CN103180267A - 加热装置 - Google Patents
加热装置 Download PDFInfo
- Publication number
- CN103180267A CN103180267A CN201180051175XA CN201180051175A CN103180267A CN 103180267 A CN103180267 A CN 103180267A CN 201180051175X A CN201180051175X A CN 201180051175XA CN 201180051175 A CN201180051175 A CN 201180051175A CN 103180267 A CN103180267 A CN 103180267A
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- CN
- China
- Prior art keywords
- stupalith
- experimental example
- magnesium
- corrosion
- aln
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 72
- 238000005260 corrosion Methods 0.000 claims abstract description 69
- 239000011777 magnesium Substances 0.000 claims abstract description 54
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 51
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 49
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 229910017083 AlN Inorganic materials 0.000 claims description 109
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 93
- 230000003628 erosive effect Effects 0.000 claims description 48
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 43
- 230000007797 corrosion Effects 0.000 claims description 41
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 23
- 239000000395 magnesium oxide Substances 0.000 claims description 23
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 22
- 239000004411 aluminium Substances 0.000 claims description 15
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000006104 solid solution Substances 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims 3
- 239000004065 semiconductor Substances 0.000 abstract description 12
- 230000005855 radiation Effects 0.000 abstract description 5
- 229910010293 ceramic material Inorganic materials 0.000 abstract 2
- 229910016523 CuKa Inorganic materials 0.000 abstract 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 84
- 239000000463 material Substances 0.000 description 55
- 229910052596 spinel Inorganic materials 0.000 description 37
- 239000011029 spinel Substances 0.000 description 37
- 238000002156 mixing Methods 0.000 description 36
- 239000000843 powder Substances 0.000 description 36
- 239000002994 raw material Substances 0.000 description 32
- 238000010304 firing Methods 0.000 description 27
- 238000012360 testing method Methods 0.000 description 22
- 238000000034 method Methods 0.000 description 21
- 239000000919 ceramic Substances 0.000 description 17
- 239000012298 atmosphere Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 14
- 238000005245 sintering Methods 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000000465 moulding Methods 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 10
- 229910052736 halogen Inorganic materials 0.000 description 9
- 150000002367 halogens Chemical class 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
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- 229920001778 nylon Polymers 0.000 description 6
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- 208000037656 Respiratory Sounds Diseases 0.000 description 5
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- 238000010586 diagram Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
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- 239000002002 slurry Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000007531 graphite casting Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
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- 239000012535 impurity Substances 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- 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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- 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
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- 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
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- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B1/00—Details of electric heating devices
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- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
- H05B3/283—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic
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Abstract
本发明涉及一种加热装置(11A),其包括具有加热半导体的加热面(12a)的基座(12A)。基座(12A)包括板状主体部(13)和面向加热面的表面耐腐蚀层(14)。表面耐腐蚀层(14)由以镁、铝、氧以及氮为主成分的陶瓷材料构成,该陶瓷材料以氮氧化铝镁相为主相,且使用CuKα线时的XRD波峰至少出现在2θ=47~50°。
Description
技术领域
本发明涉及一种加热半导体的装置。
背景技术
在半导体制造中使用于干法工艺和等离子体涂层等的半导体制造装置中,作为蚀刻用和清洗用,使用的是反应性高的F、Cl等的卤素系等离子体。因此,安装于这种半导体制造装置的构件要求有高耐腐蚀性,一般使用实施过氧化铝膜处理的铝或哈司特镍合金等的高耐腐蚀金属或陶瓷构件。特别是支撑固定Si晶片的静电卡盘材料和加热器材料,由于必须有高耐腐蚀和低发尘性,使用的是氮化铝、氧化铝、蓝宝石等的高耐腐蚀陶瓷构件。由于这些材料会随着长时间使用而逐渐腐蚀,引起发尘,因此要求有更高耐腐蚀性的材料。为应对这种要求,有人研究了作为材料使用比氧化铝等更耐腐蚀的氧化镁或尖晶石(MgAl2O4)及它们的复合材料(例如专利文献1:专利第3559426号公报)。
并且,已知一种用于加热晶片的陶瓷加热器。在这种陶瓷加热器中,要求加热器的温度均匀性以能够均匀地加热晶片。例如,专利文献2(特开平8-73280)公开了一种将电阻发热体埋设到氮化铝质陶瓷板中,并将氮化铝质的柄接合到板上的陶瓷加热器。在专利文献3(特开2003-288975号公报)中,在带柄的加热器中,通过进一步地使电阻发热体中的金属碳化物的量减少,来减少电阻发热体各处的碳化物量的偏差并使加热面的温度分布变小。
发明内容
通常,半导体制造工艺为了防止晶片的污染,将卤素系气体等腐蚀性强的气体用于装置清洗。并且,为了在晶片上均匀进行地成膜,要求晶片上的温度均匀性。作为在半导体制造装置内保持Si晶片并进一步地进行加温的构件,AlN(氮化铝)制的陶瓷加热器作为既有技术被广泛应用,在使用初期能够显示出了良好的晶片上的温度均匀性。然而,由于由腐蚀性气体进行的清洗,AlN被腐蚀,加热器表面的形状或粗糙度变化,由此,就有了随着使用期间的经过温度分布发生变化,温度均匀性无法保持的问题。
本发明的课题在于,在使用于半导体处理的陶瓷加热装置中,减少在卤素系腐蚀性气体或其等离子体气氛下使用时的粒子,并且在长时期内能够保持良好的温度均匀性。
本发明作为包括具有加热半导体的加热面的基座的加热装置,
基座包括板状主体部与面向加热面的表面耐腐蚀层,表面耐腐蚀层由以镁、铝、氧以及氮为主要成分的陶瓷材料构成,该陶瓷材料以氮氧化铝镁相为主相,且使用CuKα线时的XRD波峰至少出现在2θ=47~50°。
本发明的陶瓷材料以氮氧化铝镁相作为主相,与氮化铝相比,对卤素系气体等的腐蚀性强的气体的耐腐蚀性优良。若由该陶瓷材料形成基座的表面耐腐蚀层,即使在腐蚀环境下长时间使用,也不易产生由腐蚀导致的表面状态的变化,其结果,可以在长时期内观察到良好的晶片上的温度均匀性。
并且,板状主体部可以由与所述陶瓷材料不同的热传导性更高的材质来形成,由此,通过促进基座的平面方向的热传导,能够更进一步提高晶片上温度均匀性。
附图说明
图1是实验例1的XRD解析图表。
图2是实验例1、4的EPMA元素分布图。
图3是实验例7的XRD解析图表。
图4是实验例10的XRD解析图表。
图5是概略地示出参考方式所涉及的加热装置的剖面图。
图6是概略地示出参考方式所涉及的加热装置的外观的主视图。
图7是概略地示出本发明的实施方式所涉及的加热装置11A的剖面图。
图8是概略地示出本发明的实施方式所涉及的加热装置11A的外观的主视图。
图9是概略地示出本发明的实施方式所涉及的加热装置11B的剖面图。
图10是概略地示出本发明的实施方式所涉及的加热装置11C的剖面图。
图11是概略地示出本发明的实施方式所涉及的加热装置11D的剖面图。
图12是示出本发明的实施方式所涉及的加热装置的制造方法的流程图。
具体实施方式
以下,对本发明采用的新的陶瓷材料进行说明,然后对加热装置的构成进行说明。
[陶瓷材料]
本发明者专心研究了通过使氧化镁、氧化铝与氮化铝的混合粉末成型后进行热压烧成而得到的陶瓷材料的耐腐蚀性,发现以在特定位置具有XRD波峰的氮氧化铝镁为主相的陶瓷材料显示出非常高的耐腐蚀性。
即,本发明的陶瓷材料作为以镁、铝、氧及氮为主要成分的陶瓷材料,主相为使用CuKα线时的XRD波峰至少出现在2θ=47~50°的氮氧化铝镁相。
本发明的陶瓷材料的耐腐蚀性与尖晶石相同或高于它。因此,本发明的基座能够长时期抵抗在半导体制造工艺中使用的反应性高的F、Cl等卤素系等离子体,能够降低来自该构件的发尘量。另外,即使在腐蚀气氛下长时间使用,也不易产生由腐蚀导致的表面状态的变化,其结果,在长时期内观察到良好的晶片上的温度均匀性。
本发明的陶瓷材料,是以镁、铝、氧及氮为主要成分的陶瓷材料,主相为使用CuKα线时的XRD波峰至少出现在2θ=47~50°的氮氧化铝镁相。该氮氧化铝镁对卤素系等离子体的耐腐蚀性与尖晶石相同或更高,因此可认为以该氮氧化物为主相的本发明的陶瓷材料的耐腐蚀性也变高。此外,该氮氧化铝镁也可以具有与尖晶石相同的耐腐蚀性并且线热膨胀系数低于尖晶石。
本发明的陶瓷材料,作为副相可以含有在氧化镁中固溶了氮化铝的MgO-AlN固溶体的结晶相。由于该MgO-AlN固溶体的耐腐蚀性也较高,因此作为副相也没有问题。该MgO-AlN固溶体的使用CuKα线时的(200)面及(220)面的XRD波峰出现在氧化镁的立方晶波峰与氮化铝的立方晶波峰之间的2θ=42.9~44.8°、62.3~65.2°,此外,(111)面的XRD波峰也可出现在氧化镁的立方晶波峰与氮化铝的立方晶波峰之间的2θ=36.9~39°。由于(111)面的波峰有时难以与其他结晶相的波峰区别,因此也可以是仅(200)面及(220)面的XRD波峰出现在上述范围。同样地,(200)面或(220)面的波峰有时也难以与其他结晶相的波峰区别。
本发明的陶瓷材料为了得到与尖晶石相同或更高的耐腐蚀性,由于当包含AlN结晶相作为副相时,耐腐蚀性有降低的倾向,因而,优选AlN结晶相为少量,更加优选不包含有它。并且,尖晶石由于耐腐蚀性比氧化铝或AlN结晶高,因而,也可含有少量。但,尖晶石由于耐腐蚀性比本发明的氮氧化铝镁相以及MgO-AlN固溶体差,因而,优选其为较少量。另一方面,为了具有与尖晶石相同的耐腐蚀性并且使线热膨胀系数降低,也可以含有少量尖晶石或AlN结晶相。
本发明的陶瓷材料,为了得到与尖晶石相同或更高的耐腐蚀性,原料粉末中的镁/铝的摩尔比优选在0.20以上2以下,镁/铝的摩尔比更加优选在0.75以上2以下。当镁/铝的摩尔比不足0.20,氮化铝、尖晶石、氧化铝中某个或某些的生成量变多,恐怕会丧失高耐腐蚀的特征。镁/铝的摩尔比超过2的话,MgO-AlN固溶体容易成为主相。另一方面,为了保持与尖晶石相同的耐腐蚀性并且降低线热膨胀系数,优选原料粉末中的镁/铝的摩尔比在0.05以上1.5以下,更加优选镁/铝的摩尔比在0.1以上1以下。
本发明的陶瓷材料中,开口孔隙率优选在5%以下。此处,开口孔隙率是根据以纯水为媒质的阿基米德法测定的值。开口孔隙率超过5%的话,可能出现强度下降或材料自身脱粒而容易发尘,而且在材料加工时等容易出现气孔内发尘成分堆积,因此不优选。此外,开口孔隙率优选尽可能接近零。因此,不存在特别的下限值。
本发明的陶瓷材料中,构成主相的氮氧化铝镁的40~1000℃的线热膨胀系数为6~7ppm/K。因此,通过改变副相成分的MgO-AlN固溶体(12~4ppm/K)、尖晶石(8~9ppm/K)和氮化铝(5~6ppm/K)的比率,可在维持高耐腐蚀性的同时将线热膨胀系数控制在5.5~10ppm/K。但是,由于尖晶石和氮化铝较氮氧化铝镁和MgO-AlN固溶体的耐腐蚀性低,优选为较少。通过这种热膨胀的调整,可与氧化铝、氧化钇及氮化铝等用于半导体制造装置构件的材料的热膨胀配合,或减小热膨胀差。通过这样,可使本发明的陶瓷材料与传统材料的层叠和贴合成为可能。这样的话,可以仅将表面(第1构造体)作为本发明的具有高耐腐蚀性的陶瓷材料,下部(第2构造体)基材可使用传统材料。特别是在一体烧成中这种层叠结构及热膨胀调整是有效的。其中,通过第2构造体的基材使用以氮化铝为主体的材料,可维持高热传导,容易保持均匀的高耐腐蚀的陶瓷材料的表面温度。这种结构特别在加热器内置型半导体制造装置中是有效的。
本发明的陶瓷材料既可以作为用于具有采用上述陶瓷材料的第1构造体和以氮化铝、氧化钇以及氧化铝中至少1种为主相的第2构造体的层叠体中的材料。并且,也可以作为具有将该第1构造体与第2构造体层叠或接合后的构造的材料。这样做的话,通过耐腐蚀性高的第1构造体、具有与第1构造体不同的特性(例如传热性或机械的强度等)的第2构造体,能够更加提高除耐腐蚀性之外的其它特性。此外,第1构造体也可以作为由上述陶瓷材料形成的薄膜或板状体、层状体。并且,第2构造体也可以作为以氮化铝、氧化钇以及氧化铝为主相的薄膜或板状体、层状体。另外,接合可以以任何形态来进行,例如可以通过烧结进行接合,也可以通过粘合剂进行接合。
此时,第1构造体与第2构造体可以通过中间层接合。这样做的话,通过中间层,例如能够更加抑制由热膨胀率的不同导致的第1构造体与第2构造体的剥离等。该中间层可以作为具有第1构造体与第2构造体的中间的性质的层。该中间层也可以作为例如混合第1构造体的主相与第2构造体的主相的层。并且,该中间层也可以包含含有的成分或者成分比不同的多层。这样做的话,能够具有倾斜材料的特性。
并且,第1构造体与第2构造体之间的线热膨胀系数差在0.3ppm/K以下,第1构造体与第2构造体也可以直接接合。这样做的话,由于第1构造体与第2构造体的线热膨胀系数差小,因而高温接合两构造体(例如通过烧结进行接合)时或重复在高温-低温下使用该层叠体时不会产生裂纹或剥离。
[陶瓷材料的制造]
本发明的陶瓷材料,可将氧化镁、氧化铝和氮化铝的混合粉末在成型后烧成而制造。例如,为得到与尖晶石相同或更高的耐腐蚀性,可将混合了15质量%以上66.2质量%以下的氧化镁、63质量%以下的氧化铝、57.7质量%以下的氮化铝的粉末成型后烧成。进一步地,也可将混合了37质量%以上66.2质量%以下的氧化镁、63质量%以下的氧化铝、57.7质量%以下的氮化铝的粉末成型后烧成。另一方面,为了保持与尖晶石相同的耐腐蚀性并且降低线热膨胀系数、提高温度均匀性,也可将混合了5质量%以上60质量%以下的氧化镁、60质量%以下的氧化铝、90质量%以下的氮化铝的粉末成型后烧成。此外,烧成温度优选在1750℃以上。烧成温度不足1750℃的话,可能无法得到目标的氮氧化铝镁,因此不优选。此外,烧成温度的上限并无特别限定,但例如可以为1850℃或1900℃。此外,烧成优选采用热压烧成,热压烧成时的加压压力优选设定为50~300kgf/cm2。烧成时的气氛优选不会影响氧化物原料烧成的气氛,优选例如氮气气氛、氩气气氛、氦气气氛等惰性气氛。成型时的压力没有特别限制,适当设定为可以保持形状的压力即可。
[加热装置]
在优选的实施方式中,本发明的加热装置包括有具有加热半导体的加热面的基座以及接合到该基座的背面的支撑部。第5图~第8图概略地示例了这样的加热装置。第5图、第6图的加热装置1为参考例,第7图、第8图的加热装置11A为实施例。
基座2、12A为板状,基座2、12A的上表面2a、12a为半导体加热面。半导体加热面2a、12a不需要为平坦,可进行凹凸加工或形成与基板的大小相配合的沟槽,也可以形成吹扫气体用的沟槽。将支撑部3接合到基座的下表面(背面)2b、12b。本例中支撑部为管状,支撑部3中收容有供电构件5。供电构件连接到埋设在基座内的发热体4上。
基座为盘状,优选为大致圆盘状。基座的大小没有特别地限定,例如直径为280~380mm,厚度为8~20mm。并且,基座与支撑部的接合部分的外径没有特别地限定,直径为例如60~120mm。支撑部优选在中部具有阶差,以阶差为边界在基座侧为大直径部3a,在对侧为小直径部3c。在大直径部3a的端部以及小直径部3c的端部,分别形成法兰3b、3d(但第5图的例中没有法兰3b)。然后,将支撑部的大直径部的端部接合到基座的背面,使基座与中心轴变成同轴。
在这里,发热体优选被埋设到基座内,也可以安装到基座上。并且,发热体也可以是设在从基座偏离的位置上的红外线加热元件那样的外部发热体。
此处,在第5图、第6图的参考例中,整个基座2由均质的材质构成。与此相对,第7图、第8图的实施例中,基座12A包括板状主体部13、覆盖板状主体部13的表面13a的表面耐腐蚀层14。本例中,板状主体部13的侧面13c、背面13b没有被耐腐蚀层覆盖。本发明中,表面耐腐蚀层14通过所述陶瓷材料形成。发热体4埋设在板状主体部13内。
并且,在第9图所示的加热装置11B中,基座12B包括板状主体部13、覆盖板状主体部13的表面13a的表面耐腐蚀层14。本例中,板状主体部13的侧面13c、背面13b没有被耐腐蚀层覆盖。本发明中,表面耐腐蚀层14由所述陶瓷材料形成。与此同时,在表面耐腐蚀层14与板状主体部13的表面13a之间设有中间层17。由此,即使在反复进行加热与冷却时,在维持表面耐腐蚀层从板状主体部的剥离强度方面也很理想。
并且,在第10图所示的加热装置11C中,基座12C包括板状主体部13、覆盖板状主体部13的表面13a的表面耐腐蚀层14、以及覆盖板状主体部13的侧面13c的侧面耐腐蚀层15。本例中,板状主体部13的背面13b没有被耐腐蚀层覆盖。本发明中,表面耐腐蚀层14以及侧面耐腐蚀层15由所述陶瓷材料形成。当基座侧面被腐蚀,不仅是粒子的原因,通过来自侧面的热辐射特性变化来对晶片上温度均匀性也产生不良影响。在本实施方式中,不仅晶片侧,还能够抑制侧面上的腐蚀。另外,在表面耐腐蚀层14与板状主体部13的表面13a之间,能够设置如上所述的中间层17。并且,在侧面耐腐蚀层15与板状主体部13的侧面13c之间,也能够设置如上所述的中间层17。
并且,在第11图所示的加热装置11D中,基座12D包括板状主体部13、覆盖板状主体部13的表面13a的表面耐腐蚀层14、以及覆盖板状主体部13的背面13b的背面覆盖层16。本例中,板状主体部13的侧面13c没有被耐腐蚀层覆盖。本发明中,表面耐腐蚀层14以及背面覆盖层16由所述陶瓷材料形成。另外,在表面耐腐蚀层14与板状主体部13的表面13a之间,能够设置如上所述的中间层17。并且,在背面覆盖层16与板状主体部13的背面13b之间,也能够设置如上所述的中间层17。
作为板状主体部的材质,在使用热传导率比所述陶瓷材料高的材料的情况下,通过整个板状主体部的热传导来提高晶片上温度均匀性。然而,在这种情况下,由于来自板状主体部13的背面13b侧的散热量也变大,因而,通过不均等的热辐射,晶片上温度均匀性有可能反而劣化。在本实施方式中,由于在板状主体部的背面侧设有由所述陶瓷材料构成背面覆盖层,因而,不仅可谋求背面侧的耐腐蚀,能够整体地抑制来自基座背面侧的热辐射,更进一步改善晶片上温度均匀性。
本发明虽然通过上述陶瓷材料来形成基座,但支撑部3(即所谓的柄)的材质不一定要限定,可以示出以下的例子:
本出願的陶瓷材料、氮化铝、氧化铝、氧化镁、尖晶石
优选的是支撑部3的材质也用上述陶瓷材料。但在该的情况下,形成基座的上述陶瓷材料与形成支撑部的上述陶瓷材料不需要为相同组成,也可以是在上述的范围内相互不同的组成。
发热体可使用例如使线状的导体弯曲,加工成缠绕体的物体。发热体的线径为0.3mm~0.5mm左右,在线圈形状的情况下卷径为2mm~4mm左右,间距为1mm~7mm左右。在这里“卷径”意思是构成发热体的线圈的内径。
作为发热体的形状,除线圈形状之外,可以采用带状、网格状、螺旋弹簧状、板状、印刷电极等的各种形态。另外,理想的是在与为提升销等的或吹扫气体用而设置的贯通孔相邻的部分使发热体12绕行等,根据需要进行式样的变形。作为发热体12的材料,可优选采用钼(Mo)、钨(W)、铌(Nb)等的高熔点导电材料。
在加热装置的基座内,也可以埋设用于在基座上使等离子体产生的高频电极。作为高频电极的材质,可以转用上述的发热体材料。
[板状主体部以及中间层的材质]
在所述陶瓷材料中,作为主相的氮氧化铝镁的40~1000℃的热膨胀系数为6~7ppm/K。因而,通过改变作为副相成分的MgO-AlN固溶体(12~14ppm/K)或,尖晶石(8~9ppm/K),氮化铝(5~6ppm/K)的比率,维持高耐腐蚀性的同时,能够将线热膨胀系数控制在5.5~10ppm/K。但是,由于尖晶石或氮化铝的耐腐蚀性比氮氧化铝镁或MgO-AlN固溶体低,优选尖晶石或氮化铝更少。通过这样的热膨胀的调整,能够减小氧化铝、氧化钇以及氮化铝等与用作半导体制造装置构件的材料的热膨胀差。由此,本发明的陶瓷材料与已有材料的层叠或贴合成为可能。
具体地说,板状主体部的材质可示例氧化铝、氧化钇、氮化铝、氧化镁、氮化硅、尖晶石,特别优选氧化铝、氧化钇、氮化铝。
特别,通过以氮化铝为主相的材质来形成板状主体部,由此,能够维持高热传导,易于均匀地保持高耐腐蚀的所述陶瓷材料的表面温度。
板状主体部与各耐腐蚀层、背面覆盖层的接合方法没有特别限定。两者既可以例如通过一体烧结进行接合,也可以通过粘合剂进行接合。
作为这样的粘合剂,能够示例硅系粘合剂、丙烯系粘合剂、Al合金粘合剂。
在优选的实施方式中,耐腐蚀层、背面覆盖层与板状主体部的线热膨胀系数差在0.3ppm/K以下。在这种情况下,在高温接合耐腐蚀层、背面覆盖层与板状主体部(例如通过一体烧结进行接合)时或重复在高温-低温下使用该层叠体时,不会产生裂纹或剥离。
如上所述,板状主体部与各耐腐蚀层、背面覆盖层可以通过中间层来接合。这样做的话,能够更进一步抑制例如由热膨胀率的不同导致的耐腐蚀层、背面覆盖层的剥离。该中间层是具有耐腐蚀层、背面覆盖层与板状主体部的中间的性质的层。
具体地说,中间层可以是烧结所述陶瓷材料与板状主体部的材料的混合物后的复合陶瓷。
并且,能够多层形成中间层,通过使各中间层的组成互不相同,能够形成倾斜材料层。
[卤素系腐蚀性气体]
本发明的基座对卤素系腐蚀性气体及其等离子体的耐腐蚀性优良,特别地,对以下的卤素系腐蚀性气体或其混合物或它们的等离子体的耐腐蚀性特别优良。
NF3、CF4、ClF3、Cl2、BCl3、HBr
实施例
[陶瓷材料的制造与评价]
以下对本发明适当的适用例进行说明。MgO原料、Al2O3原料及AlN原料使用纯度99.9质量%以上、平均粒径1μm以下的市售品。此处,对于AlN原料,由于不可避免地含有1质量%左右的氧,因此是将氧从杂质元素中除开后的纯度。此外,即使使用了纯度99质量%以上的MgO原料的情况下,也可制作与使用纯度99.9质量%以上的MgO原料时同等的陶瓷材料。
1.陶瓷材料
首先,说明以镁、铝、氧及氮为主要成分的陶瓷材料(实验例1~19)。此外,实验例1~3、6~16相当于本发明的实施例,实验例4、5、17~19相当于比较例。
[实验例1~3]
·调合
称量MgO原料、Al2O3原料及AlN原料使其满足表1所示质量%,以异丙醇为溶剂,采用尼龙制的罐、直径5mm的氧化铝圆球进行4小时湿式混合。混合后取出浆料,在氮气流中进行110℃干燥。然后,通过30目的筛,制成调合粉末。此外,该调合粉末的Mg/Al的摩尔比为1.2。
·成型
将调合粉末以200kgf/cm2的压力进行单轴加压成型,制作直径35mm、厚度10mm左右的圆盘状成型体,收容到烧成用石墨铸模。
·烧成
将圆盘状成型体热压烧成而得到陶瓷材料。热压烧成中,加压压力为200kgf/cm2,以表1所示烧成温度(最高温度)烧成,直到烧成结束前都控制为Ar气氛。烧成温度下的保持时间为4小时。
[实验例4]
除了按表1所示质量%称量MgO原料及Al2O3原料以外,与实验例1同样地得到陶瓷材料。
[实验例5]
除了烧成温度设定为1650℃以外,与实验例1同样地得到陶瓷材料。
[实验例6~12]
除了按表1所示质量%称量MgO原料、Al2O3原料及AlN原料、且烧成温度设定为表1所示温度以外,与实验例1同样地得到陶瓷材料。
[实验例13~19]
除了按表1所示质量%称量MgO原料、Al2O3原料及AlN原料、烧成温度设定为表1所示温度、且烧成气氛为N2以外,与实验例1同样地得到陶瓷材料。
[评价]
将实验例1~19得到的各材料加工为各种评价用,进行以下评价。各评价结果如表1所示。另外,实验例1~19中,也制作了直径50mm的试样,但得到的评价结果与表1相同。
(1)体积密度·开口孔隙率
根据以纯水为媒质的阿基米德法测定。
(2)结晶相评价
用研钵将材料粉碎,通过X射线衍射装置确定结晶相。测定条件为CuKα、40kV、40mA、2θ=5-70°,使用密封管式X射线衍射装置(ブルカー·エイエツクスエス制D8ADVANCE)。
(3)蚀刻率
对各材料的表面进行镜面研磨,使用ICP等离子体耐腐蚀试验装置进行下述条件的耐腐蚀试验。将通过阶差仪测定的遮蔽面与暴露面的阶差除以试验时间,计算各材料的蚀刻率。
ICP:800W、偏置功率:450W、导入气体:NF3/O2/Ar=75/35/100sccm0.05Torr(6.67Pa)、暴露时间:10h、试料温度:室温
(4)构成元素
使用EPMA检测并识别构成元素,分析各构成元素的浓度。
(5)平均线热膨胀系数(40~1000℃)
使用膨胀计(ブルカー·エイエックスエス制造)于氩气气氛中测定。
(6)弯曲强度
根据JIS-R1601,通过弯曲强度试验测定。
(7)体积电阻率测定
根据JIS-C2141的方法,在大气中、室温(25℃)下测定。试验片形状为直径50mm×(0.5~1mm)、主电极为直径20mm、保护电极为内径30mm、外径40mm、外加电极为直径40mm,各电极由银形成。外加电压为2kV/mm,读取电压外加后1分钟时的电流值,根据该电流值计算室温体积电阻率。此外,对于实验例7和实验例19(MgO烧结体),在真空下(0.01Pa以下)、600℃下测定。试验片形状为直径50mm×(0.5~1mm)、主电极为直径20mm、保护电极为内径30mm、外径40mm、外加电极为直径40mm,各电极由银形成。外加电压为500V/mm,读取电压外加后1小时的电流值,根据该电流值计算体积电阻率。此外,表1的体积电阻率中,“aEb”表示a×10b,例如“1E16”表示1×1016。
[评价结果]
图1显示了实验例1的XRD解析图表。此外,实验例2、3的XRD解析图表与实验例1大致相同,因此省略图示。此外,实验例1~19检测出的结晶相汇总如表1所示。如图1所示,实验例1~3的陶瓷材料的XRD解析图表,由无法确定的多个波峰(图1中的□)与氧化镁中固溶了氮化铝的MgO-AlN固溶体的波峰(图1中的○)构成。无法确定的波峰(□)与氧化镁、尖晶石、氮化铝任意一个均不相符地在2θ=47~49°(47~50°)有波峰,推测为氮氧化铝镁。此外,这些氮氧化铝镁的波峰,与例如参考文献1(J.Am.Ceram.Soc.,93[2]322-325(2010))或参考文献2(日本专利特开2008-115065)所示的MgAlON(或氮氧化铝镁)的波峰不一致。一般,已知这些MgAlON是尖晶石中固溶了N成分的物质,可认为具有与本发明的氮氧化铝镁具有不同的晶体结构。
MgO-AlN固溶体的(111)面、(200)面及(220)面的XRD波峰出现在氧化镁的立方晶波峰与氮化铝的立方晶波峰之间的2θ=36.9~39°,42.9~44.8°,62.3~65.2°。图2显示了实验例1的EPMA元素分布图。根据图2,确认了实验例1由图1所示的氮氧化铝镁(x部)与MgO-AlN固溶体(y部)2相构成,可知前者为主相。此处,主相指的是体积比例中占50%以上的成分,副相指的是主相以外的XRD波峰确定的相。考虑到截面观察中的面积比反映出了体积比例,因此主相为在EPMA元素分布图中占50%以上面积的区域,副相为主相以外的区域。根据图2可知,氮氧化铝镁的面积比为约66%,氮氧化铝镁为主相。此外,x部特定为氮氧化铝镁的根据是,由Mg、Al、O、N这4个成分构成,与实验例4的尖晶石材料(z部)相比,Mg、N浓度高,Al浓度为相同程度,O浓度低。即,该氮氧化铝镁具有较尖晶石含有更多Mg的特征。对于其他实验例也进行同样的解析,例如实验例10的氮氧化铝镁的面积比为约87%,可知氮氧化铝镁为主相。此外,此处是作为一个例子,主相与副相的判定通过EPMA元素分布进行,但只要是可以识别各相的体积比例的方法,则可采用其他方法。
另外,EPMA元素分布图,根据浓度,颜色分为红、橙、黄、黄绿、绿、青、蓝,红为最高浓度、蓝为最低浓度、黑表示零。但是,由于图2为黑白显示,因此以下说明图2本来的颜色。实验例1中,Mg的x部为黄绿、y部为红,Al的x部为橙、y部为青,N的x部为橙、y部为青,O的x部为淡蓝、y部为橙。实验例4中,Mg整体(z部)为绿,Al整体为橙,N整体为黑,O整体为红。
并且,实验例4中,由于没有使用氮化铝,因此没有生成上述氮氧化铝镁,其陶瓷材料作为主相含有尖晶石(MgAl2O4)。实验例5中,由于烧成温度低,因此没有生成上述氮氧化铝镁,其陶瓷材料作为主相含有氧化镁,作为副相含有尖晶石和氮化铝。图3显示了实验例7的XRD解析图表,图4显示了实验例10的XRD解析图表。根据图3、4可知,实验例7、10均主要检测出了在2θ=47~49°(或47~50°)有波峰的氮氧化铝镁(图中的□),实验例7的副相为尖晶石(图中△),实验例10的副相为MgO-AlN固溶体(图中的○)。此外,对于实验例6、8、9、11、12,省略XRD解析图表的图示,主相和副相如表1所示。
然后,实验例1~3、6~8的陶瓷材料的蚀刻率为实验例4的80%以下、实验例9~12的蚀刻率为实验例4的90%以下,是较低的值,耐腐蚀性非常高。由于实验例5含有较多的耐腐蚀性低的尖晶石和氮化铝,因此蚀刻率变高。此外,实验例18所示的氧化铝的蚀刻率值比实验例4的陶瓷材料(尖晶石)更高。此外,实验例1~3、6~8的陶瓷材料的弯曲强度和体积电阻率值也非常高。
并且,也测定高温下的蚀刻率。在这里,对于实验例2及实验例10的陶瓷材料,对各材料的表面进行镜面研磨,使用ICP等离子体耐腐蚀试验装置进行下述条件的高温耐腐蚀试验。此外,通过阶差仪测定的遮蔽面与暴露面之间的阶差除以试验时间,计算各材料的蚀刻率。其结果是,各材料的蚀刻率在氧化铝的1/3倍以下、氮化铝的1/5倍以下,与尖晶石为相同水平,高温下的等离子体耐腐蚀性也良好。
ICP:800W、偏置功率:无、导入气体:NF3/Ar=300/300sccm0.1Torr、暴露时间:5h、试料温度:650℃
实验例12~16的陶瓷材料,蚀刻率与实验例4的尖晶石大致同等(212~270nm/h),线热膨胀系数低于尖晶石(5.8~6.9ppm/K)。即,实验例12~16的陶瓷材料,可以说具有与尖晶石相同的耐腐蚀性并且线热膨胀系数低,可用作静电卡盘材料和加热材料,特别是加热材料。此外,实验例17,虽然原料组成与实验例6相同,但由于烧成温度低,因此主相不是氮氧化铝镁而是尖晶石,因此较实验例6耐腐蚀性低,同时线热膨胀系数变高。此外,实验例12~16的陶瓷材料,弯曲强度和体积电阻率值也足够高。
并且,实验例7与实验例19的600℃下的体积电阻率分别为5×108Ωcm、2×1012Ωcm,主相为XRD波峰至少出现在2θ=47~49°(或47~50°)的氮氧化铝镁相的陶瓷材料,电阻低于MgO。
由以上可预测,实验例1~3、6~16制作的陶瓷材料也具有低于氧化镁的电阻。
【表1】
2.层叠烧结
接着说明将使用了上述陶瓷材料的第1构造体与第2构造体层叠烧结的层叠体(实验例20~26)。另外,实验例20~24相当于本发明的实施例,实验例25、26相当于比较例。
[实验例20、21]
实验例4、6~12的陶瓷材料,40~1000℃的平均线热膨胀系数为7~9ppm/K。实验例20、21,如表2所示,以实验例10的陶瓷材料为第1构造体的同时,以氮化铝为第2构造体,将第1及第2构造体层叠、成型为直径50mm的试料,进行层叠烧结。该氮化铝中,作为烧结助剂另外添加5质量%的氧化钇(即对于AlN100质量份添加5质量份Y2O3的比例,称为AlN[1]),或添加50质量%的氧化钇(即对于AlN100质量份添加50质量份Y2O3的比例,称为AlN[2])。氮化铝、氧化钇原料分别使用纯度99.9质量%以上、平均粒径1μm以下的市售品。此处,对于AlN原料,由于不可避免地含有1质量%左右的氧,因此是将氧从杂质元素中除开的纯度。此外,40~1000℃的平均线热膨胀系数,AlN[1]为5.7ppm/K、AlN[2]为6.2ppm/K,因此第1构造体与第2构造体之间产生热膨胀差。因此,在第1构造体与第2构造体之间设置了混合了AlN[1]或AlN[2]和实验例10的原料的中间层。通过该中间层,可以缓和热膨胀差。在使用了AlN[1]的实验例20中,中间层为按质量比25∶75、50∶50、75∶25混合的3层,在使用了AlN[2]的实验例21中,中间层为按质量比40∶60、60∶40混合的2层。以下详细说明调合、成型、烧成各工序。
·调合
第1构造体的原料使用与上述实验例10同样方法制作的调合粉末。第2构造体的原料以氮化铝为主相,如下调合。第2构造体的AlN[1]中,首先,以100质量%、5.0质量%的比例称量氮化铝粉末、氧化钇粉末,以异丙醇为溶剂,使用尼龙制的罐、尼龙制圆球进行4小时湿式混合。混合后取出浆料,在氮气流中进行110℃干燥。然后,过30目的筛,制成调合粉末。再将得到的调合粉末在大气气氛中进行450℃、5小时以上的热处理,烧失除去湿式混合中混入的碳成分。使用了AlN[1]的层叠体的中间层如下调合。首先,按质量比75∶25(中间层1)、50∶50(中间层2)、25∶75(中间层3)的比例称量实验例10的调合粉末和上述氮化铝的调合粉末,以异丙醇为溶剂,用尼龙制的罐、尼龙制圆球进行4小时湿式混合。混合后取出浆料,在氮气流中进行110℃干燥。然后过30目的筛,制成调合粉末。第2构造体的AlN[2],除了按100质量%、50质量%的比例称量氮化铝粉末、氧化钇粉末以外,按照与AlN[1]同样的方法调合。此外,使用了AlN[2]的层叠体的中间层,除了按质量比60∶40(中间层1)、40∶60(中间层2)的比例称量实验例10的调合粉末与上述氮化铝的调合粉末以外,按照与AlN[1]同样的方法调合。
·成型
首先将第2构造体的原料即氮化铝调合粉末填充至直径50mm的金属模具内,以200kgf/cm2的压力单轴加压成型。不脱模氮化铝成型体,填充中间层的调合粉末,使其上部的氮化铝较多,以200kgf/cm2的压力在每次填充时进行单轴加压成型。最后填充第1构造体的原料——实验例10的调合粉末,以200kgf/cm2加压成型。对于使用了AlN[1]的层叠体,制为第2构造体的氮化铝层为10mm、中间层为各1mm×3层、第1构造体的实验例10的层为10mm构成的合计23mm的圆盘状成型体。此外,对于使用了AlN[2]的层叠体,制为第2构造体的氮化铝层为10mm、中间层为各1mm×2层、第1构造体的实验例10的层为10mm构成的合计22mm的圆盘状成型体,将这些层叠的圆盘状成型体收容到烧成用石墨铸模中。
·烧成
通过将收容到烧成用石墨铸模的圆盘状成型体热压烧成,得到一体烧成的陶瓷材料。热压烧成中,加压压力为200kgf/cm2,以烧成温度1800℃烧成,直到烧成结束前都控制为Ar气氛。烧成温度下的保持时间为4小时。此外,对实验例20、21还实施了在烧成温度1750℃下的烧成(实验例20-1、21-1)。
上述制造方法得到的烧结体,使用了AlN[1]的层叠体(实验例20、20-1)、使用了AlN[2]的层叠体(实验例21、21-1)均由上部以高耐腐蚀的氮氧化铝镁为主、烧结体的下部以高热传导的氮化铝为主的烧结体构成,中间配置有中间层。中间层随着从第1构造体向第2构造体接近而AlN含有量增高倾斜。这些烧结体中,各层间没有裂纹、裂缝等。可认为这是由于第1构造体与第2构造体之间有中间层,因而回避了烧成中的热应力。此外,通过控制氮化铝基材的热膨胀率,减小了基材与氮氧化铝镁间产生的热应力,可令中间层较薄。可推测,这样的烧结体,适合用于例如静电卡盘或基座、加热器、板、内壁材料、监视窗、微波导入窗、微波耦合用天线等半导体制造装置用构件
[实验例22~24]
实验例22中,如表2所示,除了以实验例6的陶瓷材料为第1构造体、以氧化铝为第2构造体、无中间层、在N2气氛下层叠烧结以外,与实验例20同样地得到层叠体。实验例23,如表2所示,除了以实验例6的陶瓷材料为第1构造体、以氧化钇为第2构造体、无中间层、在N2气氛下层叠烧结以外,与实验例20同样地得到层叠体。实验例24,如表2所示,除了以实验例13的陶瓷材料为第1构造体、以氮化铝(AlN[1])为第2构造体、无中间层、在N2气氛下层叠烧结以外,与实验例20同样地得到层叠体。实验例22~24均没有发现层间有裂纹和裂缝等。此外,实验例22~24中,由于第1构造体与第2构造体之间的线热膨胀系数差较小,均在0.3ppm/K以下,因此无中间层也可防止产生裂纹和裂缝等。可推测,这些的层叠体也与实验例20,21一样,适合用于静电卡盘或基座、加热器、板、内壁材料、监视窗、微波导入窗、微波耦合用天线等的半导体制造装置用构件。此外,实验例22~24也可像实验例20、20-1、21、21-1那样设置中间层。
[实验例25、26]
实验例25,如表2所示,除了以氧化铝为第1构造体、氮化铝(AlN[1])为第2构造体、在N2气氛下层叠烧结以外,与实验例20同样地得到层叠体。实验例26,如表2所示,除了以尖晶石为第1构造体、氮化铝(AlN[1])为第2构造体、在N2气氛下层叠烧结以外,与实验例20同样地得到层叠体。实验例25、26均在层间产生了裂纹。可认为这是由于第1构造体与第2构造体之间的线热膨胀系数差过大,因此虽然设置了中间层,却无法完全防止热膨胀差造成裂纹。
【表2】
[加热装置的制造与评价]
参照第7图~第8图、第12图,对本发明所涉及的陶瓷加热器的制造方法进行说明(实验No.3~6)。
(一)首先,进行基座(板)的材料调整(S101)。对于表面耐腐蚀层14的材料,具体地说,称量MgO原料、Al2O3原料以及AlN原料,以异丙醇为溶剂,采用尼龙制的罐、直径5mm的氧化铝圆球进行4小时湿式混合。作为混合方法,采用例如被称为滚筒筛的容器自身进行旋转的大型球磨机装置来进行。取出混合后浆体,在氮气流中在110℃下干燥。其后通过有30目的筛,制成调合粉末。另外,该调合粉末的Mg/Al的摩尔比为1.2。
另一方面,对于板状主体部13的材料,将氮化铝陶瓷粉末与成型用粘接剂混合。由滚筒筛进行的混合的时间为例如30分左右。其后,通过喷雾干燥器(SD)等的制粒装置,进行制粒,得到制粒粉。
(二)然后,通过机械加压机,将表面耐腐蚀层用的调合粉末在单轴加压下成型,进而添加板状主体部用的制粒粉,同样地通过机械加压机在单轴加压下成型,制造预备的成型体(S102)。然后,在该预备的成型体内部放置发热体4以及电流导入端子部6,再次通过机械压力机进行成型。
(三)将如上所述地制作的层叠成型体投入到热压方式等的烧成炉中,进行烧成(S103)。由于热压是在碳夹具内充填或插入原料粉末或成型体,在30~50MPa的单轴加压下进行烧成,因而适合于在通常的常压烧结下难以致密化的陶瓷材料的烧成。此时的烧成条件为烧成温度1600℃~2000℃,压力100~300kg/cm2,烧成时间2~5小时。
(四)另一方面,支撑部(即所谓的柄)部分需要另外制造基座。首先,进行柄的材料调整(S104)。具体地说,与上述板状主体部的材料调整(S101)一样地得到调合粉末。将得到的调合粉末投入到冷等静压加压(冷静水压加压:Cold IsostaticPressing,CIP)等的烧成炉中,进行烧成,制造成型体(S105)。CIP是对由模具成型法而得到的单轴成型体实施等静压的成型处理的方法,能够提高成型体密度并消除密度不均。不进行模具成型,直接充填橡胶型的原料粉末并进行CIP处理也能够得到成型体。通过常压烧成炉等对这样得到的柄的成型体进行烧成(S106)。此时的烧成条件是烧成温度1600℃~2000℃,压力1~30kg/cm2,烧成时间1~5小时。然后,进行柄的外周或包装的加工(S107)。
(五)由上述的次序得到的基座与柄通过直接结合法在烧成炉内接合(S108)。此时的烧成条件为烧成温度1400℃~2000℃,压力100~300kg/cm2,烧成时间2~5小时。接合后的陶瓷加热器实施侧面加工,通过接合炉进行端子的接合。其后,进行清洗处理或温度均匀性的评价等。
另外,在表3的实验No.3,4,5,6中形成表面耐腐蚀层的材质为所述实施例(表1)中的实验例10的材质。
(比较例1的加热装置)
作为比较例1(实验No.1),由包含有5重量%氧化钇的氮化铝粉末(纯度99.5%)来形成并接合基座2以及支撑部3,制造加热装置。
(比较例2的加热装置)
作为比较例2(实验No.2),通过在表3的实验No.3,4,5,6中形成表面耐腐蚀层的材质,来形成基座。该材质为所述实施例(表1)中的实施例12的材质。支撑部3由包含有5重量%氧化钇的氮化铝粉末(纯度99.5%)来形成。
[试验条件]
·耐腐蚀试验:ICP:800W、偏置功率:450W、导入气体:NF3/O2/Ar=75/35/100sccm、0.05Torr、暴露时间:100hrs.、试料温度:600℃
·评价特性:上述的耐腐蚀试验前后的晶片上的温度均匀性、粒子量、表面粗糙度
·温度均匀性测定
将各例的加热装置设置在真空箱内,在加热装置上设置温度测定用的黑体晶片,加热到550℃,从室外部由红外线辐射温度计(IR摄像机)来测定各温度下的黑体晶片表面的温度分布。由得到的温度分布来计算温度的最大值与最小值的差△T。另外,加热器的往各温度的加热是通过安装在陶瓷板的背面的未图示的热电偶的温度控制来进行的。
.粒子量
将各例的陶瓷加热器设置在真空箱内,在陶瓷加热器上设置Si晶片,加热到550℃。采用粒子计数器来测定加热后的Si晶片的陶瓷加热器设置面侧表面的粒子量。另外,加热器的往各温度的加热是通过安装在陶瓷板的背面的未图示的热电偶的温度控制来进行的。
·表面粗糙度
通过泰勒·霍普森光学粗糙度测定器来测定基座的表面(半导体设置面)的粗糙度。测定地点为表面内的内侧与外侧的任意两处。
【表3】
在实验No.1中,耐腐蚀试验前的晶片上温度均匀性良好,但由于耐腐蚀试验后粒子增加,表面粗糙度劣化,因而晶片上温度均匀性劣化。在实验No.2中,从耐腐蚀试验后晶片上温度均匀性也没有劣化这一点看来温度均匀性极好。在实验No.3~6中,耐腐蚀试验后晶片上温度均匀性不仅没有劣化,耐腐蚀试验前的初期的晶片上温度均匀性也比实验No.2优秀。
这些作用效果在半导体处理装置领域中有划时代意义的,显然可以期待在产业上的巨大应用。
虽然对本发明的特定的实施方式进行了说明,但本发明不限定于这些特定的实施方式,在不脱离权利要求范围内,能够进行并实施各种变更或改变。
Claims (13)
1.一种加热装置,其包括具有加热半导体的加热面的基座,所述加热装置的特征在于,
所述基座包括板状主体部与面向所述加热面的表面耐腐蚀层,所述表面耐腐蚀层由以镁、铝、氧以及氮为主成分的陶瓷材料构成,该陶瓷材料以氮氧化铝镁相为主相,且使用CuKα线时的XRD波峰至少出现在2θ=47~50°。
2.根据权利要求1所述的加热装置,其特征在于,
所述基座包括覆盖所述板状主体部的背面的背面覆盖层,该背面覆盖层由以镁、铝、氧以及氮为主成分的陶瓷材料构成,该陶瓷材料以氮氧化铝镁相为主相,且使用CuKα线时的XRD波峰至少出现在2θ=47~50°。
3.根据权利要求1或2所述的加热装置,其特征在于,
所述基座包括覆盖所述板状主体部的侧面的侧面耐腐蚀层,该侧面耐腐蚀层由以镁、铝、氧以及氮为主成分的陶瓷材料构成,该陶瓷材料以氮氧化铝镁相为主相,且使用CuKα线时的XRD波峰至少出现在2θ=47~50°。
4.根据权利要求1~3任一项所述的加热装置,其特征在于,包括:
中间层,其设在所述表面耐腐蚀层、所述背面覆盖层以及所述侧面耐腐蚀层中至少一个与所述板状主体部之间。
5.根据权利要求1~4任一项所述的加热装置,其特征在于,包括:
接合到所述基座的背面的支撑部。
6.根据权利要求5所述的加热装置,其特征在于,
所述支撑部由所述陶瓷材料构成。
7.根据权利要求5或6所述的加热装置,其特征在于,包括:
发热体,其埋设在所述板状主体部的内部;以及电力供给构件,其容纳在所述支撑部的内侧空间,与所述发热体电连接。
8.根据权利要求1~7任一项所述的加热装置,其特征在于,
所述2θ为47~49°。
9.根据权利要求1~7任一项所述的加热装置,其特征在于,
所述陶瓷材料以氧化镁中固溶了氮化铝的MgO-AlN固溶体的结晶相为副相。
10.根据权利要求9所述的加热装置,其特征在于,
所述MgO-AlN固溶体的使用CuKα线时的(200)面及(220)面的XRD波峰出现在氧化镁的立方晶波峰与氮化铝的立方晶波峰之间的2θ=42.9~44.8°、62.3~65.2°。
11.根据权利要求10所述的加热装置,其特征在于,
所述MgO-AlN固溶体的使用CuKα线时的(111)面的XRD波峰出现在氧化镁的立方晶波峰与氮化铝的立方晶波峰之间的2θ=36.9~39°。
12.根据权利要求1到11任一项所述的加热装置,其特征在于,
所述陶瓷材料不包含AlN结晶相。
13.根据权利要求1到12任一项所述的加热装置,其特征在于,
所述板状主体部由以氮化铝、氧化钇或氧化铝为主相的陶瓷构成。
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