JP5177979B2 - Composite quartz glass tube for semiconductor manufacturing - Google Patents
Composite quartz glass tube for semiconductor manufacturing Download PDFInfo
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- JP5177979B2 JP5177979B2 JP2006239779A JP2006239779A JP5177979B2 JP 5177979 B2 JP5177979 B2 JP 5177979B2 JP 2006239779 A JP2006239779 A JP 2006239779A JP 2006239779 A JP2006239779 A JP 2006239779A JP 5177979 B2 JP5177979 B2 JP 5177979B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 103
- 239000002131 composite material Substances 0.000 title claims description 30
- 239000004065 semiconductor Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000000460 chlorine Substances 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 238000007496 glass forming Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 description 30
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 150000001340 alkali metals Chemical class 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004031 devitrification Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Description
本発明は、半導体の製造に使用される、拡散炉用炉心管、高温アニール処理部材などに好適な半導体製造用複合石英ガラス管に関する。 The present invention relates to a composite quartz glass tube for semiconductor production suitable for a core tube for a diffusion furnace, a high-temperature annealing treatment member, and the like used for semiconductor production.
石英ガラスは、耐熱性、耐衝撃性、耐薬品性に優れ、且つ機械的強度も高いところから半導体製造工程における部材を初め各種用途に用いられている。その例として拡散炉用炉芯管、高温アニール処理部材などが挙げられる。近年、集積回路の高集積化が急速に進展するにともない半導体の仕様が厳しくなり処理温度が高くなるとともに結晶欠陥などの欠陥の少ない高品質の半導体が求められるようになった。前記結晶欠陥を起こさせる因子としては部材自体の純度や外部、例えばヒーターやライナー管からの金属不純物、特にアルカリ金属不純物の飛散が挙げられる。石英ガラス部材自体汚染を防ぐには合成石英ガラスのような高純度の石英ガラスを使用すればよいが、合成石英ガラスは耐熱性に劣り半導体の高温熱処理中に部材が大きく変形する欠点がある。そのため通常は、天然水晶などから作成された天然石英ガラスからなる部材が用いられているが、天然水晶などには微量な不純物が含有されておりそれが半導体の結晶欠陥の原因となり高品質の半導体を生産性よく製造することを困難にしていた。その上、天然石英ガラスは、外部からの金属不純物の飛散を遮蔽する効果に乏しく半導体のこれら飛散不純物による汚染が避けがたかった。 Quartz glass is used in various applications including members in semiconductor manufacturing processes because of its excellent heat resistance, impact resistance, chemical resistance, and high mechanical strength. Examples thereof include a furnace core tube for a diffusion furnace, a high temperature annealing treatment member, and the like . In recent years, with the rapid progress of higher integration of integrated circuits, the specifications of semiconductors have become stricter, the processing temperature has become higher, and high-quality semiconductors with fewer defects such as crystal defects have been demanded. Factors causing the crystal defects include the purity of the member itself and the scattering of metal impurities, particularly alkali metal impurities from the outside, for example, a heater or a liner tube. In order to prevent contamination of the quartz glass member itself, high-purity quartz glass such as synthetic quartz glass may be used. However, synthetic quartz glass is inferior in heat resistance and has a drawback that the member is greatly deformed during high-temperature heat treatment of a semiconductor. For this reason, members made of natural quartz glass made from natural quartz or the like are usually used, but natural quartz or the like contains a small amount of impurities, which causes crystal defects in the semiconductor and is a high-quality semiconductor. It was difficult to manufacture with good productivity. Moreover, natural quartz glass has a poor effect of shielding the scattering of metal impurities from the outside, and it has been difficult to avoid contamination of the semiconductor by these scattered impurities.
こうした問題点を解決すべく、特許公報１では、半導体ウエーハの処理工程の熱酸化・拡散炉に用いられる石英ガラス炉芯管として、最内層を炉芯管総肉厚の５〜３５％とし、含有するＯＨ基量が１,０００〜２,０００ppmの合成石英ガラスで形成し、さらに、外層を天然などの高純度の石英ガラスで形成し、所定の耐熱性を保持しつつ、ＯＨ基によって金属不純物を防止する石英ガラス炉芯管が提案されている。しかし、この特許文献１の製造方法では、高純度石英ガラス管内にＳｉＣｌ４と酸水素火炎を導入して多孔質シリカ体の被膜を形成し、その後Ｈ２Ｏ蒸気を導入してガラス化することから複雑な工程を有し工業的メリットに乏しい上に、ＯＨ基が１２０ppm以上導入されることから、耐熱性に劣り近年要求される高耐熱性に答えるものではなかった。また、特許文献２には、ナトリウム、カリウム及びリチウムをいずれも１ppm以下含有し、且つ１,２８０℃温度において１０１２．４ポイズ以上の粘土を有する天然石英ガラスを外層とし、ナトリウム、カリウム及びリチウムをいずれも０．２ppm以下並びに塩素を５００〜４,０００ppm含有する合成石英ガラスを内層とする複合石英ガラス管が提案されている。しかし、この複合石英ガラス管は内層を形成する合成石英ガラスが塩素を５００〜４,０００ppm含有することから高温粘度が低く半導体の高温熱処理時に変形するなどの問題があった。その上、前記複合石英ガラス管は外部から飛散する金属不純物、特にアルカリ金属不純物の遮蔽効果が十分でなくこれらの金属不純物に基づく半導体の汚染の問題があった。 In order to solve such problems, in Patent Publication 1, as the quartz glass furnace core tube used in the thermal oxidation / diffusion furnace of the semiconductor wafer processing step, the innermost layer is 5 to 35% of the total thickness of the furnace core pipe, It is made of synthetic quartz glass with an OH group content of 1,000 to 2,000 ppm, and the outer layer is made of high-purity quartz glass such as natural material. Quartz glass furnace core tubes that prevent impurities have been proposed. However, in the manufacturing method of Patent Document 1, SiCl 4 and an oxyhydrogen flame are introduced into a high-purity quartz glass tube to form a porous silica body coating, and then H 2 O vapor is introduced to vitrify. Therefore, it has a complicated process and lacks industrial merit, and more than 120 ppm of OH group is introduced. Therefore, the heat resistance is inferior and the high heat resistance required in recent years has not been answered. Patent Document 2 discloses a natural quartz glass containing 1 ppm or less of sodium, potassium and lithium, and having a clay of 10 12.4 poise or more at a temperature of 1,280 ° C. as an outer layer, and includes sodium, potassium and lithium. A composite quartz glass tube having a synthetic quartz glass containing 0.2 ppm or less and 500 to 4,000 ppm of chlorine as an inner layer has been proposed. However, this composite quartz glass tube has a problem that the synthetic quartz glass forming the inner layer contains 500 to 4,000 ppm of chlorine, so that the high-temperature viscosity is low and the semiconductor is deformed during high-temperature heat treatment of the semiconductor. In addition, the composite quartz glass tube has an insufficient shielding effect against metal impurities, particularly alkali metal impurities, scattered from the outside, and there is a problem of contamination of the semiconductor based on these metal impurities.
こうした現状に鑑み、本発明者等は鋭意研究を続けた結果、天然石英ガラスと合成石英ガラスの２層からなる半導体製造用複合石英ガラス管において、内層を１,２８０℃における粘度が１０11.7ポイズ以上の高純度の合成石英ガラスで形成し、外層を１,２８０℃温度における粘度が１０12.０ポイズ以上の石英ガラスで形成することで、耐熱性の高い半導体製造用複合石英ガラス管が得られ１,０００℃を越す処理温度で長時間処理しても変形することがない上に、金属不純物の遮蔽効果が良好で外部から飛散する金属不純物を処理空間に飛散させることがない半導体製造用複合石英ガラス管が得られること、特に外層にアルミニウム、バリウム又はガリウムのいずれか１つを含有させることでより高い耐熱性と金属不純物遮蔽性を有する半導体製造用複合石英ガラス管が得られることを見出して、本発明を完成したものである。すなわち In view of these circumstances, the present inventors have made the continued extensive studies, the semiconductor manufacturing composite quartz glass tube made of two layers of synthetic quartz glass and natural quartz glass, the inner layer has a viscosity at 1,280 ° C. 10 11.7 forming a high purity synthetic quartz glass above poise, by viscosity outer layer at 1,280 ° C. temperature form 10 12.0 poise or more quartz glass, high heat resistance semiconductor manufacturing composite quartz glass tube Is a semiconductor that does not deform even if it is processed for a long time at a processing temperature exceeding 1,000 ° C., and has a good shielding effect against metal impurities and does not scatter metal impurities scattered from the outside into the processing space. semiconductor having to manufacture composite quartz glass tube is obtained, in particular aluminum in the outer layer, the high heat resistance and metallic impurities shielding than by containing any one of barium or gallium And it found that manufacturing a composite quartz glass tube is obtained, and completed the present invention. Ie
本発明は、耐熱性に優れている上に、金属不純物の遮蔽効果の高い半導体製造用複合石英ガラス管を提供することを目的とする。 An object of the present invention is to provide a composite quartz glass tube for semiconductor production that has excellent heat resistance and has a high metal impurity shielding effect.
上記目的を達成する本発明は、天然石英ガラスと合成石英ガラスの２層で形成される半導体製造用複合石英ガラス管において、外層が１,２８０℃温度における粘度が１０12.０ポイズ以上の天然石英ガラスからなり、内層が１,２８０℃温度における粘度が１０11.7ポイズ以上の合成石英ガラスからなることを特徴とする半導体製造用複合石英ガラス管に係る。 To achieve the above object, the present invention provides a composite quartz glass tube for semiconductor production formed of two layers of natural quartz glass and synthetic quartz glass . The outer layer has a natural viscosity at a temperature of 1,280 ° C. of 10 12.0 poise or more. made of silica glass, the inner layer according to the composite quartz glass tube for semiconductor manufacturing, wherein the viscosity at 1,280 ° C. temperature of 10 11.7 poise or more synthetic quartz glass.
本発明の半導体製造用複合石英ガラス管の外層を形成する１,２８０℃温度における粘度が１０12.０ポイズ以上の石英ガラスとしては、高純度の天然水晶などからなる天然石英ガラスが挙げられる。より好ましくはナトリウム、カリウム及びリチウムのいずれも１ppm以下の天然石英ガラスがよい。内層を形成する１,２８０℃温度における粘度が１０11.7ポイズ以上の合成石英ガラスとしては、ＷＯ２００４/０５０５７０号公報に記載するようにシリカ多孔質体を１００〜１,３００℃の還元雰囲気中で処理した後、１,３００℃以上１,９００℃以下の温度で焼成し緻密化した合成石英ガラスが挙げられる。この耐熱性に優れた合成石英ガラスは耐熱性を高く維持するため塩素濃度を５００ppm以下、ＯＨ基濃度を１００ppm以下にする。 The 1,280 ° C. viscosity of 10 12.0 poise or more quartz glass at the temperature for forming the outer layer of the semiconductor manufacturing composite quartz glass tube of the present invention, natural silica glass and the like made of a high-purity natural crystal. More preferably, natural quartz glass of any one of sodium, potassium and lithium is 1 ppm or less. The synthetic quartz glass with a viscosity of 10 11.7 poise or more at 1,280 ° C. temperature for forming the inner layer, W O2004 / 050570 No. as described in JP-porous silica and in a reducing atmosphere at 100～1,300 ° C. Examples thereof include synthetic quartz glass that has been densified by firing at a temperature of 1,300 ° C. or more and 1,900 ° C. or less after the treatment. The synthetic quartz glass having excellent heat resistance has a chlorine concentration of 500 ppm or less and an OH group concentration of 100 ppm or less in order to maintain high heat resistance.
上記耐熱性の高い合成石英ガラスとしては好ましくは波長２４５ｎｍの紫外線における吸収係数が０．０１/cm以上の合成石英ガラスがよい。この波長２４５ｎｍの紫外線における吸収係数は石英ガラスの高温粘度と相関関係があり、吸収係数が大きい程高い粘度が得られる。そして、前記合成石英ガラスは炭素や窒素など高耐熱性ドープ剤を含有することで一段と高い吸収係数が得られる。前記高耐熱性の合成石英ガラスはまた金属不純物、特にアルカリ金属不純物に対する遮蔽効果にも優れている。 The synthetic quartz glass having high heat resistance is preferably synthetic quartz glass having an absorption coefficient of 0.01 / cm or more in an ultraviolet ray having a wavelength of 245 nm. The absorption coefficient in the ultraviolet ray having a wavelength of 245 nm has a correlation with the high temperature viscosity of quartz glass, and the higher the absorption coefficient, the higher the viscosity is obtained. The synthetic quartz glass contains a high heat-resistant dopant such as carbon and nitrogen, so that a higher absorption coefficient can be obtained. The high heat-resistant synthetic quartz glass is also excellent in shielding effect against metal impurities, particularly alkali metal impurities.
上記合成石英ガラスからなる内層の厚さは複合石英ガラス管全体の厚さ対して１％であれば金属不純物の拡散防止層として有効であり、また、複合石英ガラス管の厚さに対する肉厚比９９％でも複合石英ガラス管の変形量を小さく抑えることができる。 The thickness of the inner layer made of the synthetic quartz glass is effective as a diffusion preventing layer of metal impurities, if 1% for the total thickness of the composite quartz glass tube, also the thickness to the thickness of the composite quartz glass tube Even when the ratio is 99%, the deformation amount of the composite quartz glass tube can be kept small.
本発明の半導体製造用複合石英ガラス管の外層を高純度の天然石英ガラスとすることで複合石英ガラス管の変形をより小さく保持できる。 The outer layer of the semiconductor manufacturing composite quartz glass tube of the present invention can be further kept small deformation of the composite quartz glass tube by a high purity natural quartz glass.
半導体製造用複合石英ガラス管の金属不純物の遮蔽効果としては前記アルミニウムに加えてバリウム又はガリウムも挙げられる。アルミニウムを含めたこれらの元素のドープ法としては、多孔性シリカ母材に前記元素の例えば硝酸溶液等の溶液又は微粉末を含浸又は混合した上で、還元処理・焼成処理する方法、または、石英ガラス表面に前記溶液を塗布した上で乾燥する方法などが挙げられる。アルミニウム、バリウム又はガリウムの含有は外層の外表面から０．１mmの深さに０．１ｗｔ％以上とするのがよい。特にアルミニウムを含有させた石英ガラス部材を１,０００℃以上で数時間以上加熱処理することによって部材表面に結晶石英ガラスが形成されより高い耐熱性が得られる。 In addition to the aluminum, barium or gallium can be cited as a shielding effect of metal impurities in the composite quartz glass tube for semiconductor production. As a doping method of these elements including aluminum, a porous silica base material is impregnated or mixed with a solution or fine powder of the element, such as a nitric acid solution, and then subjected to a reduction treatment / firing treatment, or quartz. The method of drying after apply | coating the said solution to the glass surface etc. is mentioned. Aluminum, containing barium or gallium preferably set to 0.1 wt% or more at a depth of 0.1mm from the outer surface of the outer layer. In particular, when a quartz glass member containing aluminum is heat-treated at 1,000 ° C. or more for several hours or more, crystalline quartz glass is formed on the surface of the member and higher heat resistance is obtained.
本発明の半導体製造用複合石英ガラス管は、高純度で、耐熱性が高く、１,０００℃を超える高温で長複合時間処理しても形状変化することがなく、また、ヒーターやライナー管等の外部から飛散する金属不純物、特にアルカリ金属不純物の遮蔽効果も優れ、処理する半導体の高品質でかつ生産性よく製造できる。 The composite quartz glass tube for semiconductor production according to the present invention has high purity, high heat resistance, and does not change its shape even when processed at a high temperature exceeding 1,000 ° C. for a long period of time. The metal impurities scattered from the outside, especially alkali metal impurities are also effectively shielded, and the semiconductor to be processed can be manufactured with high quality and high productivity.
以下に本発明の実施例をあげて説明するが、これらの実施例は例示的に示されるもので限定的に解釈されるべきでないことはいうまでもない。 Examples of the present invention will be described below, but it is needless to say that these examples are illustrative and should not be construed in a limited manner.
実施例１
不純物含有量が、Ａｌ：８ｐｐｍ、Ｆｅ：０．２ｐｐｍ、Ｎａ：０．１ｐｐｍ、Ｋ：０．１ｐｐｍで、ＯＨ基濃度：２００ｐｐｍ、１,２８０℃における粘度が１０１２．４ポイズの天然石英ガラスを用いてサイズ３００mmφ×１５００mmＬ×３mmｔの天然石英ガラスチューブを作成し、その外表面に、硝酸アルミニウムの３０％溶液を塗布したのち乾燥させた。一方、不純物含有量が、Ａｌ：０．００１ｐｐｍ、Ｆｅ：０．００１ｐｐｍ、Ｎａ：０．００１ｐｐｍ、Ｋ：０．００１ｐｐｍ、ＯＨ濃度：８０ｐｐｍ、Ｃｌ濃度：２５ｐｐｍで、１,２８０℃における粘度が１０１１．８ポイズの合成石英ガラスを用いてサイズ２７５mmφ×１５００mmＬ×１mmｔの合成石英ガラスチューブを作成し、この合成石英ガラスチューブを前記天然石英ガラス製のチューブに嵌合し、同一軸上に固定し、片端部から反対端部へ向けて、外部火炎加熱源を移動させながら、外層チューブ内面と内層チューブ外面の全面を溶接し、外層天然石英ガラス層と内層合成ガラス層からなる複合石英ガラス管を作成した。この複合石英ガラス管の外表面より深さ０．１ｍｍまでには、アルミニウムが０．１ｗｔ％ドープされているのが検知された。
Example 1
Natural quartz glass having an impurity content of Al: 8 ppm, Fe: 0.2 ppm, Na: 0.1 ppm, K: 0.1 ppm, OH group concentration: 200 ppm, and viscosity at 1,280 ° C. of 10 12.4 poise A natural quartz glass tube having a size of 300 mmφ × 1500 mmL × 3 mmt was prepared using a 30 mm diameter, and a 30% aluminum nitrate solution was applied to the outer surface of the tube, followed by drying. On the other hand, the impurity content is Al: 0.001 ppm, Fe: 0.001 ppm, Na: 0.001 ppm, K: 0.001 ppm, OH concentration: 80 ppm, Cl concentration: 25 ppm, and the viscosity at 1,280 ° C. is 10 A synthetic quartz glass tube having a size of 275 mmφ × 1500 mmL × 1 mmt is prepared using 11.8 poise synthetic quartz glass, and this synthetic quartz glass tube is fitted to the natural quartz glass tube and fixed on the same axis. While moving the external flame heating source from one end to the opposite end, the entire inner surface of the outer tube and the outer surface of the inner tube are welded to form a composite quartz glass tube composed of an outer natural quartz glass layer and an inner synthetic glass layer. Created. It was detected that 0.1 wt% aluminum was doped to a depth of 0.1 mm from the outer surface of the composite quartz glass tube.
上記複合石英ガラス管を使って、炉芯菅を作成し、作成した炉芯菅内でシリコンウエーハを、アルゴン雰囲気下で、室温から１,２００℃で、３０分間保持して加熱した後、室温まで放冷する加熱サイクルをそれぞれ２００回繰り返し行った。加熱サイクル後のシリコンウエーハの金属不純物量は、１００ｐｐｂであった。炉芯菅は、外表面部に厚さ０．２ｍｍの失透層が形成された以外は、使用開始前と変化は無く、変形も無かった。 Using the above composite quartz glass tube, a furnace core was prepared, and the silicon wafer was heated from room temperature to 1,200 ° C. in an argon atmosphere for 30 minutes and then heated to room temperature. Each heating cycle for cooling was repeated 200 times. The amount of metal impurities in the silicon wafer after the heating cycle was 100 ppb. The furnace core was the same as before the start of use and was not deformed except that a devitrification layer having a thickness of 0.2 mm was formed on the outer surface.
実施例２
不純物含有量が、Ａｌ：８ｐｐｍ、Ｆｅ：０．２ｐｐｍ、Ｎａ：０．１ｐｐｍ、Ｋ：０．１ｐｐｍで、OH基濃度：２００ｐｐｍ、１,２８０℃における粘度が１０１２．４ポイズの天然石英ガラスを用いてサイズ３００mmφ×１５００mmＬ×３mmｔの天然石英ガラスチューブを作成し、その外表面に、硝酸アルミニウムの３０％溶液を塗布したのち乾燥させた。一方、不純物含有量が、Ａｌ：０．００１ｐｐｍ、Ｆｅ：０．００１ｐｐｍ、Ｎａ：０．００１ｐｐｍ、Ｋ：０．００１ｐｐｍ、ＯＨ濃度：０．１ｐｐｍ、Ｃｌ濃度：１ｐｐｍで、波長２４５ｎｍにおける吸収係数が０．４／ｃｍの１,２８０℃における粘度が１０１２．１ポイズである合成石英ガラスを用いてサイズ２７５mmφ×１５００mmＬ×１mmｔの合成石英ガラスチューブを作成し、この合成石英ガラスチューブを前記天然石英ガラス製のチューブに嵌合し、同一軸上に固定し、片端部から反対端部へ向けて、外部火炎加熱源を移動させながら、外層チューブ内面と内層チューブ外面の全面を溶接し、外層天然石英ガラス層と内層合成ガラス層からなる複合石英ガラス管を作成した。この複合石英ガラス管の外表面より深さ０．１ｍｍまでには、アルミニウムが０．１ｗｔ％ドープされているのが検知された。
Example 2
Natural quartz glass having an impurity content of Al: 8 ppm, Fe: 0.2 ppm, Na: 0.1 ppm, K: 0.1 ppm, OH group concentration: 200 ppm, viscosity at 1,280 ° C. of 10 12.4 poise A natural quartz glass tube having a size of 300 mmφ × 1500 mmL × 3 mmt was prepared using a 30 mm diameter, and a 30% aluminum nitrate solution was applied to the outer surface of the tube, followed by drying. On the other hand, the impurity content is Al: 0.001 ppm, Fe: 0.001 ppm, Na: 0.001 ppm, K: 0.001 ppm, OH concentration: 0.1 ppm, Cl concentration: 1 ppm, and the absorption coefficient at a wavelength of 245 nm. 0.4 / viscosity at 1,280 ° C. for cm creates a synthetic quartz glass tube size 275mmφ × 1500mmL × 1mmt using synthetic quartz glass is 10 12.1 poise, the natural quartz this synthetic quartz glass tube Fitted to a glass tube, fixed on the same axis, and while moving the external flame heat source from one end to the opposite end, weld the entire inner surface of the outer tube and the outer surface of the inner tube, A composite quartz glass tube composed of a British glass layer and an inner synthetic glass layer was prepared. It was detected that 0.1 wt% aluminum was doped to a depth of 0.1 mm from the outer surface of the composite quartz glass tube.
上記複合石英ガラス管を使って、炉芯菅を作成し、作成した炉芯菅内でシリコンウエーハを、アルゴン雰囲気下で、室温から１,２００℃で、３０分間保持して加熱した後、室温まで放冷する加熱サイクルをそれぞれ２００回繰り返し行った。加熱サイクル後のシリコンウエーハの金属不純物量は、１００ｐｐｂであった。炉芯菅は、外表面部に厚さ０．２ｍｍの失透層が形成された以外は、使用開始前と変化は無く、変形も無かった。 Using the above composite quartz glass tube, a furnace core was prepared, and the silicon wafer was heated from room temperature to 1,200 ° C. in an argon atmosphere for 30 minutes and then heated to room temperature. Each heating cycle for cooling was repeated 200 times. The amount of metal impurities in the silicon wafer after the heating cycle was 100 ppb. The furnace core was the same as before the start of use and was not deformed except that a devitrification layer having a thickness of 0.2 mm was formed on the outer surface.
比較例１
不純物濃度が、Ａｌ：８ｐｐｍ、Ｆｅ：０．２ｐｐｍ、Ｎａ：０．１ｐｐｍ、Ｋ：０．１ｐｐｍ、OH濃度２００ｐｐｍで、１,２８０℃における粘度が１０１２．４ポイズの天然石英ガラスを用いて３００mmφ×１５００mmＬ×３mmｔサイズの石英ガラスチューブを作成する一方、不純物濃度が、Ａｌ：０．００１ｐｐｍ、Ｆｅ：０．００１ｐｐｍ、Ｎａ：０．００１ｐｐｍ、Ｋ：０．００１ｐｐｍ、ＯＨ濃度１２００ｐｐｍ、Ｃｌ濃度６００ｐｐｍで、１２８０℃における粘度が１０１１．５ポイズの合成石英ガラスを用いて２７５mmφ×１５００mmＬ×１mmｔサイズの合成石英ガラスチューブを作成し、この合成石英ガラスチューブを前記天然石英ガラスチューブに嵌合し、同一軸上に固定し、片端部から反対端部へ向けて、外部火炎加熱源を移動させながら、外層チューブ内面と内層チューブ外面の全面を溶接し、外部天然石英ガラス層と内部合成ガラス層からなる、複合石英ガラス管を作成した。
Comparative Example 1
Using natural quartz glass having an impurity concentration of Al: 8 ppm, Fe: 0.2 ppm, Na: 0.1 ppm, K: 0.1 ppm , OH concentration of 200 ppm and a viscosity at 1,280 ° C. of 10 12.4 poise While producing a quartz glass tube of 300 mmφ × 1500 mmL × 3 mmt size, the impurity concentration is Al: 0.001 ppm, Fe: 0.001 ppm, Na: 0.001 ppm, K: 0.001 ppm, OH concentration 1200 ppm, Cl concentration 600 ppm. Then, a synthetic quartz glass tube having a size of 275 mmφ × 1500 mmL × 1 mmt is prepared using a synthetic quartz glass having a viscosity at 1280 ° C. of 10 11.5 poise, and this synthetic quartz glass tube is fitted to the natural quartz glass tube, Fix on the same axis and move the external flame heating source from one end to the opposite end. While moving, the entire inner surface of the outer tube and the outer surface of the inner tube were welded to form a composite quartz glass tube composed of an outer natural quartz glass layer and an inner synthetic glass layer.
得られた複合石英ガラス管を使って、炉芯菅を作成し、作成した炉芯管内でシリコンウエーハを、アルゴン雰囲気下で、室温から１,２００℃で、３０分間保持して加熱した後、室温まで放冷する加熱サイクルをそれぞれ２００回繰り返し行った。加熱サイクル後のシリコンウエーハの金属不純物量は、１,０００ｐｐｂであった。そして、炉芯管はひどく変形しこれ以上の使用継続は不可能であった。 Using the resulting composite quartz glass tube, a furnace core rod was prepared, and after heating the silicon wafer in the prepared furnace core tube from room temperature to 1,200 ° C. for 30 minutes in an argon atmosphere, Each heating cycle for cooling to room temperature was repeated 200 times. The amount of metal impurities in the silicon wafer after the heating cycle was 1,000 ppb. The furnace core tube was deformed so much that it was impossible to continue using it.
本発明は、高純度で、耐熱性が高く、半導体を長時間、高温処理しても形状変化がない上に、金属不純物、特にアルカリ金属不純物の遮蔽効果が高く、処理する半導体に高品質で生成性がよく処理でき工業的に有用な石英ガラス管である。
The present invention has high purity, high heat resistance, no change in shape even if the semiconductor is processed at high temperature for a long time, and has a high shielding effect against metal impurities, particularly alkali metal impurities. It is a quartz glass tube that can be processed well and is industrially useful.
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| KR20180095879A (en) | 2015-12-18 | 2018-08-28 | 헤래우스 크바르츠글라스 게엠베하 ＆ 컴파니 케이지 | Treating the carbon-doped silica granules at elevated temperatures to reduce the alkaline earth metal content of the silica granules |
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| KR20180095622A (en) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 ＆ 컴파니 케이지 | Manufacture of Silica Glass Products from Molten Crucibles Made of Refractory Metals |
| EP3390296B1 (en) | 2015-12-18 | 2024-09-04 | Heraeus Quarzglas GmbH & Co. KG | Production of a quartz glass body in a multichamber furnace |
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