JP2010150123A - 窒化珪素・メリライト複合焼結体及びそれを用いた装置 - Google Patents
窒化珪素・メリライト複合焼結体及びそれを用いた装置 Download PDFInfo
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- JP2010150123A JP2010150123A JP2009216741A JP2009216741A JP2010150123A JP 2010150123 A JP2010150123 A JP 2010150123A JP 2009216741 A JP2009216741 A JP 2009216741A JP 2009216741 A JP2009216741 A JP 2009216741A JP 2010150123 A JP2010150123 A JP 2010150123A
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- Prior art keywords
- silicon nitride
- sintered body
- melilite
- composite sintered
- mol
- 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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- 229910001719 melilite Inorganic materials 0.000 title claims abstract description 137
- 239000002131 composite material Substances 0.000 title claims abstract description 93
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000010703 silicon Substances 0.000 title abstract description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 132
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 131
- 239000004065 semiconductor Substances 0.000 claims abstract description 35
- 238000007689 inspection Methods 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims description 54
- 239000000523 sample Substances 0.000 claims description 37
- 239000000654 additive Substances 0.000 claims description 34
- 230000000996 additive effect Effects 0.000 claims description 30
- 230000000737 periodic effect Effects 0.000 claims description 29
- 238000004519 manufacturing process Methods 0.000 claims description 24
- 229910052746 lanthanum Inorganic materials 0.000 claims description 12
- 229910052684 Cerium Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 229910052712 strontium Inorganic materials 0.000 claims description 9
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000005245 sintering Methods 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 16
- 238000010304 firing Methods 0.000 description 16
- 239000001301 oxygen Substances 0.000 description 16
- 239000000919 ceramic Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000011521 glass Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000005452 bending Methods 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- -1 W or Mo is used Chemical class 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910052695 Americium Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052685 Curium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910052766 Lawrencium Inorganic materials 0.000 description 1
- 229910052764 Mendelevium Inorganic materials 0.000 description 1
- 229910052781 Neptunium Inorganic materials 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910021472 group 8 element Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 description 1
- GONBZNBMLOZYAM-UHFFFAOYSA-K yttrium(3+);triformate Chemical compound [Y+3].[O-]C=O.[O-]C=O.[O-]C=O GONBZNBMLOZYAM-UHFFFAOYSA-K 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/28—Testing of electronic circuits, e.g. by signal tracer
- G01R31/2851—Testing of integrated circuits [IC]
- G01R31/2886—Features relating to contacting the IC under test, e.g. probe heads; chucks
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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
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- C04B35/593—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 silicon nitride obtained by pressure sintering
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- C04B35/593—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 silicon nitride obtained by pressure sintering
- C04B35/5935—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 silicon nitride obtained by pressure sintering obtained by gas pressure sintering
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Abstract
【解決手段】窒化珪素・メリライト複合焼結体は、窒化珪素及びメリライト(Me2Si3O3N4、Meは窒化珪素とメリライトを形成する金属元素)を含む複合焼結体であって、Siを、Si3N4換算で41〜83モル%、Meを、酸化物換算で13〜50モル%、含有する。また、装置は、半導体検査用装置であって、そのような窒化珪素・メリライト複合焼結体を用いて構成される。
【選択図】図1A
Description
ここで、窒化珪素の主ピーク回折強度aとは、窒化珪素のピークのうち最も高いピークの回折強度をいい、また、メリライトの主ピーク回折強度bとは、メリライトのピークのうち最も高いピークの回折強度をいう。
50≦[b/(a+b)]×100≦98を満足していることが好ましい。この場合、焼結体は、2〜6ppm/Kの範囲の任意の平均熱膨張係数(23〜150℃)を有することができる。
平均粒径0.7μmの窒化珪素(Si3N4)粉末、平均粒径1.2μmのイットリア(Y2O3)粉末、SrCO3粉末、La2O3粉末、CeO2粉末およびAl2O3粉末を用い、表1〜表5に示す組成の混合粉末を得た。得られた混合粉末とエタノールを、ボールミル容器中に投入し混合した後、加熱乾燥し、造粒した。
[理論密度比]
焼結体の寸法および重量を測定し、理論密度(イットリア(Y2O3)粉末がすべてメリライト(Me2Si3O3N4)に変換され、残りの窒化珪素はそのままで、その他添加物は各酸化物の状態で存在したと仮定して計算)に対する比率を算出した。
焼結体に吸水処理(水中にて脱泡)を行った後、乾燥させ、次式により算出した。
吸水率(%)=[(W1−W2)/W2)]×100
(W1:吸水処理後の焼結体重量、W2:乾燥後の焼結体重量)
[メリライト主ピーク強度比率]
焼結体を粉砕し、X線回折装置((株)リガク製 RU−200T)により、粉末X線回折を行い、メリライト(Me2Si3O3N4)の主ピーク回折強度bおよびSi3N4の主ピーク強度aを求め、次式より算出した。
メリライト主ピーク強度比率(%)=[b/(a+b)]×100
熱膨張係数測定機((株)リガク製 熱機械分析装置 8310シリーズ)を用いて、圧縮荷重法にて23〜150℃の平均熱膨張係数を求めた。
[曲げ強度]
JIS R 1601に準拠して室温(23℃)で測定した
[ヤング率]
JIS R 1602に規定する超音波パルス法により室温(23℃)で測定した。
3mm×4mm×10mmの形状に切断した焼結体の4mm×10mmの表面に鏡面加工を施した後、その表面をSEM(日本電子(株)製 JSM−6460LA)にて観察し、さらにEPMA(日本電子(株)製 JXA−8500F)を用いて二次電子像、反射電子像の観察、及びWDS(波長分散型X線分光器)ビームスキャンマッピングを行い、その表面における窒化珪素結晶相、メリライト結晶相、並びに、ガラス相及び窒化珪素とメリライト以外の結晶相(表中、「その他」と記載)の面積比を求めた。なお、必要に応じて(ガラス相や窒化珪素とメリライト以外の結晶相が多く、前記機器による観察だけでは面積比を求めることが困難である場合等)、STEM(走査型透過電子顕微鏡)((株)日立ハイテクノロジーズ製HD−2000)及びEDS(エネルギー分散型X線分析装置)(EDAX製Genesis)を用いた。また、場合により、鏡面加工面にエッチング処理を行い、このエッチング面をSEM等で観察して面積比を求めた。
Claims (16)
- 窒化珪素結晶相と、メリライト結晶相(Me2Si3O3N4、Meはメリライトを形成する金属元素)と、粒界相とを有する複合焼結体であって、
前記複合焼結体の切断面における前記メリライト結晶相の占める割合が、20%以上であることを特徴とする窒化珪素・メリライト複合焼結体。 - 前記複合焼結体の吸水率が1.5%以下であり、かつ、メリライト結晶相の占める割合と、前記切断面における前記窒化珪素結晶相の占める割合との和が、80%以上である請求項1に記載の窒化珪素・メリライト複合焼結体。
- Siを、Si3N4換算で41〜83モル%、
Meを、酸化物換算で13〜50モル%、
含有する請求項1または2に記載の窒化珪素・メリライト複合焼結体。 - Siを、Si3N4換算で41〜79モル%、
Meを、酸化物換算で13〜46モル%、
添加物として、周期表IIa族元素を、酸化物換算で5〜20モル%、
含有する請求項1ないし3のいずれかに記載の窒化珪素・メリライト複合焼結体。 - 添加物として、Mg、Ca、およびSrの少なくとも1種が添加される請求項4に記載の窒化珪素・メリライト複合焼結体。
- 添加物として、Srが添加される請求項4に記載の窒化珪素・メリライト複合焼結体。
- Siを、Si3N4換算で45〜83モル%、
Meを、酸化物換算で15〜49モル%、
添加物として、La、Ce、およびPrの少なくとも1種を、酸化物換算で0.3〜12モル%、
含有する請求項1ないし3のいずれかに記載の窒化珪素・メリライト複合焼結体。 - 添加物として、Al、Si、周期表IVa族元素、周期表Va族元素、および周期表VIa族元素からなる群より選択される少なくとも1種の元素がさらに添加される請求項4ないし7のいずれかに記載の窒化珪素・メリライト複合焼結体。
- Alを、酸化物換算で0.5〜10モル%含有する請求項8に記載の窒化珪素・メリライト複合焼結体。
- Meが、周期表IIIa族元素である請求項1ないし9のいずれかに記載の窒化珪素・メリライト複合焼結体。
- Meが、Yである請求項10に記載の窒化珪素・メリライト複合焼結体。
- X線回折により得られる窒化珪素の主ピーク回折強度aおよびメリライトの主ピーク回折強度bが、次式
50≦[b/(a+b)]×100≦98
を満足する請求項1ないし11のいずれかに記載の窒化珪素・メリライト複合焼結体。 - 平均熱膨張係数(23〜150℃)が2〜6ppm/Kである請求項1ないし12のいずれかに記載の窒化珪素・メリライト複合焼結体。
- ヤング率が200GPa以上である請求項1ないし13のいずれかに記載の窒化珪素・メリライト複合焼結体。
- 半導体の検査または製造を行うための装置であって、
請求項1ないし14のいずれかに記載の窒化珪素・メリライト複合焼結体を用いた部材
を備えることを特徴とする半導体検査または製造用装置。 - プローブカードである請求項15に記載の半導体検査または製造用装置。
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