TWI303857B - Aluminum nitride sintered body, semiconductor manufacturing member, and method of manufacturing aluminum nitride sintered body - Google Patents
Aluminum nitride sintered body, semiconductor manufacturing member, and method of manufacturing aluminum nitride sintered body Download PDFInfo
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- TWI303857B TWI303857B TW095110229A TW95110229A TWI303857B TW I303857 B TWI303857 B TW I303857B TW 095110229 A TW095110229 A TW 095110229A TW 95110229 A TW95110229 A TW 95110229A TW I303857 B TWI303857 B TW I303857B
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- sintered body
- aluminum nitride
- nitride sintered
- volume resistivity
- raw material
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 94
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 239000004065 semiconductor Substances 0.000 title claims description 18
- 239000002994 raw material Substances 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 35
- 239000011777 magnesium Substances 0.000 claims description 28
- 229910052749 magnesium Inorganic materials 0.000 claims description 27
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 26
- 238000005121 nitriding Methods 0.000 claims description 24
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000011164 primary particle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 description 49
- 238000000034 method Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 13
- 238000010304 firing Methods 0.000 description 13
- 239000000758 substrate Substances 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- 239000000395 magnesium oxide Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910000420 cerium oxide Inorganic materials 0.000 description 6
- 150000004767 nitrides Chemical class 0.000 description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 6
- 229910052723 transition metal Inorganic materials 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 229910052596 spinel Inorganic materials 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- 229910016523 CuKa Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000011361 granulated particle Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000010977 jade Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 101000986989 Naja kaouthia Acidic phospholipase A2 CM-II Proteins 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 241000283984 Rodentia Species 0.000 description 1
- 241000239226 Scorpiones Species 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- SKKNACBBJGLYJD-UHFFFAOYSA-N bismuth magnesium Chemical compound [Mg].[Bi] SKKNACBBJGLYJD-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229960001759 cerium oxalate Drugs 0.000 description 1
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- OHMBHFSEKCCCBW-UHFFFAOYSA-N hexane-2,5-diol Chemical compound CC(O)CCC(C)O OHMBHFSEKCCCBW-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000000504 luminescence detection Methods 0.000 description 1
- UHNWOJJPXCYKCG-UHFFFAOYSA-L magnesium oxalate Chemical compound [Mg+2].[O-]C(=O)C([O-])=O UHNWOJJPXCYKCG-UHFFFAOYSA-L 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 oxidized oxide Chemical compound 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- E—FIXED CONSTRUCTIONS
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- E05D15/00—Suspension arrangements for wings
- E05D15/26—Suspension arrangements for wings for folding wings
- E05D15/264—Suspension arrangements for wings for folding wings for bi-fold wings
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- E—FIXED CONSTRUCTIONS
- E05—LOCKS; KEYS; WINDOW OR DOOR FITTINGS; SAFES
- E05D—HINGES OR SUSPENSION DEVICES FOR DOORS, WINDOWS OR WINGS
- E05D7/00—Hinges or pivots of special construction
- E05D7/08—Hinges or pivots of special construction for use in suspensions comprising two spigots placed at opposite edges of the wing, especially at the top and the bottom, e.g. trunnions
- E05D7/081—Hinges or pivots of special construction for use in suspensions comprising two spigots placed at opposite edges of the wing, especially at the top and the bottom, e.g. trunnions the pivot axis of the wing being situated near one edge of the wing, especially at the top and bottom, e.g. trunnions
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/32—Arrangements of wings characterised by the manner of movement; Arrangements of movable wings in openings; Features of wings or frames relating solely to the manner of movement of the wing
- E06B3/48—Wings connected at their edges, e.g. foldable wings
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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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Description
1303857 九、發明說明·· 【發明所屬之技術領域】 >本發㈣有㈣氮化料結體、半㈣製制構件及 鼠化鋁燒結體之製造方法。 【先前技術】 峰，在半導體製造工程或液晶製造工程令，係使用 靜電吸盤以吸著錢定半導體基板或玻璃基板。對於靜電 吸盤而言，有利用庫儉力而吸著基板纟、與利用 J〇h_-Rahbek力而吸著基板者。庫倫力係發生在載置於 靜電吸盤之介電體層表面之基板與靜電吸盤之電極之間的 靜電吸著力。I了得則於吸著基板之靜電力，對於靜電 吸盤而言則要求高體積電阻。例如，對於利用庫倫力之靜 電吸盤而言係使用體積電阻率高之材料，而對於基板之材 料而言係使用鋁。 但是’-般IS燒結體之熱傳導率係低至謂/mK上下， 無法充分地滿^非常高純度且高熱傳導率（熱傳導率係 綱Μ左右、甚至單結晶且卿/mK左右）等例如是靜電吸 盤所要求的熱傳導性。 因此’以作為滿足熱傳導性且具有高體積電阻之材料 而言，有人於基板之材料使用氮化銘（例如，參考特許文 1)〇 口 【特許文獻1】特開2002 —220282號公報 7066-7551-PF;Forever769 5 1303857 【發明内容】 但疋’最近在半導體製造裝置中所使用之氮化紹燒結 體也有日益暴露於高溫環境的傾向。例如，在蝕刻製程或 尚密度電漿CVD製程中，基板溫度範圍一直變廣，隨之而 來的是業界對在高溫環境中也能維持高體積電阻率之材料 的殷殷期盼。 而且，在利用庫倫力之靜電吸盤中，由於為了產生庫 ❿倫力所以基板被施以高電壓，因此業界亟需一種在高電壓 環境中也能維持高體積電阻率的材料。 特別下功夫的話，通常氮化鋁燒結體在室溫、施加電 壓500V/niin中之體積電阻率係大於lxl〇1% · cm，具有高 體積電阻。但是，例如在溫度區域2〇(rc之使用環境下， 恐有所謂施加電壓為2kV/mm、體積電阻率為1χ1〇14Ω · cm 以下時，高溫高壓環境下之體積電阻率降低的問題。如此 一來，例如在使用氮化鋁燒結體作為靜電吸盤之際，即使 籲在停止施加電壓之後也會因為靜電吸盤表面有電荷殘留且 基板無法迅速脫離，而恐有對脫著應答性造成很大的影響 之虞。 ^曰 因此，本發明之目的係提供高溫高壓環境下高體積電 阻率之氮化鋁燒結體、半導體製造用構件、及氮化鋁燒結 體之製造方法。 本發明之氮化鋁燒結體之特徵係以氮化鋁成 含有0.4〜2.5wt%之鎂”。〜…… 成刀並 、 蛛"、么u〜5· Owt%之釔，且平均粒徑 為1. 0微米以下。 7066-7551-PF;Forever769 6 .1303857 根據上述氮化域結體的話，可以在高溫高㈣境下 得到高體積電阻率之氮化鋁燒結體。另外，因為在鎂單獨 之狀態、或至少&含鎂與氧氣之狀態τ，固溶於氮化銘粒 内及包核之粒界相存在的緣故，而可以在高溫高麼環境 下得到高體積電阻率之氮化鋁燒結體。 氮化鋁燒結體的晶格常數（袼子定數）之a軸長為 3.1125X1G-1。以上較佳。如此—來，可以進一步提升體積電 阻率。
3微米以上較佳。如此 步得到高體積電阻率之 氮化紹燒結體的平均粒徑為〇 一來’在高溫高壓環境下可以進一 氮化鋁燒結體。 2kV/mm cm以上 氮化鋁燒結體在真空、2〇fTC中，施加電壓為 時且電壓施加1分鐘後之體積電阻率為1χΐ〇15Ω . 較佳。 另外，氮化鋁燒結體的熱傳導率為30W/mK以上較佳。 如此一來，因為熱傳導率為30w/mK以上，可以得到具有大 於一般氮化鋁燒結體之熱傳導率的氮化鋁燒結體。^ 本發明之氮化减結體係可以適於作為^圓之處理 裝置或液晶顯示器製造裝置等半導體製造裝置内的各種構 件，且本發明之半導體製造用構件之特徵在於：至少一部 分是由以氮化鋁為主成分並含有0 4〜2 5wt%之鎂盥2 〇 〜之釔且平均粒徑為1〇微米以下之本發明的氮 化鋁燒結體所構成。根據上述半導體製造用構件的話，在 高溫高壓環境下可以提供具有高體積電阻率之特性的氮化 7Q66-7551-PF;Forever7 69 7 -1303857 鋁燒結體作為半導體製造用構件。 、 本發月之氮化鋁燒結體若平均粒徑為1 · 〇微米 以下則非常地容易得到微粒之平坦面，可以適用於例如作 為構件之要求平坦性的型材等。 2且，本發明之氮化鋁燒結體為高溫高壓環境下可以
維持高體積雷胆^座夕# W W电P羊之材枓，可以非常地適甩於作為絕緣碍 子等之構件。 • 本發明之氮化鋁燒結體的製造方法，其特徵在於：含 有將包含氮化銘原料、以氧化鎮換算之0.5〜3 0Inol%的 鏔、以氧化紀換算之0.5〜的記成形，並於175〇 °C下燒成的工程。根據上述製造方法的話，在高溫高壓環 境下可以提供高體積電阻率之氮化鋁燒結體。 氮化鋁原料粉末之平均一次粒徑為〇 5微米以下較 佳。如此一來，即使在如175(rc之低溫下也可以燒結，結 果可以將氮化銘燒結體之平均粒徑形成在h Q微米以下… •如此一來，可以進一步提升體積電阻率。 氮化銘原料之比表面積為7mVg以上較佳。如此一來， 因為比表面積為7mvg以上所以燒結性提升，結果即使在 如1750 C之低溫下也可以燒結，並可以將氮化銘燒結體之 平均粒徑形成在U微米以下。如此—來，可以進一步提 升體積電阻率。 根據本月了以&供尚溫高壓環境下高體積電阻率 之氮化鋁燒結體、半導體製造用構件、及氮化鋁燒結體之 製造方法。 8 7066-7551-PF;Forever769 1303857 【實施方式】 〔氮化铭燒結體〕 本實施例之氮化鋁燒結體係以氮化鋁為主成分並含有 〇· 4〜2· 之鎮與2_ 0〜5. 0wt%之釔，且平均粒徑為L 〇 微米以下。一旦氮化鋁燒結體内所含之鎂未滿〇4wt%時， 體積電阻率會下降。另一方面，一旦氣化銘燒結體内所含 φ之鎂超過2. 5wt%時，在高溫高壓環境下無法得到高體積電 阻率之氮化鋁燒結體。另外，一旦氮化鋁燒結體内所含之 鎂超過2. 5wt%時，熱傳導率會大幅地降低，氮化鋁之高熱 傳導率之特徵會喪失。另外，m銘燒結體内所含之 銥未滿2.0wt%時，在例如175(rc以下之低溫下的燒成中， 燒結會變得不完全，而無法得到十分緻密之燒結體。另一 方面，一旦氮化鋁燒結體内所含之銀超過5. 〇wt%時，體積 電阻率會下降。一旦氮化鋁燒結體之平均粒徑超過1·〇微 鲁米時，體積電阻率會下降。 因此，氮化鋁燒結體因為包含適量的鎂與銥（也就是上 述範圍内之鎂與銥）而且平均粒徑為丨.〇微米以下，所以在 高溫高壓環境下可以得到高體積電阻率之氮化銘燒結體。 具體而言’因為在鎂單獨之狀態、或至少包含鎂與氧氣之 狀態下，固溶於氮化鋁粒内及包含釔之粒界相存在的緣 故，而可以在高溫高壓環境下得到高體積電阻率之氮化鋁 燒結體。 另外，在氮化鋁燒結體中，由於含有選自由週期表 7066-7551-PF;Forever769 9 1303857 IVA、VA、VIA、VIIA、VIIIA族所組成之群組中至少一種 以上之過渡金屬元素的緣故，所以容易使氮化鋁燒結體黑 色化。如此一來，可以提升氮化鋁燒结體之輻射效率。以 過渡金屬元素而言，以Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、 W、Mn、Fe、Co、Ni較佳，尤其是Ti、Mo、W更佳。但是， 氮化銘燒結體之原料粉末中過渡金屬元素成 分之總量以氧 化物換算的話’小於〇· 3mol %者較佳。如此一來，一旦氮 _化銘燒結體之原料粉末中過渡金屬元素成分之總量超過 〇· 3ιηο1%時，雖然可以充分地黑色化，但是有可能會招致例 如電阻低之氨化物大量生成、且氮化鋁燒結體之體積電阻 率降低等問題。 另外，以提升氮化鋁燒結體之體積電阻率為優先之情 況下’氮化銘燒結體内所含之鎂的量以介於〇. 5〜2. 5wt% 之間者較佳，另外，以提升熱傳導率為優先之情況下，氮 化铭燒結體内所含之鎂的量以介於〇.4〜15wt%之間者較 •佳。 氮化紹燒結體的晶格常數之a轴長為31125χ1(Γ〗。以 上較佳。如此一來，可以進一步提升體積電阻率。 氮化銘燒結體的平均粒徑為0· 3微米以上較佳。如此 一來，在高溫高壓環境下可以進一步得到高體積電阻率之 氮化铭燒結體β 氮化鋁燒結體在真空、200。〇中，施加電逐為v/mm 時且電壓施加1分鐘後之體積電阻率（JIS C2141)為1χ1 〇15 Ω · Cm以上較佳。尤其是，在真空、200°C中，施加電壓 7066-7551-PF;Forever769 10 1303857 為4kV/mm時且電壓施加」分鐘後之體積電阻率（JISC2141) 為1x1 〇15Ω · cm以上更佳。如此一來，由於可以施加高電 壓’所以在作為例如是靜電吸盤的情況下，可以得到充分 的吸著力。其原因在於吸著力（庫侖力）係隨著施加電壓而 成比例增大。 氮化紹燒結體之熱傳導率（Jis R1611)為30W/IDK以上 較佳。如此一來’可以得到具有大於一般氮化鋁燒結體之 修熱傳導率的氮化紹燒結體。尤其是，氮化鋁燒結體之熱傳 導率為50W/mK以上較佳。 另外’氮化铭燒結體之開氣孔率為〇 · 1 %以下較佳、為 0.05%以下更佳。如此一來，可以進一步提升氮化鋁燒結體 之體積電阻率。 上述氮化紹燒結體係可以藉由含有將包含氮化鋁原 料、以氧化鎂換算之〇· 5〜3· 〇m〇l%的鎂、以氧化釔換算 之0. 5〜1· 5mol%的記成形，並於以下燒成的工程 •而製造。 具體而言，藉由秤量氧化鎂、氧化銥（依上述範圍計算 鎂與銥的量）並將各粉末混於作為主成分之氮化鋁粉末 中’而製作原料粉末。或著，對於氮化鋁之原料粉末，作 為氧化鎂及氧化銥前驅體而言，利用藉由加熱硝酸鎮、硫 酸鎂、草酸鎂、硝酸銥、硫酸銥、草酸銥等而生成氧化鎂 及氧化銥之化合物也可以。氧化鎮及氧化銥前驅體於粉末 狀態下添加也可以。另外，將硝酸鎂、硫酸鎂、硝酸銥、 硫酸銥等化合物溶解於溶劑而成之溶液添加至原料粉末也 7066-7551-PF;Forever769 11 1303857 可以。 之而且’混合以濕式或乾式任一種皆可;若是使用濕式 、月况，則混合後進行乾燥而得原料粉末。例如，混合係 二異丙醇作為溶媒並使㈣（PQt)及玉石，進行4小時之滋 式處合。混合後取出衆體，並於氮氣環财於u(rc下乾 b而且’於4抓下將乾燥粉末於大氣環境中進行熱處 =5小時’並將在濕式混合中混人之碳成分燒失除去，而 製作原料粉末。 在原料粉末中可以添加例如是包含以氮化銘燒結體之 :色化為目的之過渡金屬的氧化物等。但是，氮化銘燒結 體之原料粉末中過渡金屬的總量以氧化物換算㈣，以小 於0· 3mol%者較佳。 另外’氮緣原料粉末之平均—次粒徑為u微米〇 下較佳。如此-來，因為氮化銘燒結體之平均粒徑變為^ 微米以下，所以可以進一舟蔣4 M 、· ，徒升體積電阻率。尤其是，雖 ^氮化㈣料粉末之平均粒徑無下限，但是例如可以形成 -〇. 1微米W上。原因在於，如果氮化㈣料粉末之平均 -次粒徑未滿U微米的話，不只與空氣中之水分或氧氣 之反應性變得非常高、原料粉末中之氧氣量大幅地變化、 組成之控制變得困難’連體積電阻率也有可能降低。而且， 有可能產生嵩比重降低、成形性降低等問題。 另外，氮化链原料粉末之比表面積》7m2/g以上較佳、 如此-來’因為將氮化域結體之平均粒徑形成在丨0微 米以下，可以進一步提升體積電阻率。尤其是，雖然氮化 7066-7551^PF;Forever769 12 1303857 鋁原料粉末之比表面積無上限，但是例如可以小於3加2^ 以下。具有超越30m2/g之比表面積的氮化鋁原料粉末不只8 與空氣中之水分或氧氣之反應性變得非常高、原料粉末中 ;之氧氣量大幅地變化、組成之控制變得困難，連體積電阻 率也有可能降低。而且，有可能產生嵩比重降低、成形性 降低專間題。 而且，以提升氮化紹燒結體之體積電阻率為優先之情 _況下，原料粉末内所含之鎂的量若以氧化鎂換算的話，則 以介於0· 8〜3· Omol%之間者較佳。另外，以提升熱傳導率 為優先之情況下，原料粉末内所含之鎂的量若以氧化鎮換 算的話，則以介於〇· 5〜1. 5mol%之間者較佳。 較佳者係藉由模具壓製（press)法將製作之原料粉末 成形，而製作成形體。例如，以20MPa之壓製壓力，將原 料粉末進行一軸加壓成形，而製作圓盤形狀成形體。 而且，由製成之原料粉末製作漿體，並造粒而製作成 _形體也沒關係。具體而言，於製成之原料粉末内添加架橋 劑（binder)、水，、分散劑等並混合，而製作漿體。藉由喷 霧造粒法等將漿體造粒，而製作造粒顆粒。使用此造粒顆 粒’並藉由 CIP(Cold Isostatic Pressing)法、slip cast 法等成形方法，而製作成形體。 製成之成形體係於惰性氣體中、於1750°C以下之溫度 的環境下燒成者較佳。一旦燒成溫度超過1750°C時，氮化 鋁燒結體之粒徑變大、體積電阻率降低。更好的燒成溫度 係介於1600〜1700°C之間，可以將所得之氮化鋁燒結體之 13 7066-7551-PF；Forever769 1303857 體積電阻率進一步提升。在燒結時之最高溫度的保持時間 係可以達到30分鐘以上；更好的保持時間係可以介於丨小 時〜4小時之間，可以將所得之氮化鋁燒結體之體積電阻率 進一步提升。以惰性氣體環境而言，可以使用氮氣環境或 氬氣環境等。 燒成方法雖不限定，但以使用熱壓法（h〇tpress)者較 佳。如此一來，可以作成緻密的氮化鋁燒結體，可以將所 得之氮化鋁燒結體之體積電阻率進一步提升。藉由熱壓法 而得之緻密的氮化鋁燒結體之開氣孔率係以〇· 1%以下者 較佳、G.G5%以下者更佳。例如，在壓著（press)壓力為 20MPa下，通常m兄而將環境由室溫升至⑽代或 1500 C以形成真空，並將介於1〇〇〇t：或15〇吖至最高溫度 下、。.15MPa之氮氣導入所製成之成形體。藉由在最高溫 度（16〇〇°C〜1750。〇下保持2〜4小時而燒成。 如此一來，#由將包含氨化紹、以氧化鎂換算之〇 5 〜3· Oinol%的鎂、以氧拖管夕 / 6換#之〇· 5〜1· 5mol%的釔成 形，並於1750°C下燒成，*二、w >矿 成在南 咼壓環境下可以得到高 積電阻率之氮化紹燒砝駟 麂作體。接著，在上述製造條件之範圍 内，調整原料粉末之平灼抑你'^ ® 士 十$粒徑'組成、燒成溫度、或燒成 時間、燒成方法等燒成铬杜 ^ _ 、牛，可以適宜調整氮化銘燒结體 之組成或開氣孔率、嵩密_ 工Μ』 70 ”體 宜项替所π夕备 許在度、平均粒徑等。結果，可以適 Γ上播 ①、，、"體之熱傳導率、體積電阻率等： 〔半導體製造用構件〕 寺 本實施例之氮化鋁燒社 夂〜體係可以適用於在高電壓環境 7066-7551-PF;Forever769 14 1303857 中要求南體積電阻之各式各樣的半導體製造用構件。例 如’至少一部分是藉由以氮化鋁為主成分並含有〇· 4〜 2· 5wt%之鎂與2_ 〇〜5· 〇wt%之釔且平均粒徑為i 〇微米以 下之本發明的氮化鋁燒結體而形成，且可以作為埋設有金 屬構件的半導體製造用構件。根據上述半導體製造用構件 的話’在高溫高壓環境下可以提供具有高體積電阻率之特 性的氮化紹燒結體作為半導體製造用構件。 φ 例如’至少一部分是藉由以氮化鋁為主成分並含有〇· 4 〜2· 5wt%之鎮與2· 〇〜5· Owt%之釔且平均粒徑為1· 〇微米 以下之本發明的氮化鋁燒結體而形成，且可以藉由埋設金 屬構件作為靜電電極，而得到靜電吸盤作為半導體製造用 構件。 例如，至少一部分是藉由以氮化鋁為主成分並含有〇· 4 〜2· 5wt%之鎂與2· 0〜5· Owt%之釔且平均粒徑為1· 〇微米 以下之本發明的氮化鋁燒結體而形成，且可以藉由埋設金 鲁屬構件作為電阻發熱體，而得到加熱器作為半導體製造用 構件。 例如，至少一部分是藉由以氮化銘為主成分並含有〇4 〜2· 5wt%之鎂與2. 0〜5. Owt%之釔且平均粒徑為1· 〇微米 以下之本發明的氮化鋁燒結體而形成，且可以藉由埋設金 屬構件作為RF電極，而得到襯托器（susceptor)作為半導 體製造用構件。 〔其它之實施形態〕 本發明雖藉由上述實施例而記載，但是上述實施例僅 7066-7551-PF;Forever769 15 ‘1303857 是本發明之一部分，並非用以限定本發明。從上述揭示之 内容，該領域之從業人士當可以作各式各樣的替代實施型 態、實施例及運用技術。 例如，本實施例之氮化鋁燒結體若平均粒徑為1〇微 米以下則非常地容易得到微粒之平坦面，可以適用於例如 作為構件之要求平坦性的型材等。 而且，本實施例之氮化鋁燒結體為高溫高壓環境下可 _以維持高體積電阻率之材料，可以非常地適用於作為絕緣 碍子等之構件。 接著，雖然利用實施例將本發明更詳鈿地說明，但是 本發明之範圍並不限於該些相關之本發明的實施例。 〔氮化銘燒結體〕 (實施例1〜12、比較例1〜4) 根據如1所示之組成，秤量氮化鋁粉末、氧化鎂粉末、 與氧化釔粉末等並混合而製作原料粉末。而且，氮化鋁之 _平均粒徑係形成為〇·2微米。具體而言，以異丙醇為溶媒 並使用nylon製的壺（pot)及玉石，進行4小時之濕式混 合。混合後取出榘體，並於氮氣環境中於i丨〇 下乾燥。 而且，於45(TC下將乾燥粉末於大氣環境中進行5小時之 熱處理，並將在濕式混合中混入之碳成分燒失除去，而製 作原料粉末。而且，調和粉末之比率（m〇1% )係顯示忽略雜 質含有量所計算出之氮化鋁、氧化鎂、氧化釔、氧化錄、 氧化鈦粉末之比率。 在壓著壓力20MPa下，藉由模具壓著將原料粉末進行 7066-7551-PF;Forever769 16 1303857 一轴加壓成形，而製成直徑50mm〜100mm、厚度20mm左右 的圓盤狀成形體。將成形體裝入碳製的模仁（mold)中，於 氮氣環境中、以及在表1所示之燒成溫度與保持時間下藉 由熱壓法燒成，而製作氮化鋁燒結體。 加工所得之氮化鋁燒結體並進行下列（1)〜（8)之評 價。（1)分析氮化鋁燒結體内所含之Y、Mg、Ti的量。具體 而& ’係藉由誘導結合電浆（ICP)發光光譜分析而作定量分 _析。（2)分析氮化銘燒結體内所含之氧的量及碳的量。具體 而言，係藉由惰性氣艘融解紅外線吸收法而作定量分析。 (3)使用純水為媒體並藉由Archimedes法而測定開氣孔 率、嵩密度。（4)根據JIS C 2141並於真空環境下、以及 介於室溫〜200°C左右下測定體積電阻率。具體而言，係以 減驗片形狀為直径50ηπιχ0· 5ηπι或50x50x0· 5ηπι、且主電極 徑20nm、輔助（guard)電極内徑30nm、辅助（guard)電極外 徑40nm、施加電極徑40nm之規格，以銀形成各電極。施 鲁加2kV/mm之電壓（視情形而施加4kV/mm)，讀取電壓施加 後1分鐘之電流而算出體積電阻率。（5 )根據j I s R1611並 藉由laser flash法而測定熱傳導率。（6)測定氮化銘粒子 之平均粒徑。具體而言，研磨氮化鋁燒結體並以電子顯微 鏡進行微構造觀察。接著，對所得之SEM照片拉出任意條 線，並求出平均切片長度。由於與線相交之粒子的數目越 多則精度越高，所以線條數係依據粒徑而異，但是大致上 拉出60個左右之粒子與線相交的條數。於平均切片長度加 入根據粒之形狀所決定之係數，而推估平均粒徑。而且， 7066-7551-PF;Forever7 69 17 -1303857 =!定粒子且其係數設為!.5。⑺進行結晶相 : 線回折裝置對氮化鋁燒结體確 】所二結晶相'測定條件如下：CuKa、5㈣、_、2 …。；迴轉對陰極型x線回折裝置「理學電 瞻」」。（8)測定格子定數。具體而言，使用 ^wder_PatternFitting)^，根據藉由 χ 線回折裝置所測定之XRD輪廓而算出格子定數。
首先’於粉碎實施例之燒結體而得之粉末内，以重量 =1:1、之比例混人作為内部標準且格子定數已知之融 粉末’並藉由分光儀（―咖㈣於試料照射除去⑽ 沒線之CuKa線’而測定輪廓(pr〇file)。測定條件如下： 5〇kV、2Θ=3Η2(Γ、3QQmA;迴轉對陰極型χ線回折裝置 「理學電機製「RINT-2000系列」」。 而且，使用同裝置中可以選擇隨附之程式「肝打」， 以進行輪廓擬合(^^^^ — ^^卜“而導出格子定數人以 WPPF得知内部標準之格手定數與氣化鋁之袼子定數的近似 值的話，則可以進行精密計算。 藉由精密計算，執行WPPF並於測定之輪廓（pr〇file) 至擬合（fitting)範圍内指定。之後，在以半自動方式 進行擬合時，移行至以手動方式之擬合。以手動方式之精 密化計算的話，則每次在各參數中將背景強度、波峰強度、 晶格常數、半值幅、波峰之非對稱性參數、低角側之輪廓 強度的衰減率、高角側之輪廓強度的衰減率指定為「固定 或「可動」，並進行精密化計算直至計算之輪廓與測定之 7066-755l-PF；F〇rever769 18 • 1303857 輪廓一致（RwP(標準偏差）=0.1以下）為止。根據上述精密 化計算，得到信賴性高的晶格常數。 而且，關於WPPF的話，下列之論文内有詳細記述。 H. Toraya, “Whole-Powder-Pattern Fitting
Without Reference to a Structural Model : Application to X-ray Powder Diffractometer Data^ ， J. Appl. Cryst. 19， 440-447 (1986)· 加工氮化鋁燒結體所得之（1)〜（8)之評價結果如表1 所示。 7066-7551-PF;Forever769 19 • 1303857
【m 燒結艎特性 結晶相(AIN) 4 I 4 ? 4 «*—4 g Y2〇3 · AI2O3, 3Y2O3 · 5Al2〇3, MgAl2〇J Υ2〇3 · A1e〇3 Y2〇3*Al2〇3, MgAl2〇4 Y2〇3-Al2〇3, MgAl2〇4 ?Υ2〇3·Αΐ2〇3, YiOa-AlzOa 4 1 4 1 4 s 4 CO 4 4 4 CO 4 Y2〇3*Al2〇3, MgAl2〇4 Υ2〇3·Αΐ2〇3, 3Υ2〇3·5Αΐ2〇3 Y2〇3-Al2〇3, MgAl2〇4 \AgkWA 13Ye〇3 5Al2〇3, MgAh〇4 I 4 ΐ CO 4 $ 2Υζ〇3 · Αΐ2〇3, Ϊ2〇3 Αΐ2〇3 c轴長 A s s 4.9794( 4.9816 4.8809 4.9815| |4.98111 |4.9807| |4.9806| |4.9813| |4.981〇| 14.9797 g OO 03 4.9786 i 〇> 0 1 寸· ^3 〇0 CD a軸長 A 3.1125 3.1128| 3.1141 3.1133 3.11331 |3.114l| |3.1128| |3.1134| |3.1135| |3.11351 |3.1127 3.1134 3.1117 3.1131 3.1130 3.1117 AIN 平均粒徑 βΙΆ 卜 Ο CO 0 Ο in 0 〇 in 0 CO 0 〇 1—1 CO 0 CO 0 OO 0 卜 〇 CO V—H CO (Nl r-H Ο S 00 οα CO in 寸 CO 05 寸 CO 5! LO LO cn CO CO CO Oi CO 5 § f-H 抵抗率 cm) 4kV/mm 1.9xl0ls 1.6xlQ15 1 1.2χ1015 1. lxlO15 1.3xl015 | 1. OxlO151 1 i.〇xioI5| | Ι.δχΙΟ151 1 1.7xl0151 1 1.7xl0ls 1.4xl015 1.2xl015 1 1 1 1 200oC 積 (Ω · 2kV/mm | 2. lxlO15 Ι.δχΙΟ1*! 1.4χ1015 l.lxlO15 1.9xl015 1 l.OxlO15 1 1 1. OxlO151 11.δχίο1®! 1 2.8xl0,s 1 1 2.3xl0,51 I 1.8xl015! 1.4xl015 4.3x10,s 9.4xl015 6.4xl015 l.OxlO15 嵩密度 g/cm3 3.34 3.37 I 3.33 3.35 I 3.34 I CO CO CO 13.341 CO CO I 3.34 1 I 3. 30 1 I 3.34 3.34 3.28 CO CO 3.33 3.34 開氣 孔率 % f—^ 〇 o 0 Ο s 0 〇 g 0 o g 0 〇 〇 〇 〇 〇 〇 〇 〇 g 〇 0 1"^ 0 s 0 實施例1 實施例2 實施例3 實施例4 1實施例5 I 1實施例6 I 1實施例71 1實施例8| 實施例9 實施例10 實施例11 實施例12 比較例1 比較例2 比較例3 比較例4 燒結體特性 化學分析值 1 0 含有量 wt% 0.077 CO 0 0 0.076 〇 〇 0.027 LO 0 0 LO 〇 〇 0.076 g 〇 CQ 〇 O’ 0.078 0.077 0.068 0.077 0.071 0.030 0 含有量 wt% CM CO CO CO LO ΙΟ CO C<I IO CO oo CO CO 4.08 CO CO GD LO CO CO CO 09 OO CM CO CO CO OO 呀 CO 0¾ CO CO Ο CO Ti 含有量 wt% 1 1 1 〇〇 CNI 〇 0.28 1 1 1 1 1 1 1 1 1 1 1 Y 含有董 wtX 3.45 3.43 ! 3.40 ί 3.46 3.58 4.89 3.56 3.40 3.46 2.06 3.37 3.46 1 1 3.52 3.50 Mg 含有量 wt% CO CO o CO 2.26 CO ▼-H § CM 2 IO in LO 0 T-H f-H CO 寸 o CM 03 〇 CO —· 1 1 IIS 寸 (M CNI 寸 Osl 寸 S 最高 溫度 °c 1700 Il700 1750 1700 〇 〇 1700 1800 1750 1700 1700 1700 1700 1800 1600 1800 1800 原料粉末 a 1 1 1 in CO 0 CD <M CD 1 1 1 1 1 1 1 1 1. 1 1 Yb2〇3 mol% 1 1 1 1 1 1 1 1 1 1 1 1 1 0 1 1 ll 0.89 00 00 0 £ ο 0· 88 0.87 CO CM H 0· 88 0· 89 0· 88 0. 63 0.89 0.89 1 1 0_ 88 0.80 MgO mol% 〇 o 00 CD 2.93 t- σ> —· 2.93 & OO σ> 〇 〇 1.98 1.98 0.80 1.49 1.99 1.98 1.98 1 AIN粉末| 卜 σ> 卜 oi 卜 cri 10.6 10· 6 ai 卜 σ> 卜 ατ> 卜 CD 卜 ori 卜 ai 卜 α> 卜 σί 卜 σ> 卜 σί 寸 CO 酸素 含有量 wtx CO n CO CQ f-H CO C<l t-H CO CM CO C<l f—^ CO CO CO οα ^—4 oo CQ CO C<l CO CS3 ^4 CO csa eo C<l CO n τ·Η CO C<l CO CO s 0 實施例1 1實施例21 1實施例31 1實施例41 實施例5 實施例6 1實施例7| 實施例8| 實施例9 實施例10 實施例11 實施例12 比較例1 比較例2 比較例3 比較例4 6 9 卜Μα)Ass /丨 TLnLn卜-9 9 0卜 ♦1303857 在1600〜1750°C之範圍内將包含平均粒係〇·2微米且 比表面積係9· 7m2/g或10· 6m2/g之氮化鋁原料粉末、以氧 化鎂換算之0.5〜3· Omol%鎂、與以氧化釔換算之〇5〜 1·5ηιο1%釔的原料粉末燒成而得之第卜12實施例之氮化 鋁燒結體具有高至3· 3g/cm3以上之嵩密度，且成為非常敏 密之氮化銘燒結體。 另外，對於任一個第1〜12實施例之氮化鋁燒結體而 _言，氮化鋁之平均粒徑係〇· 3〜1· 〇微米、2〇〇。〇電壓施加 2kV下之體積電阻率係ixi〇15q · Cln以上。因此，相較於 體積電阻率介於9xl012〜6χι〇"ω · Cm之比較例卜4之氮化 鋁燒結體而言，體積電阻率係增加了。尤其是，第9實施 例為包含氮化鋁、1· 12wt%之鎂、與3.46wt%之釔並於][700 C下、、’呈過2】、時而燒成之氮化鋁燒結體，具體積電阻率增 至 3χ1015Ω · cm 〇
另外，第1實施例為包含氮化鋁、0 56wt%之鎂、^ 3.45wt%>^^ 17〇〇〇Ctm 結體’具有高體積電阻率、高熱料率；其中，體積電户」 率係2x10 Ω cm且熱傳導率係56W/mK。第2圖係表示今 實&"之氮化鋁燒結體進行鏡面研磨且施以熱钱刻斤 得之試料的SEM觀察結果。 第2圖係表示對第7實施例之氮化銘燒結體進行鏡面 研磨且施以熱㈣而得之試料的SEM觀察結果。在第7實 加例中II化銘之平均粒徑為〇·3微米（非常小之微粒）， 具有第卜12實施例中最小之微粒。 7066-7551-PF；F〇rever769 21 1303857 另外，任何一個實施例1〜12之氮化鋁燒結體皆具有優 於鋁之熱傳導專，且熱傳導率大於31W/mK。 相對地’比較例1為不包含釔且在比175(rc高的18〇〇 °C下將氮化紹、與1.19wt%鎂之原料粉末燒成而得之說化 紹燒結體’由於沒有包含紀之粒界相且氮化銘之平均粒押 也在1.0微米以上的緣故’所以體積電阻率變差。 比較例2為不包含釔且在1 600°c下將包含氧化記、氮 春化鋁、與1. 13wt%鎂之原料粉末燒成而得之氮化銘燒結 體，且由於沒有包含釔之粒界相的緣故，所以體積電限率 變得非常地差。 比較例3為在比1750〇局的1800C下將包含氮化銘、 1. llwt%鎂、與3· 52wt%釔之之原料粉末燒成而得之氮化 鋁燒結體，且由於氮化鋁之平均粒徑也在1 · 〇微米以上的 緣故，所以體積電阻率變差。 比較例4為不包含鎂，且在比1750°C高的1800。(：下將 籲包含氮化鋁、與3. 5wt%釔之原料粉末燒成而得之氮化鋁 燒結體。熱傳導率雖然高，但是體積電阻率卻變得非常地 差。 【圖式簡單說明】 第1圖係表示第 1實施例 圖面代用照片。 第2圖係表示第* 7實施例 圖面代用照片。 7066-7551-PF；Forever769 22 之氮化鋁燒結體之微構造的 之氮化鈒燒結體之微構造的 1303857 【主要元件符號說明】 無。
7066-7551-PF;Forever769 23
Claims (1)
- .1303857 ^ 十、申請專利範圍·· 1 ·種氮化鋁燒結體，其特徵在於：以氮化鋁為主成 刀並s有〇·4〜2.5wt%之鎮與2.0〜5.0wt%之名乙，且平均 粒徑為1. 0微米以下。 2_如申請專利範圍第丨項所述之氮化鋁燒結體，其中 晶格常數之a軸長為3· 1125x10,以上。 3·如申請專利範圍第丨或2項所述之氮化鋁燒結體， 泰其中平均粒徑為〇· 3微米以上。 4. 如申請專利範圍第〖或2項所述之氮化鋁燒結體， 其中在真空、20(TC中，施加電壓為2kV/mm時且電壓施加 1分鐘後之體積電阻率為1χ1〇15Ω .⑽以上。 5. 如申請專利範圍第丨或2項所述之氮化鋁燒結體， 其中熱傳導率為30W/mK以上。 6· 一種氮化鋁燒結體之製造方法，其特徵在於：含有 將包含氮化鋁原料、以氧化鎂換算之0·5〜3 0ιη〇ι%的鎂、 •以氧化紀換算之的纪成形，並於i75〇〇c以 下燒成的工程。 7.如申請專利範圍第6項所述之氮化鋁燒結體之製造 方法，其中前述氮化鋁原料之平均一次粒徑為〇 5微米以 下。 8·如申請專利範圍第6或7項所述之氮化鋁燒結體之 製造方法，其中前述氮化鋁原料之比表面積為7mVg以上。 9· 一種半導體製造用構件，其特徵在於：利用申請專 利範圍第1或2項所述之氮化鋁燒結體，至少構成一部分。 7 066—7 551-PF;Forever7 69 24
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| WO2012014873A1 (ja) * | 2010-07-26 | 2012-02-02 | 京セラ株式会社 | 静電チャック |
| TWI450855B (zh) * | 2011-08-04 | 2014-09-01 | 高純度氮化鋁製造方法 | |
| JP6100703B2 (ja) * | 2012-01-26 | 2017-03-22 | 京セラ株式会社 | 静電チャックおよびその製造方法 |
| WO2018221504A1 (ja) * | 2017-05-30 | 2018-12-06 | 京セラ株式会社 | 窒化アルミニウム質焼結体、および半導体保持装置 |
| KR102339550B1 (ko) | 2017-06-30 | 2021-12-17 | 주식회사 미코세라믹스 | 질화 알루미늄 소결체 및 이를 포함하는 반도체 제조 장치용 부재 |
| JP7213710B2 (ja) | 2018-03-23 | 2023-01-27 | 日本碍子株式会社 | 複合焼結体、半導体製造装置部材および複合焼結体の製造方法 |
| KR102461995B1 (ko) * | 2021-09-17 | 2022-11-03 | 주식회사 미코세라믹스 | 저열전도 샤프트를 구비하는 고온용 서셉터 |
| WO2023090862A1 (ko) | 2021-11-19 | 2023-05-25 | 주식회사 케이에스엠컴포넌트 | 반도체 제조 장치용 세라믹 히터 |
| KR102535856B1 (ko) | 2021-11-19 | 2023-05-26 | 주식회사 케이에스엠컴포넌트 | 반도체 제조 장치용 세라믹 히터 |
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| DE3777564D1 (de) | 1986-12-11 | 1992-04-23 | Asahi Chemical Ind | Aluminiumnitridprodukte und verfahren zu ihrer herstellung. |
| CA1322565C (en) * | 1988-09-27 | 1993-09-28 | Milo L. Rohrlach | Vehicle inner panel |
| EP0393524A3 (en) | 1989-04-17 | 1993-02-10 | Kawasaki Steel Corporation | Method of making a sintered body of aluminium nitride |
| JPH02275765A (ja) | 1989-04-17 | 1990-11-09 | Kawasaki Steel Corp | 窒化アルミニウム焼結体の製造方法 |
| JPH06191955A (ja) * | 1992-12-22 | 1994-07-12 | Matsushita Electric Works Ltd | 窒化アルミニウム焼結体の製造方法 |
| JPH06321640A (ja) * | 1993-05-14 | 1994-11-22 | Matsushita Electric Works Ltd | 窒化アルミニウム焼結体の製造方法 |
| JPH1067560A (ja) * | 1996-03-18 | 1998-03-10 | Fuji Electric Co Ltd | 高熱伝導率セラミックスおよびその製造方法 |
| JP3457495B2 (ja) * | 1996-03-29 | 2003-10-20 | 日本碍子株式会社 | 窒化アルミニウム焼結体、金属埋設品、電子機能材料および静電チャック |
| JP3433063B2 (ja) * | 1997-09-29 | 2003-08-04 | 日本碍子株式会社 | 窒化アルミニウム焼結体、電子機能材料および静電チャック |
| JPH11260534A (ja) * | 1998-01-09 | 1999-09-24 | Ngk Insulators Ltd | 加熱装置およびその製造方法 |
| JP4013386B2 (ja) * | 1998-03-02 | 2007-11-28 | 住友電気工業株式会社 | 半導体製造用保持体およびその製造方法 |
| JP4641569B2 (ja) * | 1998-07-24 | 2011-03-02 | 日本碍子株式会社 | 窒化アルミニウム質焼結体、耐蝕性部材、金属埋設および半導体保持装置 |
| JP4312372B2 (ja) * | 2000-12-11 | 2009-08-12 | 日本碍子株式会社 | 静電チャックおよびその製造方法 |
| TWI243158B (en) * | 2000-12-21 | 2005-11-11 | Ngk Insulators Ltd | Aluminum nitride sintered bodies |
| JP2002220282A (ja) * | 2001-01-24 | 2002-08-09 | Tokuyama Corp | 窒化アルミニウム焼結体とその製造方法 |
| JP4493264B2 (ja) * | 2001-11-26 | 2010-06-30 | 日本碍子株式会社 | 窒化アルミニウム質セラミックス、半導体製造用部材および耐蝕性部材 |
| JP2003226580A (ja) * | 2001-11-26 | 2003-08-12 | Ngk Insulators Ltd | 窒化アルミニウム質セラミックスおよび半導体製造用部材 |
| JP4482472B2 (ja) * | 2005-03-24 | 2010-06-16 | 日本碍子株式会社 | 静電チャック及びその製造方法 |
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| US20060217259A1 (en) | 2006-09-28 |
| JP2006273584A (ja) | 2006-10-12 |
| TW200723436A (en) | 2007-06-16 |
| JP4987238B2 (ja) | 2012-07-25 |
| KR100756619B1 (ko) | 2007-09-10 |
| US7422992B2 (en) | 2008-09-09 |
| KR20060103146A (ko) | 2006-09-28 |
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