WO2006057404A1 - ヒータユニット - Google Patents
ヒータユニット Download PDFInfo
- Publication number
- WO2006057404A1 WO2006057404A1 PCT/JP2005/021880 JP2005021880W WO2006057404A1 WO 2006057404 A1 WO2006057404 A1 WO 2006057404A1 JP 2005021880 W JP2005021880 W JP 2005021880W WO 2006057404 A1 WO2006057404 A1 WO 2006057404A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- carbide
- heater
- carbon
- temperature
- sintered
- Prior art date
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 60
- 229910052799 carbon Inorganic materials 0.000 description 59
- 239000000843 powder Substances 0.000 description 40
- 238000005245 sintering Methods 0.000 description 37
- 238000000034 method Methods 0.000 description 32
- 239000011368 organic material Substances 0.000 description 24
- 239000012535 impurity Substances 0.000 description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 239000005011 phenolic resin Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- -1 hexamine Chemical compound 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000007849 furan resin Substances 0.000 description 3
- 238000005304 joining Methods 0.000 description 3
- 239000011344 liquid material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000009529 body temperature measurement Methods 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 239000011269 tar Substances 0.000 description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- ZZHNUBIHHLQNHX-UHFFFAOYSA-N butoxysilane Chemical compound CCCCO[SiH3] ZZHNUBIHHLQNHX-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 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
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluenecarboxylic acid Natural products CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- ZMYXZXUHYAGGKG-UHFFFAOYSA-N propoxysilane Chemical compound CCCO[SiH3] ZMYXZXUHYAGGKG-UHFFFAOYSA-N 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67098—Apparatus for thermal treatment
- H01L21/67103—Apparatus for thermal treatment mainly by conduction
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/148—Silicon, e.g. silicon carbide, magnesium silicide, heating transistors or diodes
Definitions
- the present invention relates to a heater unit including a heater composed of a material cover containing carbon carbide.
- metal heaters such as nichrome generate metal at a rapid temperature rise and have an adverse effect on the object to be heated.
- ceramic heaters such as aluminum nitride and boron nitride were not able to heat at a high temperature of 100 ° C or higher or rapidly. Carbon heaters were too powerful to be used in air.
- Patent Document 1 Japanese Patent Laid-Open No. 2003-308951
- the present invention relates to the following items:
- An electrode for raising the temperature of the heater by energization a heater made of a material containing silicon carbide connected to the electrode, a wafer holder for holding a heated object, the heater, and the wafer holder.
- a heater unit comprising: a chamber that surrounds at least an inner surface provided with a reflective layer.
- FIG. 1 (a) is a side cross-sectional view of a heater unit according to an embodiment
- FIG. 1 (b) is a perspective view of the heater unit that works on the embodiment.
- FIGS. 2 (a) to 2 (c) are process diagrams of a joining method of the heater 1 and the electrode 2.
- FIG. 3 is a graph showing the temperature rise / fall characteristics of the heater unit 20.
- FIG. 4 is a diagram (partially enlarged view of FIG. 3) showing the temperature rise characteristics of the heater unit 20.
- FIG. 5 is a diagram (partially enlarged view of FIG. 3) showing a temperature drop characteristic of the heater unit 20.
- the heater unit 20 which is effective in the embodiment is
- An electrode 2 that raises the temperature of the heater 1 by energization
- a heater 1 that is also configured with material forces including carbon carbide connected to the electrodes;
- the electrode 2 is preferably made of a material cover containing carbon carbide. This is because the thermal conductivity is improved and good temperature rise / fall characteristics can be obtained.
- the heater 1 and the electrode 2 are integrally formed by using a joined body having the same members as those. This is because the heater 1 and the electrode 2 are formed integrally using members having the same thermal conductivity, so that the soaking characteristic of the heater 1 is improved. If the heater 1 and the electrode 2 are joined using a joining member made of a different member, the soaking characteristic of the heater 1 tends to deteriorate.
- the wafer holder 5 is formed using various materials without particular limitation as long as it can hold an object to be heated and has high temperature resistance.
- the wafer holder 5 is made of quartz.
- the wafer holder 5 is a portion that hits the lower side of the heated body when the heated body is placed. Is equipped with a thermocouple.
- the chamber 13 includes a lower chamber 3 a that houses and holds the heater 1 and the wafer holder 5, and an upper chamber 3 b that is disposed to face the lower chamber 3 a when the heater unit 20 is used.
- the inside of the chamber 13 is curved so that the radiant heat is concentrated on the heated object.
- the inner surface of the chamber 13 is provided with a reflective layer 8 having high heat radiation rate and acid resistance.
- the heat radiation rate is preferably 0.01-0.80.
- Examples of the reflective layer 8 include substances having an emissivity of about 0.02, such as gold plating. Further, the reflective layer 8 may be provided by mirror finishing the inside of the chamber 13. Since the reflective layer 8 is provided on the inner surface of the chamber 13, it becomes difficult for heat to be accumulated in the heater unit 20, so that the temperature rise / fall characteristics of the heater unit 20 are improved.
- the heater unit 20 may be connected to a heating control means having a digital control circuit.
- the temperature of the object to be heated is measured at a predetermined cycle using a thermocouple, and if it tends to overheat, the heating is controlled to prevent overheating of the object to be heated.
- the temperature measurement cycle is set to 0.05 seconds or less (1 ° CZ seconds), preferably 0.01 seconds or less.
- the heater 1 and the electrode 2 constituting the heater unit 20 are manufactured according to the hot press method described later. At that time, the heater 1 and the electrode 2 can be engaged with each other (FIG. 2 (a)), and a free play portion is formed at the joint 10 (FIG. 2 (b)) when engaged. Protrusions are formed at one end of the electrode 2 provided with communication holes in the part.
- slurry containing silicon carbide (SiC) and carbon (C) is poured into the joint 10 of the heater 1 and the electrode 2. Thereafter, the joint is partially heated. Subsequently, high-purity silicon (Si) is inserted into the joint, and excess C and Si are reacted to form SiC.
- SiC silicon carbide
- SiC carbon
- the heater 1 and the electrode 2 are integrated as shown in FIG. 2 (c).
- the ceramic heater unit 20 shown in Fig. 1 (a) is manufactured by assembling the structural member 3.
- the above heater and electrode were manufactured by a hot press method. However, the heaters and electrodes described above may be manufactured by other manufacturing methods, such as reaction sintering and improved methods. [0016] (Example)
- the heater unit 20 shown in FIGS. I ( a ) and (b) was used as the heater unit.
- the object to be heated a wafer having a thermal conductivity of 160 wZm'k having a single crystal silicon force was used as the object to be heated. The wafer was heated to 700 ° C, held at the above temperature for about 10 minutes, and then cooled. The temperature measurement cycle of the heated object was 0.01 seconds.
- FIGS. Figure 3 shows the overall temperature rise / fall experiment.
- FIG. 4 is an enlarged view of the temperature rising region in FIG. Fig. 5 is an enlarged view of the temperature drop region in Fig. 3.
- the rate of temperature increase from 70 ° C to 700 ° C was 630 ° C Z min. Also, the rate of temperature decrease from 700 ° C to 200 ° C is about 500 ° CZ.
- a method for manufacturing a carbide used for manufacturing a heater unit will be described.
- a sintered carbon carbide having a free carbon content of 2 to 10% by weight is used.
- Such a sintered carbonized carbide can be obtained by firing a mixture of a sintered carbide powder and a non-metallic sintering aid.
- the carbon carbide powder will be described.
- the carbide powder ⁇ type,
- the grain size of the used carbide powder is small. Preferably, it is about 0.01 to 10 m, more preferably 0.05 to 2 ⁇ m. If the particle size is less than 0.01 ⁇ m, handling in processing steps such as weighing and mixing becomes difficult, and if it exceeds one, the specific surface area of the powder, that is, the contact area with the adjacent powder. Is not preferable because it becomes small and it is difficult to increase the density.
- High purity carbon carbide powder is, for example, a key compound (hereinafter referred to as “key source”).
- key source An organic material that generates carbon by heating, and a z polymerization catalyst or a crosslinking catalyst, and the resulting solid is fired in a non-oxidizing atmosphere.
- liquid and solid compounds can be widely used, but at least one liquid compound is used. Examples of the liquid key source include polymers of alkoxysilanes (mono-, G, tree, tetra).
- tetraalkoxysilane polymers are preferably used. Specific examples include methoxysilane, ethoxysilane, propyloxysilane, butoxysilane, and the like. From the viewpoint of handling, ethoxysilane is preferable.
- the degree of polymerization of the tetraalkoxysilane polymer is about 2 to 15, a liquid low molecular weight polymer (oligomer) is formed.
- oligomer liquid low molecular weight polymer
- a solid key source that can be used in combination with a liquid key source includes carbon carbide. Carbide carbides here include silica sol (colloidal ultrafine silica) in addition to mono-acid silicate (SiO) and diacid silicate (SiO 2).
- a tetraalkoxysilane oligomer having a good homogeneity and a ring ring property, or a mixture of an oligomer of tetraalkoxysilane and fine powder silica is preferable. Further, it is preferable that these key sources have high purity.
- the initial impurity content is preferably 20 ppm or less, more preferably 5 ppm or less.
- an organic material that generates carbon by heating in addition to a liquid material, a liquid material and a solid material may be used in combination.
- An organic material having a high residual carbon ratio and capable of being polymerized or crosslinked by a catalyst or heating is preferable.
- monomers such as phenol resin, furan resin, polyimide, polyurethane, polybulal alcohol, and prepolymers are preferred.
- liquid materials such as cellulose, sucrose, pitch, and tar are also used.
- resole type phenolic resin is preferable in terms of thermal decomposability and purity.
- the purity of the organic material may be appropriately controlled according to the purpose.
- the mixing ratio of the source of the key and the organic material can be determined by intensifying a preferable range based on the molar ratio of carbon to key (hereinafter abbreviated as “CZSi”).
- CZSi molar ratio of carbon to key
- the czsi obtained from the elemental analysis of a carbonized carbon intermediate obtained by carbonizing a mixture of a key source and an organic material at 1000 ° C. As shown in the following reaction formula, carbon reacts with oxide silicon and changes to carbonized carbide.
- CZSi when CZSi is 3.0, the free carbon in the carbonized carbon intermediate is 0%. Actually, SiO gas etc. is volatilized, so CZSi has a lower value. In any case, free carbon is generated. Since free carbon has the effect of suppressing grain growth, C / Si should be determined according to the particle size of the target powder particles, and the key source and the organic material should be blended to achieve the ratio. . For example, when firing a mixture of a key source and an organic material at about 1 atm and 1600 ° C or higher, mixing with CZSi in the range of 2.0 to 2.5 suppresses the generation of free carbon. can do.
- the blending ratio can be appropriately determined according to the purpose.
- the action and effect of free carbon caused by the carbonized carbide powder are very weak compared with the action and effect of free carbon generated from the sintering aid, the free carbon caused by the carbonized carbide powder is The effect of the present invention is not essentially affected.
- the impurity carbon contained in the carbonized carbide powder is preferably about 30 wt% or more and about 40 wt% or less.
- the carbon content of silicon carbide (SiC) is theoretically about 30% by weight, but is reduced from 30% by weight when containing non-carbon impurities and 30% by weight when containing carbon impurities. Increase more.
- the carbon carbide powder obtained by adding and firing an organic material as described above contains carbon-based impurities, so the carbon content is greater than 30% by weight. Therefore, if the carbon content in the carbide powder is less than 30% by weight, the proportion of non-carbon impurities is high, which is not preferable in terms of purity. On the other hand, if it exceeds 40% by weight, the density of the resulting sintered carbide body is lowered, which is not preferable in terms of strength, acid resistance, and the like.
- a mixture of a key source and an organic material can be cured to form a solid.
- Curing methods include a method using a crosslinking reaction by heating, a method using a curing catalyst, and a method using electron beam or radiation.
- the curing catalyst used depends on the organic material used. However, when phenol resin or furan resin is used as the organic material, acids such as toluenesulfonic acid, toluenecarboxylic acid, acetic acid, succinic acid, hydrochloric acid, sulfuric acid, amines such as hexamine, etc. Can be mentioned. Solids containing the key source and organic material are heated and carbonized as needed.
- Carbonization is performed by heating at 800 ° C to 1000 ° C for 30 to 120 minutes in a non-acidic atmosphere such as nitrogen or argon. Further, when heated at 1350 ° C. to 2000 ° C. in a non-oxidizing atmosphere, silicon carbide is generated.
- the firing temperature and firing time affect the particle size and the like of the resulting carbide powder, and may be appropriately determined. However, firing at 1600 to 1900 ° C. is efficient and preferable.
- the method for obtaining the high-purity silicon carbide powder described above is described in detail in the specification of JP-A-9-48605.
- the sintered carbide body used in the present invention has a free carbon content of 2 to 10% by weight. This free carbon originates from the organic material used in the nonmetallic sintering aid, and the amount of free carbon can be reduced by adjusting the loading conditions such as the addition amount of the nonmetallic sintering aid. Can range.
- a non-metallic sintering aid that can be a free carbon source, that is, a material containing an organic material that generates carbon by heating (hereinafter sometimes referred to as "carbon source”) may be used.
- carbon source a material containing an organic material that generates carbon by heating
- the above organic material may be used alone or as a sintering aid with the above organic material coated on the surface of a carbide powder (particle size: about 0.01 to 1 micron). From this point, it is preferable to use an organic material alone.
- organic materials that generate carbon by heating include coal tar pitch, pitch tar, phenol resin, furan resin, epoxy resin, phenoxy resin, saccharides with a high residual carbonization rate, Examples thereof include monosaccharides such as darcos, small saccharides such as sucrose, polysaccharides such as cellulose and starch, and the like.
- the organic material is preferably liquid at room temperature, dissolved in a solvent, or softened by heating such as having thermoplasticity and heat melting properties.
- the use of phenol resin increases the strength of the sintered carbonized carbide, and is more preferably resol type phenol resin.
- the nonmetallic sintering aid may be dissolved in an organic solvent if desired, and the solution and the carbide carbide powder may be mixed.
- the organic solvent to be used varies depending on the non-metallic sintering aid. For example, when phenol resin is used as the sintering aid, lower alcohols such as ethyl alcohol, ethyl ether, acetone, etc. may be selected. it can.
- high-purity silicon carbide sintered bodies not only high-purity silicon carbide powder, but also sintering aids and organic solvents with low impurity content! Favored ,.
- the amount of the nonmetallic sintering aid added to the carbide carbide powder is determined so that the free carbon of the sintered carbide carbide is 2 to 10% by weight. If the free carbon is outside this range, the chemical change to SiC that progresses during the bonding process, and the bonding between the sintered carbide bodies becomes insufficient.
- the free carbon content (% by weight) is determined by heating the sintered carbide carbide body in an oxygen atmosphere at 800 ° C for 8 minutes, and measuring the amount of generated CO and CO with a carbon analyzer.
- the measured force can be calculated.
- the amount of sintering aid added varies depending on the type of sintering aid used and the amount of surface silica (silicon oxide) in the carbide powder.
- the amount of surface silica (silicon oxide) of the carbide powder is quantified using hydrogen fluoride water in advance, and the stoichiometry sufficient to reduce this oxide oxide ( Calculate the stoichiometry calculated by formula (I).
- the amount added can be determined so that the free carbon falls within the above-mentioned suitable range.
- the description of the non-metallic sintering aid for the sintered carbide carbide described above is described in more detail in the specification of Japanese Patent Application No. 9-041048.
- a method for sintering a mixture of a carbide carbide powder and a nonmetallic sintering aid will be described.
- the silicon carbide powder and the nonmetallic sintering aid are mixed homogeneously.
- a solution obtained by dissolving a sintering aid in an organic solvent as described above may be used.
- the mixing method include known methods such as a method using a mixer, a planetary ball mill and the like.
- the equipment used for mixing is preferably a synthetic resin material in order to prevent metal element impurities from being mixed. Mixing is preferably performed for about 10 to 30 hours, particularly for about 16 to 24 hours, and mixed thoroughly. After thorough mixing, the solvent is removed and the mixture is evaporated to dryness. Thereafter, the mixture is sieved to obtain a raw material powder of the mixture. Spice to dry A granulating device such as a rice dryer may be used.
- the raw material powder thus obtained is placed in a molding die.
- the molding die to be used is made of graphite because metal impurities are not mixed in the sintered carbide body.
- the contact part is made of graphite so that the raw material powder and the metal part of the mold are not in direct contact with each other, or a polytetrafluoroethylene sheet (Teflon) is used for the contact part. (Registered trademark) sheet) can be used preferably.
- Teflon polytetrafluoroethylene sheet
- a high-purity graphite material for the mold and the heat insulating material in the furnace.
- a graphite material or the like that is sufficiently baked at a temperature of 2500 ° C. or higher and does not generate impurities even when used at a high temperature can be used.
- the raw material powder placed in the molding die is subjected to hot pressing.
- Wide of Nag 300 ⁇ 700kgfZcm 2 in particular constraints Te pressure Nitsu ⁇ of the hot press it can be carried out by the pressure of the range.
- pressurizing at 400 kgfZcm 2 or more it is necessary to use hot press parts such as dies and punches having excellent pressure resistance.
- Hot pressing is performed at a temperature of 2000 ° C to 2400 ° C. It is preferable that the temperature is raised to the hot pressing temperature gently and stepwise. When the temperature is raised in this way, chemical changes, state changes, and the like that occur at each temperature can be sufficiently advanced, and as a result, the introduction of impurities, cracks, and generation of voids can be prevented.
- An example of the temperature raising process is shown below. First, 5: the molding die was put raw material powder LOg was placed in a furnace, the furnace is evacuated of 10 _ 4 torr. Gently raise the temperature from room temperature to 200 ° C and keep it at 200 ° C for about 30 minutes. Then, heat up to 700 ° C in 6-10 hours and keep at 700 ° C for 2-5 hours.
- the holding time at the constant temperature varies depending on the size of the sintered carbonized carbide, and may be set appropriately.
- the determination of whether or not the force has sufficient holding time can be based on the time point when the degree of vacuum decrease is reduced to some extent.
- the temperature is raised from 700 ° C to 1500 ° C in 6 to 9 hours and held at 1500 ° C for about 1 to 5 hours. While the temperature is maintained at 1500 ° C., the reaction in which the oxide oxide is reduced and converted to carbide is advanced (Equation (1)).
- the holding time is insufficient, silicon dioxide remains and the carbide powder Since it adheres to the surface, it prevents the densification of the particles and causes the growth of large grains.
- the determination of whether the holding time is sufficient is based on whether or not the generation of by-product carbon monoxide and carbon dioxide is stopped, that is, the reduction of the vacuum level is reduced and the reduction reaction start temperature is reached.
- the hot pressing is preferably performed after the inside of the furnace is heated to about 1500 ° C. at which sintering starts, and then filled with an inert gas in order to make the inside of the furnace a non-oxidizing atmosphere.
- an inert gas it is preferable to use argon gas that is non-reactive even at high temperatures, such as nitrogen gas or argon gas. If a high-purity silicon carbide sintered body is produced, use an inert gas with a high purity.
- the temperature forces 2000 o C ⁇ 2400 o C, pressure Caro heat and Caro the furnace so that the pressure force S300 ⁇ 700kgf / cm 2. If the maximum temperature is less than 2000 ° C, the densification is insufficient.
- the maximum temperature exceeds 2400 ° C, it is not preferable because the powder or the raw material of the molded body may sublimate (decompose). It is preferable to raise the temperature from around 1500 ° C to the maximum temperature over 2 to 4 hours and hold at the maximum temperature for 1 to 3 hours. Sintering proceeds rapidly at 1850-1900 ° C and completes during the maximum temperature holding time.
- the pressurization condition is less than 300 kgfZcm 2 , the density increase is insufficient, and if it exceeds 700 kgfZcm 2 , the graphite mold may be damaged, which is not preferable in terms of production efficiency.
- the sintered carbide body used is densified and has a density of 2.9 gZcm 3 or more and a porosity of 1% or less, preferably a density of 3. OgZcm 3 or more, and a porosity of 0.8% or less is particularly preferable.
- a densified carbide body sintered body When a densified carbide body sintered body is used, mechanical properties such as bending strength and fracture strength, and electrical properties of the obtained bonded carbide body are improved.
- the use of a densified silicon carbide sintered body is preferable in terms of contamination because the constituent particles are reduced in size.
- a method for increasing the density of the sintered carbide body there is a method in which a forming step is performed in advance prior to the sintering step.
- This molding process is performed at a lower temperature and lower pressure than the sintering process. Is.
- the bulky powder can be made compact (small volume) in advance, and by repeating this step many times, it becomes easy to produce a large molded body.
- An example of various conditions of the molding process performed in advance prior to the sintering process is shown below.
- the raw material powder obtained by homogeneously mixing the silicon carbide powder and the nonmetallic sintering aid is placed in a molding die, and the temperature is 80 ° C to 300 ° C, preferably 120 ° C to 140 ° C., pressure 50 kgfZcm 2 ⁇ : LOOkgfZcm 2 is pressed for 5 to 60 minutes, preferably 20 to 40 minutes to obtain a molded body.
- the heating temperature may be appropriately determined according to the characteristics of the nonmetallic sintering aid.
- the density of the resulting molded product is 1.8 gZcm 2 or more when using powder with an average particle size of about 1 m, and 1 when using powder with an average particle size of 0.5 m. It is preferable to press at 5 g / cm 2 . If the density of the molded body to be used is within this range, it is preferable because it becomes easy to increase the density of the sintered carbide body. Cut the molded body so that the resulting molded body is compatible with the mold used in the s
- Impurity elements in the sintered carbide body used in the present invention (in the 1989 IUPAC inorganic chemical nomenclature revised version of the periodic table of elements, C, N, 0, Si with an atomic number of 3 or more excluding Si
- the total content of (element) is preferably 5 ppm or less because it can be used in processes requiring high cleanliness, for example, semiconductor manufacturing processes. More preferably, it is 3 ppm or less, and particularly preferably 1 ppm or less.
- the impurity content by chemical analysis has only a meaning as a reference value in actual use.
- the evaluation of the contamination property of the carbon-carbide assembly may differ depending on the force that the impurities are uniformly distributed and whether the impurities are unevenly distributed.
- the materials specifically exemplified above and the exemplified sintering method are used, a sintered carbide body having an impurity content of 1 ppm or less can be obtained.
- the content of impurity elements contained in the raw materials used for example, carbide carbide powder and non-metallic sintering aid
- inactive gas is reduced.
- Examples include a method of removing impurities by adjusting the sintering conditions such as sintering time, temperature, etc. to 1 ppm or less.
- the impurity element here is the same as described above. In the periodic table of the 1989 IUPAC inorganic chemical nomenclature revised edition, atomic number 3 or more (except for C, N, 0, Si) )).
- Other physical property values of the sintered carbide carbide used in the present invention are bending strength at room temperature. 550 to 800 kgfZmm 2 , Young's modulus 3.5 X 10 4 to 4.5 X 10 4 , Pickers hardness 550 to 80 OkgfZmm 2 , Poisson's ratio 0.14 to 0.21, thermal expansion coefficient 3.8 X 10— 6 to 4. 2 X 10 " 6 1 / ° C, thermal conductivity 150WZm'K or more, specific heat 0.15 ⁇ 0.18 & 173 '° ⁇ , thermal shock resistance 500 ⁇ 700 AT ° C, specific resistance 1 It is preferable that ⁇ ′cm because the various characteristics of the obtained carbonized carbide joined body will be good.
- the silicon carbide sintered body described in the specification can be preferably used.
- the surface to be bonded of the sintered carbide body is smooth in terms of adhesion.
- the surface roughness Ra of the surface to be bonded is 0.5 m or less. Is more preferably 0.02 m or less.
- the surface roughness of the sintered carbonized carbide can be adjusted to the above range by grinding or puffing with a turret of 200 to 800 mesh.
- the silicon metal used in the present invention is preferably one having a purity of 98% or more, more preferably a purity of 99% or more, and particularly preferably a purity of 99.9%. If silicon metal with low purity is used, a covalent compound is formed by an impurity element in the carbonized carbide bonded body, and the fire resistance is lowered. In particular, when used in connection with semiconductor processes, such as wafer jigs, it is preferable to use those with a purity of 99.999% or more.
- the silicon metal used is powder, the powder is preferably 100 mesh or more. If the size of the silicon metal is less than 100 mesh, the surfaces to be joined are likely to be displaced, and dimensional accuracy cannot be obtained. The upper limit is not particularly limited, but what is actually available is less than 350 mesh.
- the amount of silicon metal used for bonding affects the bonding strength and the like of the resulting silicon carbide bonded body.
- the bonding strength of the obtained silicon carbide bonded body is improved and the remaining silicon metal remains. It has been found that there is no reduction in the bonding strength or contamination due to.
- Formula (DkX ⁇ bonded surface area of carbonized carbide bonded body (cm 2 ) ⁇ X ⁇ free carbon content of sintered carbonized carbide (%) ⁇ (g) For example, when two sintered bodies having the same surface are joined, the surface area seen on the projection surface of the surface of one of the sintered carbide bodies is shown.
- the total surface area seen from the projected surface of all bonded surfaces of the sintered carbide is the 1Z2 area.
- k is 0.08 to 0.12, and is a coefficient obtained experimentally.
- the dimension is g / cm 2
- Silicon metal is sandwiched between the surfaces of two or more sintered silicon carbide bodies to be joined.
- a silicon metal powder is spread on the surface of one of the carbide carbide sintered bodies, and then the surface on which the other silicon carbide sintered body is joined is overlapped on the surface on which the silicon metal is dispersed.
- the silicon carbide sintered body may be disposed close to each other so as to obtain a predetermined space (arranged so that the bonding surfaces face each other), and the space may be filled with metal silicon powder. At this time, it is not necessary to pressurize in particular. For example, when joining in the state in which the sintered carbide bodies are stacked, it is sufficient that the surface does not shift even if the weight of the sintered carbide bodies is loaded.
- a method of spraying silicon metal on the surface of the sintered carbide body for example, there is a method using a funnel or the like so that the surface of the sintered carbide body is covered with silicon metal.
- the silicon carbide sintered body sandwiching the silicon metal is subjected to a high-temperature heat treatment.
- the heat treatment is preferably performed in a vacuum or in an inert gas atmosphere other than nitrogen gas, which is preferably performed in a non-acidic atmosphere.
- the inert gas used is preferably argon gas or helium gas.
- nitrogen gas is used as an inert gas, it reacts with silicon metal at a high temperature to form nitride nitride, and the joint surface may be peeled off or broken due to a difference in thermal expansion.
- argon gas and helium gas are non-reactive even at high temperatures, such problems do not occur and are preferable.
- the heating temperature is preferably 1450 ° C to 2200 ° C as long as it is equal to or higher than the melting point of silicon metal. Below 1450 ° C, silicon metal does not melt, and at 2200 ° C, silicon metal partially sublimes.
- the upper limit is preferably 2000 ° C when j8 type carbide is used as the raw material, and 1800 ° C when ⁇ type is used. In particular, bonding at about 1600 ° C is preferable because a high-strength bonded body can be produced efficiently. Further, it is preferable to raise the temperature gently because the reaction between silicon metal and free carbon in the sintered carbonized carbon body proceeds sufficiently. Specifically It is preferable to raise the temperature at 5 ° CZ min to 15 ° CZ min, especially about 10 ° CZ min.
- a heater unit having excellent temperature rise and temperature drop characteristics is provided.
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JP2003308951A (ja) * | 2002-04-15 | 2003-10-31 | Sumitomo Osaka Cement Co Ltd | 給電用電極棒と給電用端子との連結構造、ヒータエレメント、加熱装置及び基板加熱装置 |
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