYSA-N aluminum cerium Chemical compound [Al].[Ce] HIPVTVNIGFETDW-UHFFFAOYSA-N 0.000 description 1
- ZWOQODLNWUDJFT-UHFFFAOYSA-N aluminum lanthanum Chemical compound [Al].[La] ZWOQODLNWUDJFT-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- VRPQIIJGEJVXBK-UHFFFAOYSA-N fluoro hypofluorite lanthanum Chemical compound [La].FOF VRPQIIJGEJVXBK-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/553—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on fluorides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/5156—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on rare earth compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/645—Pressure sintering
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B38/0058—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity
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- C04B38/0067—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the density of the end product
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32458—Vessel
- H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
- H01J37/32495—Means for protecting the vessel against plasma
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- 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
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/54—Particle size related information
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Abstract
本發明之燒結體包含釔之氟氧化物。釔之氟氧化物較佳為YOF及/或Y5O4F7。較佳為本發明之燒結體包含50質量%以上之釔之氟氧化物。關於本發明之燒結體,較佳為相對密度為70%以上,又,較佳為開放氣孔率為10%以下。又,亦較佳為本發明之燒結體之3點彎曲強度為10MPa以上且300MPa以下。
Description
本發明係關於一種包含釔之氟氧化物之燒結體。
於半導體之製造中之各步驟、尤其是乾式蝕刻、電漿蝕刻及清洗之步驟中,使用氟系腐蝕性氣體、氯系腐蝕性氣體及使用該等之電漿。半導體製造裝置之構成構件因該等腐蝕性氣體或電漿而腐蝕,又,自構成構件之表面剝離之微細粒子(微粒)容易附著於半導體表面,而導致製品不良。為此,對於半導體製造裝置之構成構件,需使用對鹵素系電漿耐蝕性較高之陶瓷作為主體材料。
作為此種主體材料,現使用氧化鋁、氧化釔、鋁釔複合氧化物、或氟化釔(參照專利文獻1~3)。
又,作為用以防止蝕刻裝置之腐蝕之耐蝕性材料,申請人迄今為止提出有包含釔之氟氧化物之熔射材料(專利文獻4)。
專利文獻1:日本專利特開2011-136877號公報
專利文獻2:日本專利特開2013-144622號公報
專利文獻3:日本專利特開2000-219574號公報
專利文獻4:日本專利特開2014-109066號公報
對於氧化鋁等含鋁化合物,有對半導體矽之鋁污染之擔憂。氧化釔被指摘電漿耐性不充分,表面會因照射氟系電漿發生變質而形成氟化釔(YF3)。氟化釔為氟化物,因此於化學穩定性方面存疑。
又,於將釔之氟氧化物用作熔射材料而塗佈半導體裝置之內部之情形時,所獲得之塗膜之緻密性存在極限,難言遮斷鹵素系腐蝕氣體之性能充分。
因此,本發明之課題在於提供一種能夠解決上述先前技術所存在之各種缺陷的燒結體。
本發明提供一種包含釔之氟氧化物之燒結體。
又,本發明提供一種上述燒結體之製造方法,其包括如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體之步驟;及藉由將上述成形體於5MPa以上且100MPa以下之壓力下、800℃以上且1800℃以下之溫度下進行燒結,而獲得上述燒結體之步驟。
又,本發明提供一種上述燒結體之製造方法,其包括如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體之步驟;及將上述成形體於無加壓下、1000℃以上且2000℃以下之溫度下進行燒結之步驟。
本發明之燒結體對鹵素系電漿顯示出優異之耐性,而作為蝕刻裝置等半導體製造裝置之構成材料有用。又,本發明之燒結體之製造方法可高效率地製造緻密之燒結體作為本發明之燒結體。
圖1係實施例1中所獲得之燒結體之粉末藉由XRD(X ray
diffraction,X射線繞射)繞射測定所獲得之X射線圖。
圖2係實施例2中所獲得之燒結體之粉末藉由XRD繞射測定所獲得之X射線圖。
圖3係實施例3中所獲得之燒結體之粉末藉由XRD繞射測定所獲得之X射線圖。
圖4係實施例4中所獲得之燒結體之粉末藉由XRD繞射測定所獲得之X射線圖。
圖5係實施例2中所獲得之燒結體於電漿照射前後之SEM(Scanning Electron Microscope,掃描式電子顯微鏡)照片。
圖6係比較例1之單晶矽於電漿照射前後之SEM照片。
圖7係比較例2之氧化鋁於電漿照射前後之SEM照片。
圖8係比較例3之氧化釔於電漿照射前後之SEM照片。
圖9係比較例4之氟化釔於電漿照射前後之SEM照片。
圖10係表示於實施例及比較例之試樣表面於電漿照射前後之F/O比之變化的圖表。
圖11係實施例2中所獲得之燒結體於電漿照射後之剖面SEM照片及元素分佈圖。
圖12係比較例3中所獲得之燒結體於電漿照射後之剖面SEM照片及元素分佈圖。
以下,基於本發明之較佳之實施形態說明本發明。本發明之燒結體之特徵之一在於包含釔之氟氧化物。本發明之釔之氟氧化物係包含釔(Y)、氧(O)、氟(F)之化合物。作為釔之氟氧化物,可為釔(Y)、氧(O)、氟(F)之莫耳比為Y:O:F=1:1:1之化合物。或者,作為釔之氟氧化物,亦可為上述莫耳比為Y:O:F=1:1:1之化合物以外之化合物。作為此種化合物,包含包括Y5O4F7或Y7O6F9等在內之該等中
1種以上之氟氧化物。該等可使用1種或將2種以上組合而使用。於本發明中,較佳為上述莫耳比為Y:O:F=1:X:3-2X(X為0.5~1.2)之化合物,尤佳為YOF及Y5O4F7。
藉由使用YOF,而具有獲得機械強度優異之燒結體、獲得緻密且無破裂之燒結體、與其他組成相比耐蝕性優異等優點。又,藉由使用Y5O4F7,具有於低溫下獲得緻密且無破裂之燒結體、藉由在氧化後生成YOF而提高耐蝕性等優點。
於本發明中,將釔之氟氧化物製成燒結體而非製成熔射材料,藉此可提高對鹵素系腐蝕氣體之阻隔性。於製成熔射材料之情形時,存在如下情況:構成熔射材料之各粒子因熔射而熔解者堆積形成熔射膜,導致於該熔解之粒子間之微小空隙流入鹵素系腐蝕氣體。與其相比,燒結體之緻密性較高,對鹵素系腐蝕氣體之阻隔性優異,因此例如將其用於半導體裝置之構成構件之情形時,可防止鹵素系腐蝕氣體向該部材內部之流入。因此,本發明之燒結體係防止因鹵素系腐蝕氣體引起之腐蝕的性能較高者。如此鹵素系腐蝕氣體之阻隔性較高之部材被適宜地用於例如蝕刻裝置之真空室構成構件或蝕刻氣體供給口、聚焦環、晶圓支架等。就將本發明之燒結體製成更緻密者之觀點而言,該燒結體之相對密度較佳為70%以上,更佳為80%以上,進而較佳為90%,尤佳為95%以上。相對密度(RD)越高越好,作為上限可列舉100%。就提高耐蝕性之觀點而言,較佳為氣孔率、尤其是開放氣孔率(OP)較小。開放氣孔率係藉由下述所記載之方法求出,較佳為10%以下,進而較佳為2%以下,尤佳為0.5%以下。具有此種相對密度(RD)及開放氣孔率(OP)之燒結體於藉由下述製造方法(1)或(2)製造本發明之燒結體時,可藉由調整其溫度條件或壓力條件而獲得。
此處所謂相對密度(RD)及開放氣孔率可基於JIS R1634,藉由阿基米德法進行測定,具體而言,藉由以下之方法進行測定。
將燒結體放入蒸餾水中,於利用膜片型真空泵之減壓下保持1小時後,測定水中重量W2[g]。又,利用濕布去除多餘之水分,測定飽水重量W3[g]。其後,放入乾燥器使燒結體充分地乾燥後,測定乾燥重量W1[g]。根據以下之式,算出鬆密度ρb[g/cm3]與開放氣孔率OP。
ρb=W1/(W3-W2)×ρ1(g/cm3)
OP=(W3-W1)/(W3-W2)×100(%)
此處,ρ1[g/cm3]係蒸餾水之密度。使用所獲得之鬆密度ρb、及理論密度ρc[g/cm3],根據以下之式算出相對密度(RD)[%]。
RD=ρb/ρc×100(%)
又,本發明之燒結體之3點彎曲強度σf較佳為一定以上之較高值。具體而言,本發明之燒結體之3點彎曲強度σf較佳為10MPa以上,更佳為20MPa以上,進而較佳為50MPa以上,尤佳為100MPa以上。又,3點彎曲強度σf越高,作為半導體製造裝置之構成材料越具備高強度,故而較佳,作為上限,就燒結體之製造之容易性等觀點而言,較佳為300MPa以下。具有上述強度之燒結體可藉由利用下述之製造方法(1)或(2)製造本發明之燒結體而獲得。
3點彎曲強度σf係藉由以下之方法進行測定。
藉由切斷燒結體,並對單面進行鏡面研磨,而製作厚度1.5~3.0mm、寬度約4mm、長度約35mm之短條形之試片。將其置於SiC製治具上,利用萬能材料試驗機(1185型,INSTRON製造)進行3點彎曲試驗。條件設為支點間距離30mm、十字頭速度0.5mm/min、試片數設為5片。基於JIS R1601,使用以下之式算出彎曲強度σf[MPa]。
σf=(3×Pf×L)/(2×w×t2)(MPa)
此處,Pf為試片斷裂時之荷重[N],L為跨距[mm],w為試片之寬
度[mm],t為試片之厚度[mm]。
又,本發明之燒結體之彈性模數較佳為25GPa以上且300GPa以下,更佳為50GPa以上且300GPa以下,進而較佳為100GPa以上且250GPa以下,最佳為150GPa以上且200GPa以下。藉由設為此種範圍之彈性模數,作為半導體製造裝置之構成材料成為具備較高之耐久性者,且對鹵素系電漿顯示出優異之耐性。作為用以獲得此種彈性模數之方法之一,可列舉於下述燒結體之製造方法中,調整原料粉末之平均粒徑、成形方法、加壓方法等之方法。
彈性模數係依據JIS R1602,藉由以下之方法而求出。
測定係使用示波器(Oscilloscope)(WJ312A,LECROY製造)及脈衝發生接收器(Pulser-Receiver,5072PR,Olympus NDT製造)。使用接著劑(縱波用:COUPLANT B GLYCERIN(Olympus製造),橫波用:Sony Cote SHN-B25(Nichigo Nikko製造))使縱波振子(V110,5MHz)、橫波振子(V156,5MHz)固定於試片,根據脈衝之傳輸速度測定縱波速度V1[m/s]與橫波速度Vt[m/s]。根據所獲得之V1與Vt、試片之鬆密度ρb[kg/mm3],使用以下之式算出彈性模數E[GPa]。
E=ρb.(Vt 2.V1 2-4Vt 4)/(V1 2-Vt 2)×10-9(GPa)
又,本發明之燒結體之熱導率較佳為5.0W/(m.K)以上,更佳為10.0W/(m.K)以上。如此具有較高之熱導率之燒結體可適宜地用於要求均熱性之構成構件或溫度變化較大之構成構件之用途。又,於將本發明之燒結體用於蝕刻裝置之氣體或電氣等之導入端子等要求隔熱性之構成構件之用途之情形時,該燒結體之熱導率為5.0W/(m.K)以下,尤佳為低至3.0W/(m.K)以下程度。熱導率可藉由以下方式進行測定。
使用邊長10mm、厚度1mm之正方形板狀試樣。於試樣之兩面塗佈鉑,自其上較薄地噴附加入有碳粒子之噴霧(FC-153,Fine Chemical Japan製造)。將經黑化處理之試樣設置於治具,對正面照射由氙閃光燈產生之脈衝(脈衝寬度0.33ms),測定試樣背面之溫度變化,藉此求出熱擴散係數α。溫度變化係將半數時間之10倍設為計算範圍。又,使用氧化鋁作為標準試樣,求出比熱容量C。於溫度25℃、濕度50%、空氣中進行測定,且進行3次測定。測定係使用熱常數測定裝置(LFA447,NETZSCH製造)。
基於JIS R1611,使用以下之式求出熱導率λ[W/(m.K)]。
λ=α×C×ρ(W/(m.K))
此處,α為熱擴散係數[m2/s],C為比熱容量[J/kg.K],ρ為試樣之鬆密度[kg/m3]。
本發明之燒結體可為實質上僅包含釔之氟氧化物者,但亦可包含釔之氟氧化物以外之成分。所謂實質上,意指除了氟氧化物以外,僅包含不可避免之雜質,具體而言,係指氟氧化物之含量為98質量%以上。作為此處所謂之不可避免之雜質,例如可列舉於藉由下述之(1)或(2)之方法進行製造之情形時之氧化釔等副產物。
具體而言,就進一步發揮本發明之耐電漿性之效果之觀點、或機械強度提高等觀點而言,本發明之燒結體中之釔之氟氧化物之含量較佳為50質量%以上。就該觀點而言,燒結體中之釔之氟氧化物之量更佳為80質量%以上,進而較佳為90質量%以上,尤佳為98質量%以上。燒結體中之釔之氟氧化物之含量越高越好。
於藉由定性分析確認到本發明之燒結體包含釔之氟氧化物及氧化釔之情形時,燒結體中之釔之氟氧化物之含量可藉由以下之方法進行測定。該情形時之定性分析例如可藉由X射線繞射測定而進行。
針對將氧化釔與氟氧化釔以一定比率混合而成之粉末試樣,進
行X射線繞射測定。所獲得之繞射波峰中,取氧化釔之最大波峰強度與氟氧化釔之最大波峰強度之比,相對於混合比進行繪圖,而製作校準曲線。按照校準曲線,測定氧化釔與氟氧化釔之混合比,將於兩者之合計設為100之情形時之氟氧化釔之比率設為氟氧化釔之含量。燒結體之X射線繞射測定係將燒結體製成粉末者之測定,可藉由下述實施例中所記載之方法進行。
又,於藉由上述定性分析而判明燒結體中包含釔之氟氧化物及氧化釔以外之物質之情形時,針對該物質,與上述方法同樣地測定該物質與氟氧化釔之混合比,藉此求出氟氧化釔之含量即可。
本發明之燒結體於將其製成粉末時之使用CuKα射線或Cu-Kα1射線之X射線繞射測定(掃描範圍:2θ=10°~80°)中,最大強度之繞射波峰較佳為源自釔之氟氧化物之波峰。又,於該X射線繞射測定中,觀察到源自釔之氟氧化物以外之成分之波峰亦無妨,但較佳為該波峰較小,或未觀察到該波峰。例如於將上述掃描範圍內之源自釔之氟氧化物之最大波峰之高度設為1時,源自釔之氟氧化物以外之成分之最大波峰之高度較佳為0.5以下,更佳為0.05以下。尤其於上述X射線繞射測定中,於將上述掃描範圍內之源自釔之氟氧化物之最大波峰之高度設為1時,源自YF3之波峰之最大波峰之高度較佳為0.1以下,更佳為0.03以下。又,於上述X射線繞射測定中,於將上述掃描範圍內之源自釔之氟氧化物之最大波峰之高度設為1時,源自Y2O3之最大波峰之高度較佳為0.2以下,更佳為0.05以下。燒結體粉末之X射線繞射測定可藉由下述實施例中所記載之方法進行。本發明之燒結體之上述波峰比可藉由調整原料粉末中之釔之氟氧化物之比率、或燒結條件之溫度或燒結氛圍等,而設為上述範圍內。
於本發明之燒結體包含YOF之情形時,作為該YOF較佳為包含菱形晶體(rhombohedral crystal),於本發明之燒結體包含Y5O4F7之情形
時,作為該Y5O4F7較佳為包含斜方晶體(orthorhombic crystal)。該等結晶相可藉由進行燒結體表面或粉末之X射線繞射測定而鑑定。
作為本發明之燒結體中之釔之氟氧化物以外之成分,例如可列舉:各種燒結助劑、黏合劑樹脂、碳等。又,本發明之燒結體除了釔之氟氧化物以外,亦可含有先前使用之氧化鋁、氧化釔、鋁釔複合氧化物、或氟化釔、含有釔以外之其他稀土元素之化合物等各種陶瓷材料。
本發明之燒結體藉由為包含釔之氟氧化物之燒結體,而與其他陶瓷材料之燒結體相比,對鹵素系電漿具有優異之耐性,又,與先前之包含釔之氟氧化物之熔射材料相比,緻密性及對鹵素系腐蝕性氣體之阻隔性優異。
以下,對本發明之燒結體之較佳之製造方法進行說明。作為本發明之燒結體之製造方法,例如可列舉以下之(1)之方法。
(1)一種燒結體之製造方法,其具有如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體之步驟;及藉由將上述成形體於5MPa以上且100MPa以下之壓力下,於800℃以上且1800℃以下之溫度下進行燒結,而獲得上述燒結體之步驟。
首先,對(1)之方法進行說明。
於上述(1)之方法中,獲得成形體之步驟與燒結成形體之步驟亦可同時進行。例如,將粉末試樣置入模具中,將其直接加壓燒結之方法亦包括在上述(1)之方法中。
作為包含上述釔之氟氧化物之原料粉末中之釔之氟氧化物,可列舉與上述燒結體所含之釔之氟氧化物相同者。原料所使用之釔之氟氧化物通常為粉末狀。原料粉末所含之釔之氟氧化物之平均粒徑較佳為5μm以下,更佳為1.5μm以下,進而較佳為1.1μm以下,尤佳為1μm以下。平均粒徑係體積基準之累計分率為50%之粒徑(以下,簡稱
為「D50」),且係藉由雷射繞射、散射式粒度分佈測定法進行測定。具體之測定方法如下所述。作為原料粉末之平均粒徑之較佳粒徑,可列舉與原料粉末所含之釔之氟氧化物之平均粒徑相同之粒徑。
(平均粒徑之測定方法)
利用日機裝股份有限公司製造之Microtrac HRA進行測定。測定時係使用2質量%六偏磷酸鈉水溶液作為分散介質,向Microtrac HRA之試樣循環器之室中添加試樣(顆粒)直至裝置判定為適當濃度為止。
原料粉末除了釔之氟氧化物以外,亦可使用上述之燒結助劑或黏合劑等作為其他成分,較佳為本發明之燒結體之燒結助劑及黏合劑樹脂等其他成分之量較少。尤其於原料粉末中,燒結助劑較佳為5質量%以下,更佳為2質量%以下。本發明之製造方法之特徵之一在於即便不使用燒結助劑,或儘量減少其量,亦可獲得緻密之燒結體。作為此處所謂之燒結助劑,可列舉:SiO2、MgO、CaO、進而各種稀土類氧化物等。原料粉末之成形可使用模具加壓法、橡膠加壓(靜水壓)法、板材成形法、擠出成形法、鑄造成形法等。於無加壓燒結之情形時,較佳為藉由利用油壓加壓等所進行之單軸加壓進行加壓後,進行靜水壓而成形。該情形時之單軸加壓之壓力較佳為20MPa以上且85MPa以下,更佳為22MPa以上且75MPa以下。又,靜水壓時之壓力較佳為85MPa以上且250MPa以下,更佳為100MPa以上且220MPa以下。於進行加壓燒結之情形時,較佳為藉由利用油壓加壓等所進行之單軸加壓進行加壓成形後,進行加壓燒結。作為該情形時之單軸加壓之壓力,較佳為10MPa以上且100MPa以下,更佳為15MPa以上且80MPa以下。原料粉末中,釔之氟氧化物之含量較佳為80質量%以上,更佳為95質量%以上,尤佳為98質量%以上。
於(1)之方法中,將上述中所獲得之成形體加壓燒結。作為具體之加壓燒結法,可使用熱壓、脈衝通電加壓(SPS)、熱靜水壓(HIP)。
作為加壓燒結之加壓壓力,較佳為5MPa以上且100MPa以下。藉由設為5MPa以上,具有容易獲得緻密且耐電漿性較高之燒結體之優點,藉由設為100MPa以下,具有抑制衝壓模具之破損等優點。就該等觀點而言,加壓燒結之加壓壓力較佳為20MPa以上,更佳為100MPa以下。又,燒結溫度較佳為800℃以上且1800℃以下。藉由設為800℃以上,具有容易促進緻密化,此外使所添加之黏合劑分解、蒸發,原料中所含之未反應成分發生反應而形成氟氧化物等優點。藉由設為1800℃以下,具有抑制氟氧化物之分解,抑制加壓燒結設備之損壞之優點。就該等觀點而言,燒結溫度更佳為1000℃以上且1700℃以下。
又,於上述範圍內之壓力及溫度下加壓燒結之時間(最高溫度下之保持時間)較佳為0小時以上且6小時以下,更佳為20分鐘以上且2小時以下。
尤其於熱壓之情形時,作為加壓燒結之加壓壓力,較佳為30MPa以上且50MPa以下,燒結溫度較佳為1300℃以上且1700℃以下。又,於脈衝通電加壓燒結之情形時,作為加壓燒結之加壓壓力,較佳為30MPa以上且100MPa以下,燒結溫度更佳為1000℃以上且1500℃以下。
本發明之燒結體亦可代替(1)之方法而藉由下述(2)之方法適宜地製造。
(2)一種燒結體之製造方法,其具有如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體之步驟;及將上述成形體於無加壓下,於1000℃以上且2000℃以下之溫度下進行燒結之步驟。
(2)之方法於進行無加壓燒結之方面與(1)之方法不同,但獲得原料粉末之成形體之步驟與(1)之方法相同。
就獲得緻密之燒結體之觀點,或去除混入之有機物之觀點而言,燒結溫度較佳為1000℃以上,就抑制氟氧化物之分解,抑制對加壓燒結設備之損壞等觀點而言,較佳為2000℃以下。就該等觀點而言,燒結溫度更佳為1200℃以上且1800℃以下。又,於上述燒結溫度下燒結之時間(最高溫度下之保持時間)較佳為0小時以上且24小時以下,更佳為0小時以上且6小時以下。於本製造方法中,即便為無加壓燒結亦可將上述原料粉末於上述溫度下進行燒結,藉此可獲得充分緻密之燒結體。
(1)及(2)中之任一方法中之燒結均可於含氧之氛圍下進行,亦可於惰性氛圍下進行。然而,就防止生成氧化釔之觀點而言,較佳為於惰性氛圍下進行。作為含氧之氛圍,可列舉大氣,作為惰性氛圍,可列舉氬氣等稀有氣體或氮氣或真空等。又,關於(1)及(2)中之任一方法中之燒結,至1200℃之升溫及降溫較佳為以0.5℃/分鐘以上且40℃/分鐘以下之速度進行,1200℃以上之溫度區域之升溫及降溫較佳為以1℃/分鐘以上且30℃/分鐘以下之速度進行。
如此而獲得之燒結體可用於蝕刻裝置中之真空室及該室內之試樣台或夾頭、聚焦環、蝕刻氣體供給口等半導體製造裝置之構成構件。又,本發明之燒結體除了可用於半導體製造裝置之構成構件以外,亦可用於各種電漿處理裝置、化學設備之構成構件之用途。
以下,藉由實施例進一步詳細地說明本發明。然而,本發明之範圍並不限定於該實施例。
[實施例1](藉由無加壓燒結所進行之包含YOF之燒結體之製造)
將YOF粉末(平均粒徑0.8μm)約1.4g置入直徑15mm之圓形之模具中,藉由油壓加壓以25.5MPa之壓力進行單軸加壓並保持1分鐘,而進行一次成形。將所獲得之一次成形品進而以200MPa保持1分鐘
而進行均壓成形。將其置入氧化鋁製之坩堝中,鋪上底粉,於其上放置成形體,蓋上蓋子,進而將坩堝整體置入碳製之較大坩堝中。於Ar氣流中(流速2升/分鐘),以30℃/min升溫至1200℃,進而以10℃/min升溫至1600℃,於1600℃下保持1小時後,以10℃/min降溫至1200℃,其後以30℃/min降溫。藉此獲得燒結體。對所獲得之燒結體藉由上述方法測定相對密度RD,結果為96%,開放氣孔率為0.2%。藉由下述方法,測定所獲得之燒結體之粉末之XRD。將所獲得之X射線圖示於圖1。如圖1所示,於該X射線圖中,僅觀察到視為源自YOF之波峰,未觀察到源自YOF以外之成分之波峰,僅使用YOF作為原料粉末,據此視為該燒結體係包含大致100質量%之YOF者。對實際獲得之燒結體藉由上述方法測定釔之氟氧化物之量,結果為100質量%。
使用磁製研缽與研杵將燒結體之一部分粉碎而獲得粉末,將該粉末設置於玻璃製支架上,進行XRD測定。XRD之測定條件設為:連續掃描下、Cu靶、球管電壓40kV、球管電流30mA、掃描範圍2θ=10°~80°、掃描速度0.050°2θ/s。Kβ射線係利用彎曲石墨濾波器而去除。
[實施例2](藉由加壓燒結所進行之包含YOF之燒結體之製造)
將YOF粉末(平均粒徑0.8μm)約20g置入縱35mm、橫35mm之四角形之模具中,藉由油壓加壓,以18.4MPa之壓力進行一次成形。將其置入與上述方形模具相同之尺寸之碳製之熱壓模具中,藉由熱壓進行燒結。於Ar流中(流速2升/分鐘),以30℃/min升溫至1200℃,進而以10℃/min升溫至1600℃,於1600℃下保持1小時後,以10℃/min降溫至1200℃,其後以30℃/min降溫。於1600℃下保持1小時之期間,以36.7MPa之壓力進行單軸加壓。藉此獲得燒結體。對實際獲得之燒結體藉由上述方法測定相對密度RD,結果為99.5%,開放氣孔率為
0.1%。又,藉由上述方法測定3點彎曲強度,結果為120MPa。又,藉由上述方法測定彈性模數,結果為183GPa,藉由上述方法測定熱導率,結果為17W/(m.K)。與實施例1同樣地,測定所獲得之燒結體之粉末之XRD。將所獲得之X射線圖示於圖2。如圖2所示,於該X射線圖中,僅觀察到視為源自YOF之波峰,未觀察到源自除YOF以外之成分之波峰,作為原料粉末僅使用YOF,據此視為該燒結體含有100質量%之YOF。對所獲得之燒結體藉由上述方法測定釔之氟氧化物之量,結果為100質量%。
[實施例3](藉由無加壓燒結所進行之包含Y5O4F7之燒結體之製造)
將Y5O4F7粉末(平均粒徑1.1μm)約1.4g置入直徑15mm之圓形之模具中,藉由油壓加壓以25.5MPa之壓力進行單軸加壓並保持1分鐘,而進行一次成形。對所獲得之一次成形品,進而以200MPa保持1分鐘而進行均壓成形。將其置入氧化鋁(alumina)製坩堝中,鋪上底粉,於其上放置成形體,蓋上蓋子,進而將坩堝整體置入碳製之較大之坩堝中。於Ar氣流中(流速2升/分鐘),以30℃/min升溫至1200℃,進而以10℃/min升溫至1400℃後,以10℃/min降溫至1200℃,其後以30℃/min降溫。藉此獲得燒結體。於1400℃下之保持時間為0小時。對所獲得之燒結體藉由上述方法測定相對密度RD,結果為99.6%,開放氣孔率為0.1%。又,針對所獲得之燒結體,與實施例1同樣地測定所獲得之燒結體之粉末之XRD。將所獲得之X射線圖示於圖3。如圖3所示,於該X射線圖中,主要觀察到視為源自Y5O4F7之波峰,僅觀察到極少視為源自Y5O4F7以外之成分之波峰,僅使用Y5O4F7作為原料粉末,據此視為該燒結體係含有Y5O4F795質量%以上者。
[實施例4](藉由加壓燒結所進行之包含Y5O4F7之燒結體之製造)。
將Y5O4F7粉末(平均粒徑1.1μm)約20g置入縱35mm、橫35mm之四角形之模具中,藉由油壓加壓,以18.4MPa之壓力進行一次成形。
將其置入與上述方形模具相同尺寸之碳製之熱壓模具中,藉由熱壓進行燒結。於Ar氣流中(流速2升/分鐘),以30℃/min升溫至1200℃,進而以10℃/min升溫至1400℃後,以10℃/min降溫至1200℃,其後以30℃/min降溫。於1400℃下之保持時間為0小時。於溫度為1200℃以上之期間,以36.7MPa進行單軸加壓。藉此獲得燒結體。對所獲得之燒結體藉由上述方法測定相對密度RD,結果為99.8%,開放氣孔率為0.1%。又,對所獲得之燒結體藉由上述方法測定3點彎曲強度,結果為26MPa。又,藉由上述方法測定彈性模數,結果為157GPa,藉由上述方法測定熱導率,結果為2.9W/(m.K)。又,針對所獲得之燒結體,與實施例1同樣地測定所獲得之燒結體之粉末之XRD。將所獲得之X射線圖示於圖4。如圖4所示,於該X射線圖中,主要觀察到視為源自Y5O4F7之波峰,僅觀察到極少源自Y5O4F7以外之成分之波峰,及僅使用Y5O4F7作為原料粉末,據此視為該燒結體係包含Y5O4F795質量%以上者。
[實施例5](藉由無加壓燒結所進行之包含YOF之燒結體之製造)
除了將於Ar氣體氛圍下燒結設為大氣氛圍下,將1600℃下之保持時間由1小時設為2小時,除此以外,與實施例1同樣地獲得相對密度RD為87%,開放氣孔率為0.2%之燒結體。XRD測定之結果為,該燒結體除了YOF亦含有大量之Y2O3。
[比較例1]
使用單晶矽(Si)。
[比較例2]
使用氧化鋁(Al2O3)之燒結體。
[比較例3]
使用氧化釔(Y2O3)之燒結體。
[比較例4]
使用氟化釔(YF3)之燒結體。
針對實施例2中所獲得之燒結體、比較例1之單晶及比較例2~4之燒結體,藉由如以下之[評價1]所記載般進行SEM觀察(S-4800,Hitachi High-Technologies Corporation)而評價耐電漿性。
[評價1]
利用電漿處理裝置(PT7160,ELMINET),對實施例2中所獲得之燒結體、比較例1之單晶及比較例2~4之燒結體之表面,照射CF4+O2電漿。將CF4設為0.8刻度,將O2設為0.2刻度,將輸出設為100W並保持30分鐘。
利用掃描型電子顯微鏡(SEM)觀察電漿照射前後之實施例2及比較例1~4之各固體表面。將分別對固體表面攝影而獲得之SEM照片示於圖5~圖9。於圖5~圖9中各自上側為照射前之SEM照片,下側為照射後之SEM照片。
如圖5所示,幾乎未見實施例2之釔之氟氧化物於照射前後之變化。相對於此,如圖6所示,確認到比較例1之矽於照射前較平坦,但於照射後表面粗糙之情況。如圖7所示,確認到比較例2之氧化鋁(alumina)於照射後,產生大量之照射前未見之白色粒子。如圖8所示,幾乎未見比較例3之氧化釔於照射前後之變化。如圖9所示,比較例4之氟化釔於照射後大量產生龜裂。
據此,根據燒結體表面之SEM觀察,顯示出實施例2之釔之氟氧化物之燒結體及比較例3之氧化釔之燒結體與其他燒結體或單晶相比對鹵素系電漿具有耐性。
以下,對上述[評價1]中所獲得之電漿照射前後之各試樣,進而藉由以下之[評價2]所記載之評價方法對耐電漿性進行評價。
[評價2]
針對各試樣表面,利用附屬於掃描型電子顯微鏡(S-4800,
Hitachi High-Technologies Corporation)之裝置進行EDX(Energy Dispersive X-ray,能量色散X射線)分析。將倍率設為5000倍,使加速電壓變化為1kV、3kV、10kV及30kV而進行測定,藉由ZAF法利用下述式求出相對於電子穿透深度R的原子質量濃度Ci之變化。進而根據所求出之關係求出自各試樣表面起至電子穿透深度0.1μm(100nm)為止之部分之F原子及O原子之質量濃度。根據所獲得之濃度,求出該部分之F/O之原子比。將表示電漿照射前之F/O之原子比(照射前F/O)、電漿照射後之F/O之原子比(照射後F/O)、及電漿照射前後之F/O之原子比之變化量(照射後F/O/照射前F/O)之圖表示於圖10。於下述式中ρ為密度,A為原子量,E0為加速電壓,λ0為0.182。Z為平均原子序,若將各者之元素之原子序設為Zi,將質量濃度設為Ci,則以Z=ΣCiZi表示。
如圖10所示,於各比較例之矽(Si)、氧化鋁(Al2O3)、氧化釔(Y2O3)及氟化釔(YF3)之各試樣中,藉由氟系電漿照射,F/O比大幅度增加。即,確認到F元素向該等試樣表面之侵入。尤其關於比較例3之氧化釔(Y2O3),照射後之F/O比不到照射前之2倍,關於比較例4之氟化釔(YF3),照射後之F/O比超過照射前之2倍,因氟系電漿照射而於該等燒結體表面氟大幅度增加。相對於此,於實施例2之釔之氟氧化物之試樣中,因電漿照射而引起之F/O比之增加極少,幾乎不發生變化。因此,認為釔之氟氧化物對含氟電漿之穩定性最高。
上述[評價1]中所獲得之電漿照射後之各試樣中,對比較例3之氧
化釔(yttria)試樣及實施例1之釔之氟氧化物之試樣藉由以下之方法進行評價,進而藉由以下之[評價3]所記載之評價方法對耐電漿性進行評價。
[評價3]
於電漿照射後之試樣之表面蒸鍍鉑作為記號後,利用日立離子研磨裝置IM4000,與表面垂直地照射Ar離子,而製作剖面觀察用試樣。利用裝有高感度之EDX之掃描型電子顯微鏡(SU-8200,Hitachi High-Technologies Corporation)觀察該剖面觀察用試樣,而獲得SEM照片,並且獲得氧、氟、鉑、釔之原子分佈圖。將實施例2之燒結體剖面之SEM照片及原子分佈圖示於圖11,將比較例3之燒結體剖面之SEM照片及原子分佈圖示於圖12。於圖11及圖12之任一者中,上部左側均為SEM照片,上部右側均為氟原子分佈圖,下部右側均為鉑原子分佈圖,下部左側均為將鉑原子分佈圖與氟原子分佈圖重疊之圖。
於圖11及圖12中之上部左側之SEM圖像中,沿上下方向延伸之帶狀者為鉑塗層,其左側為試樣。鉑層之右側為離子研磨時之再堆積層,並非原來之試樣。即,鉑之緊鄰左側為試樣之表面。本發明之燒結體由於包含YOF,故而本身含有氟元素。因此,於圖11中,於氟原子分佈圖之上部右側之圖中,屬於鉑層之黑色部分以外之灰色部分表示氟原子之存在位置,該灰色部分在屬於鉑之黑色部分之左側整體地擴展。即,根據圖11中之氟原子分佈圖,與氟距表面之深度無關,同樣地分佈。於圖11之下部左側之使鉑原子分佈圖與氟原子分佈圖重疊之圖中亦相同,未見試樣表面之氟原子之聚集。即,於本發明之燒結體中,未見氟電漿之影響。
另一方面,儘管比較例3之氧化釔(yttria)燒結體原本不含氟,但於觀察電漿照射後之該燒結體剖面之圖12中,由於上部右側之氟原子分佈圖中存在灰色部分,故而於該部分存在氟。由圖12之下部左側之
使鉑原子分佈圖與氟原子分佈圖重疊之圖及圖12之SEM照片明確,所謂比較例3之燒結體中之氟原子之存在位置係集中於鉑層之緊鄰左側,其距試樣表面約50nm之範圍。即,可知關於比較例3之氧化釔之燒結體,因電漿照射,氟原子侵入表面。
結合考慮上述[評價1]~[評價3]之結果,明確本發明之燒結體對鹵素系電漿之耐蝕性高於比較例1~4之任一材料。因此,明確本發明之燒結體作為蝕刻裝置等半導體製造裝置之構成構件有用。
Claims (10)
- 一種燒結體,其包含釔之氟氧化物。
- 如請求項1之燒結體,其中釔之氟氧化物為YOF。
- 如請求項1之燒結體,其中釔之氟氧化物為Y5O4F7。
- 如請求項1之燒結體,其包含50質量%以上之釔之氟氧化物。
- 如請求項1之燒結體,其相對密度為70%以上。
- 如請求項1之燒結體,其開放氣孔率為10%以下。
- 如請求項1之燒結體,其彈性模數為25GPa以上且300GPa以下。
- 如請求項1之燒結體,其3點彎曲強度為10MPa以上且300MPa以下。
- 一種如請求項1之燒結體之製造方法,其包括如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體的步驟;及藉由將上述成形體於5MPa以上且100MPa以下之壓力下、800℃以上且1800℃以下之溫度下進行燒結,而獲得上述燒結體之步驟。
- 一種如請求項1之燒結體之製造方法,其包括如下步驟:獲得包含釔之氟氧化物之原料粉末之成形體的步驟;及將上述成形體於無加壓下、1000℃以上且2000℃以下之溫度下進行燒結之步驟。
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