JP5143367B2 - Opaque sintered body - Google Patents
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- JP5143367B2 JP5143367B2 JP2006067506A JP2006067506A JP5143367B2 JP 5143367 B2 JP5143367 B2 JP 5143367B2 JP 2006067506 A JP2006067506 A JP 2006067506A JP 2006067506 A JP2006067506 A JP 2006067506A JP 5143367 B2 JP5143367 B2 JP 5143367B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 84
- 239000000377 silicon dioxide Substances 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 14
- 239000010419 fine particle Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- 238000005452 bending Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000005049 silicon tetrachloride Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 229910052581 Si3N4 Inorganic materials 0.000 description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 7
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- -1 alkyl silicate Chemical compound 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000003377 silicon compounds Chemical class 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Description
本発明は軽量で曲げ強度に優れ、白色度が高く、かつ表面平滑性に優れた不透明焼結体を提供するものである。 The present invention provides an opaque sintered body that is lightweight, excellent in bending strength, high in whiteness, and excellent in surface smoothness.
一般的な半導体製造工程における様々な熱処理工程において、石英ガラス製の治具が使用されている。この石英ガラス製の治具が使用される理由は、被処理物のシリコンウエハーを金属等の不純物によって汚染させず、かつ、高温耐熱性・耐薬品性に優れていることによるものである。
石英ガラスは透明石英ガラスの他に、外見が白色に見える不透明石英ガラスと呼ばれるものもあり、半導体製造工程用の治具として主に断熱用製品として利用されており、特許文献１及び２に開示されている。
In addition to transparent quartz glass, quartz glass is also known as opaque quartz glass that looks white, and is mainly used as a product for heat insulation as a jig for semiconductor manufacturing processes, and is disclosed in Patent Documents 1 and 2 Has been.
この白色の不透明石英ガラスは、一般的な透明石英ガラスと同じ原料である天然水晶粉などの珪酸質原料粉末に添加剤として窒化珪素微粉末（Ｓｉ3Ｎ4）を一定量添加したものを酸素・水素の混合炎などにより溶融してインゴット化したものである。添加剤である窒化珪素を加えることにより、高温時における窒化珪素の熱分解により発生した窒素ガスによりインゴット自体が溶融時に発泡して不透明石英ガラスが製造される。
溶融インゴット内部には、平均粒径で８０μｍ程度の独立した気泡が形成され、この泡によって溶融インゴット自体は白く見えると共に、一般的な透明石英ガラスと比較して断熱特性・遮光性等に優れる性質を有することになる。
This white opaque quartz glass is made by adding a certain amount of silicon nitride fine powder (Si 3 N 4 ) as an additive to a siliceous raw material powder such as natural quartz powder which is the same raw material as general transparent quartz glass. -It is melted and ingot by hydrogen mixed flame. By adding silicon nitride as an additive, the ingot itself is foamed when melted by nitrogen gas generated by thermal decomposition of silicon nitride at a high temperature to produce opaque quartz glass.
Inside the molten ingot, independent bubbles with an average particle size of about 80 μm are formed, and the bubbles make the molten ingot itself appear white and have excellent heat insulating properties, light shielding properties, etc. compared to general transparent quartz glass Will have.
しかしながら、この不透明石英ガラスは断熱特性・遮光性において優れている反面、内部気泡の影響によりガラス表面の平滑性（表面粗さ）が透明石英ガラスのものより劣っている。一般的な石英ガラス加工である切断加工や研削加工を施すことによって表面の粗さを抑えることは困難であるため、ガラス表面を酸素・水素混合炎で処理をする、いわゆる焼き仕上げ加工という処理方法によって表面に数十μｍ程度の透明層（焼き仕上げ層）を形成することで表面平滑性を改善する試みがなされている。 However, while this opaque quartz glass is excellent in heat insulating properties and light shielding properties, the smoothness (surface roughness) of the glass surface is inferior to that of transparent quartz glass due to the influence of internal bubbles. Since it is difficult to reduce the surface roughness by cutting or grinding, which is a general quartz glass processing, the so-called baked finish processing method that treats the glass surface with an oxygen / hydrogen mixed flame Attempts have been made to improve surface smoothness by forming a transparent layer (baked finish layer) of about several tens of μm on the surface.
また、添加剤の窒化珪素をある一定量以上加えると、耐熱特性・遮光性の目安となる白色度が増加するが、溶融インゴットの平均気泡径が大きくなり、その結果、表面粗さが悪くなる（粗くなる）傾向となる。機械的特性もこの気泡の存在によって低下し、例えば４点曲げ強度が透明石英ガラスに比べて弱いという問題を有している。 Adding a certain amount or more of silicon nitride as an additive increases whiteness, which is a measure of heat resistance and light shielding properties, but increases the average cell diameter of the molten ingot, resulting in poor surface roughness. It tends to be (rough). The mechanical characteristics are also lowered by the presence of the bubbles, and there is a problem that, for example, the four-point bending strength is weaker than that of transparent quartz glass.
特許文献３（特開平７−１６５４３４号「発泡シリカガラスの製造方法」）のようにシリカ粉末と窒化珪素添加剤粉末との混合粉末を成型後に加熱発泡させて低密度の軽量化された断熱・保温材に適した材料としての発泡石英ガラスがある。しかしながら、この発泡石英ガラスも低密度化が達成できても、より発泡させるために気泡径も大きく強度面で問題があり、表面粗さも悪く、表面状態を改善するための機械的加工や熱的加工によっても平滑な面が得られないという問題を有していた。
本発明は、低密度でありながら高い機械的強度をもち、かつ表面平滑性に優れた新たな断熱・構造材を提供するものである。
As in Patent Document 3 (Japanese Patent Laid-Open No. 7-165434, “Method for producing foamed silica glass”), a mixed powder of silica powder and silicon nitride additive powder is heated and foamed after molding to reduce the weight and heat of the low density. There is foamed quartz glass as a material suitable for a heat insulating material. However, even if this foamed quartz glass can achieve a lower density, there is a problem in terms of strength because the bubble diameter is larger and the strength is poor, the surface roughness is poor, and mechanical processing and thermal treatment are required to improve the surface condition. There was a problem that a smooth surface could not be obtained even by processing.
The present invention provides a new heat insulating / structural material having a low mechanical density and a high mechanical strength and an excellent surface smoothness.
本発明は、四塩化珪素やアルキルシリケートなどの珪素化合物を酸素・水素火炎中で加水分解させ、形成されたシリカ微粒子をターゲットに積層させて軸方向に成長させて高純度のシリカ多孔質の積層体を製造し、この積層体を温度１１００〜１４００℃で８〜１６時間加熱処理し、嵩密度が１．３×１０3Ｋｇ／ｍ3以下、曲げ強度が３９ＭＰａ以上とした不透明焼結体である。 In the present invention, a silicon compound such as silicon tetrachloride or alkyl silicate is hydrolyzed in an oxygen / hydrogen flame, and the formed silica fine particles are laminated on a target and grown in the axial direction to laminate a high purity porous silica. The laminate was heat-treated at a temperature of 1100 to 1400 ° C. for 8 to 16 hours, and an opaque sintered body having a bulk density of 1.3 × 10 3 Kg / m 3 or less and a bending strength of 39 MPa or more. is there.
シリカ多孔質体の熱処理は、窒素もしくは一酸化炭素と窒素の混合ガス、もしくは塩素と窒素の混合ガス雰囲気中でおこなう。得られた不透明シリカ焼結体は、従来の不透明石英ガラスよりも機械的曲げ強度に優れていると共に、シリカ微粒子の粒径が微小であるため表面粗さが小さい。
シリカ多孔質体の加熱処理は、電気炉によっておこなう。加熱条件は一酸化炭素ガス含有雰囲気内で、温度１１００〜１４００℃で、処理時間は８〜１６時間程度が好ましい。１１００℃未満では一酸化炭素含有ガスとの反応が充分に進行せず強度が低下し、また、１４００℃を超えると焼結体の透明化が進行して不透明シリカ焼結体が得られない恐れがある。白色度の高いものを得るためには１３００℃未満とすることが好ましい。
The heat treatment of the porous silica is performed in an atmosphere of nitrogen, a mixed gas of carbon monoxide and nitrogen, or a mixed gas of chlorine and nitrogen. The obtained opaque silica sintered body is superior in mechanical bending strength to conventional opaque quartz glass, and has a small surface roughness because the particle size of the silica fine particles is very small.
The heat treatment of the porous silica is performed by an electric furnace. The heating conditions are preferably a carbon monoxide gas-containing atmosphere, a temperature of 1100 to 1400 ° C., and a treatment time of about 8 to 16 hours. If the temperature is lower than 1100 ° C., the reaction with the carbon monoxide-containing gas does not proceed sufficiently and the strength is lowered. If the temperature exceeds 1400 ° C., the sintered body may become transparent and an opaque silica sintered body may not be obtained. There is. In order to obtain a high whiteness, the temperature is preferably less than 1300 ° C.
低温度域での温度加熱となる場合は、一定時間以上加熱を保持しないと焼結が不十分となり、また、一定以上の加熱保持時間を超えると焼結体の密度を低密度に保てなくなる。
このように焼結体の嵩密度は焼結時の加熱条件並びに処理時間によってコントロールできるものであり、焼結体の嵩密度を１．３×１０3Ｋｇ／ｍ3以下に制御することができる。
In case of temperature heating in a low temperature range, if the heating is not maintained for a certain time or longer, the sintering will be insufficient, and if the heating and holding time for a certain time is exceeded, the density of the sintered body cannot be kept low. .
Thus, the bulk density of the sintered body can be controlled by heating conditions and processing time during sintering, and the bulk density of the sintered body can be controlled to 1.3 × 10 3 Kg / m 3 or less. .
一酸化炭素ガス含有雰囲気としては、一酸化炭素ガスとＨｅ、Ａｒなどの不活性ガスとの混合ガス雰囲気としても良いが、一酸化炭素ガスと窒素ガスとの混合ガスとすることが好ましい。これは窒素ガスの方が経済的にも有利であり、また、窒素ガスによりシリカ焼結体中のＳｉ−ＯＨ構造がＳｉ−Ｎ構造となると考えられるためである。Ｓｉ−Ｎ結合は結合強度が強いため、還元性の強いガスである一酸化炭素ガスによりＯＨ基やＣｌ基が除去された後のシリカ焼結体構造を強固にして、嵩密度が低いのにもかかわらず、機械的強度が高いものとなる。 The carbon monoxide gas-containing atmosphere may be a mixed gas atmosphere of carbon monoxide gas and an inert gas such as He or Ar, but is preferably a mixed gas of carbon monoxide gas and nitrogen gas. This is because nitrogen gas is more economically advantageous, and it is considered that the Si—OH structure in the sintered silica becomes a Si—N structure due to the nitrogen gas. The Si-N bond has a strong bond strength, so that the structure of the sintered silica after the OH group and Cl group are removed by the carbon monoxide gas, which is a highly reducing gas, is strengthened and the bulk density is low Nevertheless, the mechanical strength is high.
本発明のシリカ微粒子の積層体を加熱処理した焼結体は、白色を呈し、嵩密度が１．３×１０3Ｋｇ／ｍ3以下、曲げ強度が３９ＭＰａ以上である不透明焼結体である。
この不透明焼結体は、シリカ微粒子の粒径が０．１〜０．５μｍであって、白色度が９８％以上であり、表面粗さがＲａで０．３μｍ以下のものである。
The sintered body obtained by heat-treating the laminate of silica fine particles of the present invention is an opaque sintered body that exhibits white color, has a bulk density of 1.3 × 10 3 Kg / m 3 or less, and a bending strength of 39 MPa or more.
This opaque sintered body has a silica fine particle diameter of 0.1 to 0.5 μm, a whiteness of 98% or more, and a surface roughness Ra of 0.3 μm or less.
本発明の不透明焼結体は、シリカ微粒子を堆積させた多孔質体を加熱処理して焼結したものであるので、低密度であると共に、高い機械的強度を有し、かつ表面平滑性に優れたものである。高純度に精製された四塩化珪素やアルキルシリケートなどの珪素化合物を原料として酸素・水素火炎中で加水分解させ、得られたシリカ微粒子をターゲットに堆積させ、軸方向に成長させることにより得られるシリカ多孔質体を焼結するものであり、原料の四塩化珪素やアルキルシリケートなどの珪素化合物に含有される金属元素、Ｎａ，Ｌｉ，Ｋなどのアルカリ金属、Ｃａ，Ｍｇなどのアルカリ土類金属、Ｆｅ，Ａｌ，Ｃｕ，Ｚｎ，Ｃｏ，Ｃｒ，Ｎｉ，Ｔｉなどの遷移金属の不純物が、それぞれ５０ｐｐｂ以下、好ましくは２０ｐｐｂ以下のものを使用することが可能である。このような高純度の四塩化珪素やアルキルシリケートなどの珪素化合物は、蒸留精製などで簡単に得ることができるため、金属不純物が５０ｐｐｂ以下の極めて高純度な不透明焼結体を得ることができる。 The opaque sintered body of the present invention is obtained by heating and sintering a porous body on which silica fine particles are deposited, so that it has low density, high mechanical strength, and surface smoothness. It is excellent. Silica obtained by hydrolyzing silicon compounds such as silicon tetrachloride and alkyl silicate purified to high purity in an oxygen / hydrogen flame as raw materials, and depositing the resulting silica fine particles on the target and growing them in the axial direction A porous body is sintered, a metal element contained in a silicon compound such as silicon tetrachloride or alkylsilicate as a raw material, an alkali metal such as Na, Li or K, an alkaline earth metal such as Ca or Mg, It is possible to use transition metal impurities such as Fe, Al, Cu, Zn, Co, Cr, Ni, and Ti that are 50 ppb or less, preferably 20 ppb or less, respectively. Since such silicon compounds such as high-purity silicon tetrachloride and alkyl silicate can be easily obtained by distillation purification or the like, an extremely high-purity opaque sintered body having a metal impurity of 50 ppb or less can be obtained.
実施例
以下、実施例により本発明を具体的に説明するが、本発明はこれら実施例に限定されるものでないことはいうまでもない。
高純度の四塩化珪素を気化させて酸素・水素火炎を形成しているバーナーの中心層に導入することによって加水分解させ、シリカ粉をターゲット上に付着させ、軸方向に引上げ成長させ、２００ｍｍφ×６００ｍｍＬ、嵩密度０．３×１０3Ｋｇ／ｍ3のシリカ多孔質体を得た。
このシリカ多孔質体を２００ｍｍφ×１００ｍｍの寸法に切り出してサンプルとした。このサンプルをシリカガラス製炉芯管を装着した横型管状炉内にセットし、一酸化炭素ガス及び窒素ガスの混合ガスを流通させ、管状炉を１１００℃まで昇温させた後、６０℃／時間の昇温速度で１２８０℃まで昇温させ、その温度で１２時間保持し、室温で冷却した。
得られたシリカ焼結体を３ｍｍの厚さに切断して白色度、表面粗さ、シリカ微粒子の粒径、熱的特性等の各種特性について測定した。なお、ＪＩＳに定められている曲げ強度の測定は、規定に従い、４０ｍｍ×４ｍｍ×３ｍｍ厚に切り出したものを使用して測定した。
Examples Hereinafter, the present invention will be specifically described by way of examples, but it is needless to say that the present invention is not limited to these examples.
Hydrolysis is achieved by vaporizing high purity silicon tetrachloride and introducing it into the central layer of the burner forming an oxygen / hydrogen flame, causing silica powder to adhere to the target, and pulling up and growing in the axial direction. A porous silica material having 600 mmL and a bulk density of 0.3 × 10 3 Kg / m 3 was obtained.
This silica porous body was cut into a size of 200 mmφ × 100 mm and used as a sample. This sample was set in a horizontal tubular furnace equipped with a silica glass furnace core tube, a mixed gas of carbon monoxide gas and nitrogen gas was circulated, the temperature of the tubular furnace was increased to 1100 ° C., and then 60 ° C./hour. The temperature was raised to 1280 ° C. at a rate of temperature rise, maintained at that temperature for 12 hours, and cooled at room temperature.
The obtained silica sintered body was cut into a thickness of 3 mm and measured for various properties such as whiteness, surface roughness, silica fine particle size, and thermal properties. In addition, the measurement of the bending strength prescribed | regulated to JIS was measured using what was cut out to 40 mm x 4 mm x 3 mm thickness according to regulation.
比較例
珪石粉に窒化珪素を０．２ｗｔ％添加混合した原料粉末を、酸水素火炎溶融法により溶融して嵩密度２．０６×１０3Ｋｇ／ｍ3、平均泡径８０μｍの不透明石英ガラスインゴットを得た。この不透明石英ガラスの諸特性も実施例と同様に測定した。
Comparative Example An opaque quartz glass ingot having a bulk density of 2.06 × 10 3 Kg / m 3 and an average bubble diameter of 80 μm obtained by melting a raw material powder obtained by adding and mixing 0.2 wt% of silicon nitride to silica stone powder by an oxyhydrogen flame melting method Got. Various characteristics of the opaque quartz glass were also measured in the same manner as in the examples.
実施例の焼結体は、外見が白色であり、その白色度を、コニカミノルタ製の色彩色差計ＣＲ−４００で測定した。結果を表１に示す。表１に示すよう白色度（％）は、９８％であり、比較例の不透明石英ガラスの７０％に比べても大きい値を示した。また、この白色度は生成した焼結体のどの部分においてもほぼ同じであり、白色度は均一化されている。
なお、比較例に準じて窒化珪素の添加量だけを５倍及び１０倍増やして製造した不透明石英ガラスの白色度を測定したが、５倍品で７８％、１０倍品で７９％と、白色度は向上したものの、表面粗さは更に悪いものとなっていた。
The sintered bodies of the examples have a white appearance, and the whiteness was measured with a color difference meter CR-400 manufactured by Konica Minolta. The results are shown in Table 1. As shown in Table 1, the whiteness (%) was 98%, which was larger than 70% of the opaque quartz glass of the comparative example. Further, this whiteness is almost the same in any portion of the produced sintered body, and the whiteness is uniform.
In addition, according to the comparative example, the whiteness of the opaque quartz glass manufactured by increasing only the addition amount of silicon nitride by 5 times and 10 times was measured, but the whiteness was 78% for the 5 times product and 79% for the 10 times product. Although the degree was improved, the surface roughness was worse.
焼結体はこの０．１〜０．５μｍのシリカ微粒子の焼結集合体であり、この粒子間の小さな空隙が微小気泡として存在している。実際にはこの焼結体中の微小気泡は、閉気泡ではなく、開放状態の微小気孔が連続したものであることが認められる。
The sintered body is a sintered aggregate of silica fine particles of 0.1 to 0.5 μm, and small voids between the particles exist as microbubbles. Actually, it is recognized that the microbubbles in the sintered body are not closed cells but continuous micropores.
実施例の焼結体の嵩密度は１．０９×１０3Ｋｇ／ｍ3であった。比較例の不透明石英ガラスの嵩密度が２．０６×１０3Ｋｇ／ｍ3であり、約５３％であり軽量で低密度である。 The bulk density of the sintered body of the example was 1.09 × 10 3 Kg / m 3 . The bulk density of the opaque quartz glass of the comparative example is 2.06 × 10 3 Kg / m 3 , about 53%, light weight and low density.
焼結体の機械的強度（４点曲げ強度）は、表２のように１０サンプル測定して平均で５０ＭＰａとなり、比較例の不透明石英ガラスに比べて約３０％高い結果が得られた。
焼結体の曲げ強度は、低密度でありながら不透明石英ガラスの曲げ強度である３９ＭＰａ以上となっている。
The mechanical strength (4-point bending strength) of the sintered body was 50 samples on average when 10 samples were measured as shown in Table 2, and about 30% higher than the opaque quartz glass of the comparative example was obtained.
The bending strength of the sintered body is 39 MPa or more, which is the bending strength of opaque quartz glass, although it is low density.
実施例で得た素材を石英ガラスの加工で一般的に使用される内周刃切断機（＃１７０）で切断後、ロータリー平面加工研削機（＃１２０）で研削し、研削面の表面粗さを測定した。表３に示すように、表面粗さＲａは０．３μｍ以下に抑えられており、比較例の不透明石英ガラスの表面粗さＲａよりも小さかった。
その他の切断機や研削機、または研磨機等を用いても、加工ツールや加工条件を変えることで更に表面粗さを抑えることができた。
After the material obtained in the examples was cut with an inner peripheral cutting machine (# 170) generally used in the processing of quartz glass, it was ground with a rotary surface processing grinder (# 120), and the surface roughness of the grinding surface Was measured. As shown in Table 3, the surface roughness Ra was suppressed to 0.3 μm or less, and was smaller than the surface roughness Ra of the opaque quartz glass of the comparative example.
Even when other cutting machines, grinding machines, polishing machines, etc. were used, the surface roughness could be further suppressed by changing the processing tools and processing conditions.
上記焼結体の熱的特性（熱伝導率、比熱、熱拡散率、熱容量）をレーザーフラッシュ法熱定数測定装置を用いて測定した。その結果を表４に示す。
比較例の不透明石英ガラスに比べて焼結体は熱伝導率も０．５Ｗ／（ｍ・Ｋ）以下となっており、断熱・耐熱効果が向上している。
The thermal characteristics (thermal conductivity, specific heat, thermal diffusivity, heat capacity) of the sintered body were measured using a laser flash method thermal constant measuring apparatus. The results are shown in Table 4.
Compared to the opaque quartz glass of the comparative example, the sintered body has a thermal conductivity of 0.5 W / (m · K) or less, and the heat insulation and heat resistance effects are improved.
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