JP4813400B2 - Method for etching quartz glass member - Google Patents
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- JP4813400B2 JP4813400B2 JP2007048232A JP2007048232A JP4813400B2 JP 4813400 B2 JP4813400 B2 JP 4813400B2 JP 2007048232 A JP2007048232 A JP 2007048232A JP 2007048232 A JP2007048232 A JP 2007048232A JP 4813400 B2 JP4813400 B2 JP 4813400B2
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- quartz glass
- etching
- glass member
- resin
- coating layer
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- 238000005530 etching Methods 0.000 title claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 30
- 238000000034 method Methods 0.000 title claims description 26
- 239000011347 resin Substances 0.000 claims description 53
- 229920005989 resin Polymers 0.000 claims description 53
- 239000011247 coating layer Substances 0.000 claims description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 15
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- 150000001735 carboxylic acids Chemical class 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 3
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000003486 chemical etching Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910021488 crystalline silicon dioxide Inorganic materials 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 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
- 239000000758 substrate Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Surface Treatment Of Glass (AREA)
Description
本発明は、不透明部と透明平滑部とが任意の位置に形成され、半導体処理用部材を形成するためのエッチング方法に関する。 The present invention relates to an etching method for forming a semiconductor processing member in which an opaque portion and a transparent smooth portion are formed at arbitrary positions.
従来、表面に凹凸が形成された不透明石英ガラスは、半導体熱処理治具の把持部の形成材料として、また半導体ウエーハの気相成長膜生成処理（Chemical Vapor Deposition）時のポリシリコン膜や炭化珪素膜の剥離を防止する部材としても用いられてきた。前記不透明石英ガラスの製造方法としては、サンドブラスト法や化学的エッチング法などが挙げられるが、サンドブラスト法では石英ガラス部材に結晶質二酸化珪素粉等の無機粒子を吹き付け機械的に削り取ることから、形成した表面の凹凸の下にマイクロクラック層が発生し、機械的強度を低下させる上に、ＣＶＤ工程等で使用を継続するに従ってパーティクルを発生する場合があり、それが半導体ウエーハを汚染する問題があった。その一方、化学的エッチング法による不透明化でマイクロクラック層は発生しないが、部材全体がエッチング液に浸漬されることから部材全体が不透明化されガスシール性が要求される部分が損なわれ、例えばＣＶＤ工程で使用すると真空吸引時やガス反応時に影響を受け、プロセスが一定化しない問題があった。 Conventionally, opaque quartz glass with irregularities formed on its surface has been used as a material for forming the gripping part of semiconductor heat treatment jigs, and as a polysilicon film or silicon carbide film during semiconductor wafer vapor deposition (Chemical Vapor Deposition). It has also been used as a member for preventing peeling. Examples of the method for producing the opaque quartz glass include a sand blasting method and a chemical etching method. In the sand blasting method, inorganic particles such as crystalline silicon dioxide powder are sprayed on the quartz glass member and mechanically scraped off. A microcrack layer is generated under the surface irregularities, and in addition to lowering the mechanical strength, there are cases where particles are generated as the use is continued in the CVD process and the like, which has a problem of contaminating the semiconductor wafer. . On the other hand, although the microcrack layer is not generated by the opacity by the chemical etching method, the entire member is immersed in the etching solution, so that the entire member is made opaque and the portion requiring gas sealability is impaired. When used in the process, there was a problem that the process was not stabilized due to the influence of vacuum suction or gas reaction.
その一方、石英ガラスを初めとするガラス基板の表面に部分的に凹凸を形成する方法として、部材表面にマスク材を被覆し、露出部をエッチング処理する方法が例えば特許文献１などで提案されている。そして、前記マスク材として、ポリエチレンなどの耐薬品性に優れた樹脂シートの使用も特許文献２などで提案されている。しかし、この樹脂シートを用いる処理方法では部材とシート間の密着性が十分でなくエッチング液がその隙間から浸み込み不規則な凹凸が形成される問題があった。
こうした現状に鑑み、本発明者は鋭意研究した結果、石英ガラス部材を耐薬品性に優れ、且つ熱収縮性のある樹脂で部材の透明で平滑さを要する部分を被い、加熱処理して樹脂被覆層を形成することで、部材と樹脂被覆層との密着性が優れている上に、エッチング液の浸み込みがなく、所望の位置に良好な凹凸を形成できることを見出した。さらに、部材表面に第１の熱収縮性樹脂被覆層を形成したのち、第１の樹脂被覆層より１〜５mm大きい第２の樹脂被覆層が形成できるように熱収縮性樹脂を被せ、加熱処理することで任意の位置の不透明部と透明部とを有する石英ガラス治具が容易に製造できることをも見出して本発明を完成したものです。すなわち
本発明は、任意の位置に不透明部と透明平滑部とを有する石英ガラス部材を製造するエッチング方法を提供することを目的とする。
In view of the current situation, the present inventor has intensively studied, and as a result, the quartz glass member is a resin having excellent chemical resistance and heat shrinkability, covering a transparent and smooth part of the member, and heat-treating the resin. It has been found that by forming the coating layer, the adhesiveness between the member and the resin coating layer is excellent, and the etching solution does not penetrate and favorable irregularities can be formed at a desired position. Further, after forming the first heat-shrinkable resin coating layer on the surface of the member, the heat-shrinkable resin is covered so that a second resin coating layer 1 to 5 mm larger than the first resin coating layer can be formed, and heat treatment is performed. As a result, it was found that a quartz glass jig having an opaque part and a transparent part at an arbitrary position can be easily manufactured, and the present invention has been completed. That is, an object of the present invention is to provide an etching method for producing a quartz glass member having an opaque part and a transparent smooth part at an arbitrary position.
上記目的を達成する本発明は、石英ガラス部材のエッチング方法において、石英ガラス部材の外表面の少なくとも一部にチューブ状の熱収縮性樹脂を被せ、熱収縮させて樹脂被覆層を形成したのち、フッ化水素を主成分とするエッチング液で処理し、次いで前記樹脂被覆層を剥離することを特徴とする石英ガラス部材のエッチング方法に係る。 The present invention that achieves the above object is the method for etching a quartz glass member, wherein at least a part of the outer surface of the quartz glass member is covered with a tube-shaped heat-shrinkable resin and thermally contracted to form a resin coating layer. In addition, the present invention relates to a method for etching a quartz glass member, characterized by treating with an etching solution containing hydrogen fluoride as a main component and then peeling off the resin coating layer .
本発明の石英ガラス部材のエッチング方法では、上述のとおり耐薬品性に優れ、かつチューブ状の熱収縮性の樹脂を石英ガラス部材の一部に被せ、加熱収縮させて樹脂被覆層を形成したのち、フッ化水素を主成分とするエッチング液で処理し、洗浄し、樹脂被覆層を剥離することでエッチング液の浸み込みがなく、任意の位置に均一な微細な凹凸を有する部材が容易に製造できる。前記石英ガラス部材としては、半導体ウエーハの製造に用いられる半導体熱処理装置用部材、ガス反応を行うためのベルジャー等の容器などが挙げられるが、これらの部材は概ね円筒又はチューブ形状であるので、それに被せる熱収縮性樹脂はチューブ状に成形して用いる。前記熱収縮性樹脂としては、ポリオレフィン、ポリ塩化ビニル、フッ素樹脂等が挙げられる。樹脂被覆された石英ガラス部材は、次いでフッ化水素を主成分とするエッチング液で処理されるが、樹脂被覆層は２層構造以上としエッチング液の浸み込みを防ぐのがよい。より好ましくは、２層目の樹脂被覆層を最初の樹脂被覆層の端部より１〜５mm長くなるように熱収縮性樹脂を被せ、加熱収縮させるのがよい。樹脂被覆する前の部材の部材外表面と熱収縮性樹脂内面との隙間は０．５〜４mm程度であり、また樹脂被覆膜の厚さは０．０５〜４mm程度となる。前記範囲の樹脂被覆膜層を有することでエッチング液が例え樹脂被覆層に浸み込むことがあっても第２層の樹脂被覆層にとどまり、第１層の樹脂被覆層は完全に保護され任意の位置に不透明部と透明部とが形成できる。 In the method for etching a quartz glass member according to the present invention, as described above, a resin-coated layer is formed by covering a part of the quartz glass member with excellent chemical resistance and having a tubular heat-shrinkable resin, followed by heat shrinkage. By treating with an etchant containing hydrogen fluoride as a main component, washing, and peeling off the resin coating layer, there is no penetration of the etchant, and a member having uniform fine irregularities at any position can be easily obtained. Can be manufactured. Examples of the quartz glass member include a semiconductor heat treatment apparatus member used for manufacturing a semiconductor wafer, and a vessel such as a bell jar for performing a gas reaction. heat-shrinkable resin covering the Ru used by forming into a tubular shape. Examples of the heat-shrinkable resin include polyolefin, polyvinyl chloride, and fluororesin. The resin-coated quartz glass member is then treated with an etching solution containing hydrogen fluoride as a main component, but the resin coating layer should have a two-layer structure or more to prevent penetration of the etching solution. More preferably, the second resin coating layer is covered with a heat-shrinkable resin so as to be 1 to 5 mm longer than the end portion of the first resin coating layer, and is heat-shrinked. The gap between the member outer surface and the heat-shrinkable resin inner surface of the member before resin coating is about 0.5 to 4 mm, and the thickness of the resin coating film is about 0.05 to 4 mm. By having the resin coating film layer in the above-mentioned range, even if the etching solution may penetrate into the resin coating layer, it remains in the second resin coating layer, and the first resin coating layer is completely protected. An opaque part and a transparent part can be formed at an arbitrary position.
上記エッチング液としては、フッ化水素を主成分とするが、さらにフッ化アンモニウムと有機カルボン酸、好ましくは酢酸を含有してもよい。前記エッチング液がフッ化アンモニウムを含有する場合、フッ化水素及びフッ化アンモニウムの合計含有量は１０〜４０重量％、フッ化水素とフッ化アンモニウムのモル比は、フッ化水素：フッ化アンモニウム＝０．５：１〜２：１の範囲がよい。また、有機カルボン酸は２０〜７５重量％の範囲で含有される。有機カルボン酸としては、蟻酸、安息香酸などのモノカルボン酸、蓚酸のようなジカルボン酸などが挙げられるが、酢酸が特に好適である。この有機カルボン酸を含有することでエッチング液は安定する上に、含有量を調節することで任意の大きさの凹凸を形成することができる。エッチング処理液の調整方法としては、フッ化水素、フッ化アンモニウム、水、必要に応じて有機カルボン酸を均一に混合する方法、フッ化水素、フッ化アンモニウム及び水に混合した主液にその使用時に有機カルボン酸からなる補助剤を混合する方法などが挙げられる。 The etching solution contains hydrogen fluoride as a main component, but may further contain ammonium fluoride and an organic carboxylic acid, preferably acetic acid. When the etching solution contains ammonium fluoride, the total content of hydrogen fluoride and ammonium fluoride is 10 to 40% by weight, and the molar ratio of hydrogen fluoride to ammonium fluoride is hydrogen fluoride: ammonium fluoride = A range of 0.5: 1 to 2: 1 is preferable. The organic carboxylic acid is contained in the range of 20 to 75% by weight. Examples of the organic carboxylic acid include monocarboxylic acids such as formic acid and benzoic acid, and dicarboxylic acids such as oxalic acid. Acetic acid is particularly preferable. By containing this organic carboxylic acid, the etching solution is stabilized, and irregularities of an arbitrary size can be formed by adjusting the content. Etching treatment liquid adjustment method includes hydrogen fluoride, ammonium fluoride, water, and a method of uniformly mixing organic carboxylic acid as required, and its use in main liquid mixed with hydrogen fluoride, ammonium fluoride and water. The method of mixing the adjuvant which consists of organic carboxylic acid sometimes is mentioned.
本発明では、石英ガラス部材の外表面の少なくとも一部にチューブ状の熱収縮性樹脂を被せ、熱収縮させて樹脂被覆層を形成したのち、フッ化水素を主成分とするエッチング液で処理し、前記樹脂被覆層を除去することで、樹脂被覆層へのエッチング液の浸み込みがなく、石英ガラス部材の任意の位置に均一な微細な凹凸が形成できる。
In the present invention, at least a part of the outer surface of the quartz glass member is covered with a tube-shaped heat-shrinkable resin, heat-shrinked to form a resin coating layer, and then treated with an etching solution mainly containing hydrogen fluoride. and, wherein by removing the resin coating layer, there is no lump immersion only the etching solution into the resin coating layer, a uniform fine irregularities on any position of the quartz glass member is cut with formation.
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
直径１２mm石英ガラス製インジェクターの根元部分に直径１４mm、肉厚０．３mmのポリエチレン製熱収縮性チューブ（住友電工ファインポリマー社製、商品名スミチューブＡ）をインジェクターの端部から５２mmの長さに被せ熱収縮させた。得られた樹脂被覆インジェクターにさらに直径１４mmの前述のポリエチレン製熱収縮性チューブを１層目より被覆長さが３mm長くなるように被せ加熱処理した。得られた２層樹脂被覆インジェクターをフッ化水素１５重量％、フッ化アンモニウム１５重量％、酢酸３５重量％を含むエッチング処理液に常温で３０分浸漬しエッチング処理した。処理後部材を純水で洗浄し、被覆樹脂を剥がした。２層樹脂被膜には３mmまでエッチング液が浸み込んでいたが１層目の被覆樹脂部にはエッチング液の浸み込みがなかった。得られた部材には均一な微細な凹凸が形成されていた。
Example 1
Cover the base of the 12 mm diameter quartz glass injector with a polyethylene heat-shrinkable tube (Sumitomo Electric Fine Polymer, trade name Sumitube A) with a diameter of 14 mm and a wall thickness of 0.3 mm from the end of the injector to a length of 52 mm. Heat-shrinked. The obtained resin-coated injector was further heat-treated by covering the above-mentioned polyethylene heat-shrinkable tube having a diameter of 14 mm with a coating length of 3 mm longer than the first layer. The obtained two-layer resin-coated injector was immersed in an etching solution containing 15% by weight of hydrogen fluoride, 15% by weight of ammonium fluoride, and 35% by weight of acetic acid at room temperature for 30 minutes. After the treatment, the member was washed with pure water, and the coating resin was peeled off. The etching solution soaked up to 3 mm in the two-layer resin coating, but the etching solution did not soak into the first-layer coating resin portion. Uniform fine irregularities were formed on the obtained member.
比較例１
実施例１の石英ガラス製インジェクターの根元部分にテトラフルオロエチレン樹脂製のシールテープを貼り、実施例１と同じエッチング処理液に浸漬したところ、シールテープの半分以上にエッチング液の浸み込みがあった。
Comparative Example 1
When a tetrafluoroethylene resin seal tape was applied to the base of the quartz glass injector of Example 1 and immersed in the same etching treatment solution as in Example 1, more than half of the seal tape had infiltrated the etchant. It was.
比較例２
比較例１においてシールテープを貼り付ける代わりに加熱し溶解したワックス溶液を塗布し、冷却固化した以外、比較例１と同様にしてエッチング処理を行った。塗布したワックスは溶解し、エッチング処理液がワックスの色を呈した。
Comparative Example 2
Etching was performed in the same manner as in Comparative Example 1 except that a wax solution dissolved by heating was applied instead of sticking the seal tape in Comparative Example 1, and the solution was cooled and solidified. The applied wax was dissolved, and the etching solution exhibited a wax color.
本発明のエッチング方法では部材に不透明部とガスシール性に優れた透明平滑部とが任意に形成でき、半導体ウエーハの熱処理用部材や気相反応用部材として有用な石英ガラス部材が簡便に製造できる。 In the etching method of the present invention, an opaque portion and a transparent smooth portion excellent in gas sealability can be arbitrarily formed on the member, and a quartz glass member useful as a heat treatment member or a gas phase reaction member of a semiconductor wafer can be easily produced.
Claims (6)
ガラス部材のエッチング方法。 The quartz glass member according to any one of claims 1 to 3, wherein the tubular heat-shrinkable resin is one kind of heat-shrinkable resin selected from polyolefin, polyvinyl chloride, and fluororesin. Etching method.
ラス部材のエッチング方法。 The method for etching a quartz glass member according to any one of claims 1 to 3, wherein the etching solution containing hydrogen fluoride as a main component contains hydrogen fluoride, ammonium fluoride, and an organic carboxylic acid.
6. The method for etching a quartz glass member according to claim 5, wherein the organic carboxylic acid is acetic acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007048232A JP4813400B2 (en) | 2007-02-28 | 2007-02-28 | Method for etching quartz glass member |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007048232A JP4813400B2 (en) | 2007-02-28 | 2007-02-28 | Method for etching quartz glass member |
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| JP2008208007A JP2008208007A (en) | 2008-09-11 |
| JP4813400B2 true JP4813400B2 (en) | 2011-11-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS491609A (en) * | 1972-04-18 | 1974-01-09 | ||
| JPS58185453A (en) * | 1982-04-23 | 1983-10-29 | Nippon Electric Glass Co Ltd | Working method of glass pipe |
| JP4437365B2 (en) * | 2000-09-28 | 2010-03-24 | 信越石英株式会社 | Silica glass jig for semiconductor industry and manufacturing method thereof |
| JP2004339036A (en) * | 2003-05-19 | 2004-12-02 | Nishiyama Stainless Chem Kk | High-strength glass plate and method for toughening glass |
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