JP6288636B2 - Corrosion resistant parts for precision machinery - Google Patents
Corrosion resistant parts for precision machinery Download PDFInfo
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- JP6288636B2 JP6288636B2 JP2013232536A JP2013232536A JP6288636B2 JP 6288636 B2 JP6288636 B2 JP 6288636B2 JP 2013232536 A JP2013232536 A JP 2013232536A JP 2013232536 A JP2013232536 A JP 2013232536A JP 6288636 B2 JP6288636 B2 JP 6288636B2
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- fluororesin
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- 230000007797 corrosion Effects 0.000 title claims description 55
- 238000005260 corrosion Methods 0.000 title claims description 55
- 239000003575 carbonaceous material Substances 0.000 claims description 45
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 32
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 23
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000004065 semiconductor Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 36
- 238000000034 method Methods 0.000 description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 30
- 239000010410 layer Substances 0.000 description 30
- 238000011156 evaluation Methods 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 238000011109 contamination Methods 0.000 description 11
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000000576 coating method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 125000001153 fluoro group Chemical group F* 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 230000005856 abnormality Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 238000005422 blasting Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 2
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Paints Or Removers (AREA)
Description
本発明は、精密機械用耐食性部材に関し、より詳しくは、炭素材料にフッ素樹脂をコーティングした耐食性部材を使用することにより、金属コンタミネーションが発生することなく、強度があり加工が容易な精密機械用耐食性部材に関する。 TECHNICAL FIELD The present invention relates to a corrosion-resistant member for precision machinery, and more particularly, for a precision machine that is strong and easy to process without the occurrence of metal contamination by using a corrosion-resistant member obtained by coating a carbon material with a fluororesin. The present invention relates to a corrosion resistant member.
電子部品の製造工程には材料の研磨、洗浄、加熱等の工程が含まれており、通常、これらの処理工程に用いられる製造装置には、金属又は石英で主に構成された部材が使用される。 The manufacturing process of electronic parts includes processes such as polishing, cleaning, and heating of materials. Usually, members mainly composed of metal or quartz are used in manufacturing apparatuses used in these processing processes. The
例えば、特許文献１には半導体又は平板ディスプレイ等の製造装置の処理室内壁等への反応生成物堆積、内壁等の腐食による金属汚染、放出ガスによるプロセスのゆらぎなどを抑制した複数のプロセスを可能にする多機能製造装置システムおよびそれに用いる保護皮膜構造が開示されている。
具体的には、金属材料の表面に、下地層として母材の直接酸化により形成した１μｍ以下の膜厚の酸化物皮膜を有する第１皮膜層を有し、さらに２００μｍ程度の第２皮膜層を形成し、第２皮膜層はプラズマ溶射法により形成した酸化アルミニウム、酸化イットリウム、酸化マグネシウムおよびこれらの混晶、ＮｉＰメッキ、Ｎｉメッキ、Ｃｒメッキ、フッ素樹脂皮膜のうち少なくともひとつから成ることが開示されており、これにより母材金属表面を腐食させることを防ぎ、金属汚染を低減させることができると記載されている（特許文献１要約参照）。
For example, Patent Document 1 enables a plurality of processes in which reaction product deposition on the inner wall of a processing chamber of a manufacturing apparatus such as a semiconductor or flat panel display, metal contamination due to corrosion of the inner wall, etc., and process fluctuations due to released gas are suppressed. A multi-function manufacturing apparatus system and a protective film structure used therefor are disclosed.
Specifically, the surface of the metal material has a first film layer having an oxide film with a thickness of 1 μm or less formed by direct oxidation of a base material as a base layer, and further a second film layer of about 200 μm is formed. It is disclosed that the second coating layer is composed of at least one of aluminum oxide, yttrium oxide, magnesium oxide and mixed crystals thereof, NiP plating, Ni plating, Cr plating, and fluororesin coating formed by plasma spraying. Thus, it is described that the base metal surface can be prevented from being corroded and metal contamination can be reduced (see abstract of Patent Document 1).
しかし、表面をコーティングしていても金属で主に構成された部材を使用すると、温度変化や強酸性または強アルカリ性の薬剤によって内壁面等が腐食することによる金属コンタミネーションが発生する可能性があるという問題点がある。電子部品を製造する際には、高い清浄レベルが要求される。特に半導体はコンタミネーションに弱く、可能な限り清浄な環境で製造することが望ましい。 However, if a member mainly composed of metal is used even if the surface is coated, there is a possibility that metal contamination will occur due to corrosion of the inner wall surface or the like due to temperature change or strong acidic or strong alkaline chemicals. There is a problem. When manufacturing electronic components, a high cleaning level is required. In particular, semiconductors are vulnerable to contamination, and it is desirable to manufacture them in as clean an environment as possible.
また、特許文献２には半導体の製造で使用する超音波洗浄用石英ガラス槽及びその製造方法、並びに該超音波洗浄用石英ガラス槽を用いた洗浄方法が開示されている。
具体的には、石英ガラス槽の表面全体を膜厚１０μｍ〜５ｍｍのフッ素系樹脂皮膜で覆われていることを特徴とする超音波洗浄用石英ガラス槽が開示されており、超音波が透過し良好な洗浄が行えることが記載されている。
Patent Document 2 discloses a quartz glass tank for ultrasonic cleaning used in the manufacture of semiconductors, a method for manufacturing the same, and a cleaning method using the quartz glass tank for ultrasonic cleaning.
Specifically, there is disclosed a quartz glass tank for ultrasonic cleaning characterized in that the entire surface of the quartz glass tank is covered with a fluorine resin film having a film thickness of 10 μm to 5 mm, and the ultrasonic wave is transmitted. It describes that good cleaning can be performed.
しかし、石英で主に構成された部材を使用することで金属コンタミネーションは発生しなくなるものの、金属部材に比べて加工しにくいため、様々な形態の精密機械に加工できないという問題点がある。また、金属部材に比べて強度が低いため、耐久性が低いという問題点もある。 However, although metal contamination does not occur by using a member mainly composed of quartz, it is difficult to process compared to a metal member, so that it cannot be processed into various forms of precision machines. In addition, since the strength is lower than that of the metal member, there is a problem that durability is low.
本発明は、上記した従来技術の問題点を解決すべくなされたものであって、炭素材料にプライマー層を介してフッ素樹脂皮膜を設けることで、金属コンタミネーションが発生しない、強度があって加工が容易な精密機械用耐食性部材を提供するものである。 The present invention has been made to solve the above-mentioned problems of the prior art, and by providing a fluororesin film on a carbon material through a primer layer, metal contamination does not occur, and processing is performed with strength. It is an object of the present invention to provide a corrosion resistant member for precision machinery that is easy to handle.
請求項１に係る発明は、炭素材料と、前記炭素材料上に形成されたプライマー層と、前記プライマー層上に形成されたフッ素樹脂皮膜とを有し、前記炭素材料が等方性黒鉛からなり、前記プライマー層がチタネート系プライマーまたはクロム酸系プライマーからなることを特徴とする精密機械用耐食性部材に関する。
The invention according to claim 1 includes a carbon material, a primer layer formed on the carbon material, and a fluororesin film formed on the primer layer, and the carbon material is made of isotropic graphite. Further, the present invention relates to a corrosion-resistant member for precision machinery , wherein the primer layer comprises a titanate primer or a chromic acid primer.
請求項２に係る発明は、前記プライマー層がチタネート系プライマーからなることを特徴とする請求項１記載の精密機械用耐食性部材に関する。 The invention according to claim 2 relates to the corrosion resistant member for precision machinery according to claim 1, wherein the primer layer is composed of a titanate primer.
請求項３に係る発明は、前記クロム酸系プライマーがフッ素樹脂とクロム酸及びリン酸を含む混合液であることを特徴とする請求項１記載の精密機械用耐食性部材に関する。 The invention according to claim 3 relates to the corrosion resistant member for precision machinery according to claim 1, wherein the chromic acid primer is a mixed solution containing a fluororesin, chromic acid and phosphoric acid.
請求項４に係る発明は、前記チタネート系プライマーがチタニウムジイソプロポキシビス（トリエタノールアミネート）とフッ素樹脂の混合物であることを特徴とする請求項１または２記載の精密機械用耐食性部材に関する。 The invention according to claim 4 relates to the corrosion resistant member for precision machinery according to claim 1 or 2, wherein the titanate primer is a mixture of titanium diisopropoxybis (triethanolaminate) and a fluororesin.
請求項５に係る発明は、前記精密機械が半導体製造装置であることを特徴とする請求項１乃至４のいずれかに記載の精密機械用耐食性部材に関する。 The invention according to claim 5 relates to the corrosion-resistant member for precision machine according to any one of claims 1 to 4, wherein the precision machine is a semiconductor manufacturing apparatus.
請求項６に係る発明は、前記精密機械が熱交換器であることを特徴とする請求項１乃至４のいずれかに記載の精密機械用耐食性部材に関する。 The invention according to claim 6 relates to the corrosion-resistant member for precision machine according to any one of claims 1 to 4, wherein the precision machine is a heat exchanger.
請求項１に係る発明によれば、炭素材料を基材として用いることで加工が容易になるため、様々な形状の精密機械用部材として使用することができ、金属コンタミネーションが発生しない精密機械とすることができる。
また、炭素材料上にフッ素樹脂皮膜をコーティングした耐食性部材を精密機械において使用することで強度が増し、部材の腐食を抑えることができる。
さらに、炭素材料とフッ素樹脂皮膜の間にプライマー層を設けることで、炭素材料とフッ素樹脂皮膜との密着性を強くし、フッ素樹脂皮膜の剥離を防ぐことができる。
また、炭素材料とフッ素樹脂皮膜の間にチタネート系プライマーまたはクロム酸系プライマーからなるプライマー層を設けることで、炭素材料とフッ素樹脂皮膜との密着性をより強くし、フッ素樹脂皮膜の剥離を防ぐことができる。
According to the first aspect of the present invention, since the processing is facilitated by using the carbon material as the base material, it can be used as a member for precision machines of various shapes, and the precision machine does not generate metal contamination. can do.
In addition, the use of a corrosion-resistant member obtained by coating a carbon material with a fluororesin film in a precision machine increases the strength and suppresses corrosion of the member.
Furthermore, by providing a primer layer between the carbon material and the fluororesin film, the adhesion between the carbon material and the fluororesin film can be strengthened, and peeling of the fluororesin film can be prevented.
In addition, by providing a primer layer made of titanate primer or chromic acid primer between the carbon material and the fluororesin film, the adhesion between the carbon material and the fluororesin film is further strengthened, and the fluororesin film is prevented from peeling off. be able to.
請求項２に係る発明によれば、炭素材料とフッ素樹脂皮膜の間にチタネート系プライマーからなるプライマー層を設けることで、炭素材料とフッ素樹脂皮膜との密着性をより強くし、フッ素樹脂皮膜の剥離を防ぐことができる。また、チタネート系プライマーは毒性が低いため、環境に対して悪影響を及ぼすことを防止することができる。 According to the invention of claim 2, by providing a primer layer composed of a titanate primer between the carbon material and the fluororesin film, the adhesion between the carbon material and the fluororesin film is further increased, Peeling can be prevented. In addition, since titanate-based primers have low toxicity, they can prevent adverse effects on the environment.
請求項３に係る発明によれば、クロム酸系プライマーとしてフッ素樹脂とクロム酸及びリン酸を含む混合液からなるプライマー層を設けることで、密着性をより強くすることができる。 According to the invention which concerns on Claim 3, adhesiveness can be strengthened more by providing the primer layer which consists of a liquid mixture containing a fluororesin, chromic acid, and phosphoric acid as a chromic acid system primer.
請求項４に係る発明によれば、チタネート系プライマーとしてチタニウムジイソプロポキシビス（トリエタノールアミネート）とフッ素樹脂の混合物からなるプライマー層を設けることで、密着性をより強くすることができる。 According to the invention which concerns on Claim 4, adhesiveness can be strengthened more by providing the primer layer which consists of a mixture of titanium diisopropoxybis (triethanolaminate) and a fluororesin as a titanate-type primer.
請求項５に係る発明によれば、炭素材料上にフッ素樹脂皮膜をコーティングし、炭素材料とフッ素樹脂皮膜の間にチタネート系プライマーまたはクロム酸系プライマーからなるプライマー層を設けた耐食性部材を半導体製造装置において使用することで、金属コンタミネーションが発生しない、強度がある加工が容易な半導体製造装置とすることができる。 According to the invention of claim 5, a corrosion-resistant member in which a fluororesin film is coated on a carbon material and a primer layer made of a titanate primer or a chromic acid primer is provided between the carbon material and the fluororesin film is manufactured as a semiconductor. By using it in the apparatus, it is possible to provide a semiconductor manufacturing apparatus that does not generate metal contamination and that can be easily processed with strength.
請求項６に係る発明によれば、炭素材料上にフッ素樹脂皮膜をコーティングし、炭素材料とフッ素樹脂皮膜の間にチタネート系プライマーまたはクロム酸系プライマーからなるプライマー層を設けた耐食性部材を熱交換器において使用することで、金属コンタミネーションが発生しない、耐久性の高い熱交換器とすることができる。
また、炭素材料は熱伝導性が高いため、効率よく熱交換できる熱交換器を提供することができる。
According to the invention of claim 6, heat exchange is performed on the corrosion-resistant member in which a fluororesin film is coated on the carbon material and a primer layer composed of a titanate primer or a chromic acid primer is provided between the carbon material and the fluororesin film. By using it in an oven, it is possible to provide a highly durable heat exchanger that does not generate metal contamination.
Moreover, since the carbon material has high thermal conductivity, a heat exchanger capable of efficiently exchanging heat can be provided.
１．精密機械用耐食性部材
以下、本発明に係る精密機械用耐食性部材について詳細に説明する。
1. Hereinafter, the corrosion-resistant member for precision machines according to the present invention will be described in detail.
本発明の目的は、炭素材料にプライマー層を介してフッ素樹脂をコーティングした構成とすることにより、金属コンタミネーションが発生することなく、強度があり加工が容易な精密機械用耐食性部材を提供することにある。 An object of the present invention is to provide a corrosion-resistant member for precision machinery that is strong and easy to process without generating metal contamination by adopting a configuration in which a fluororesin is coated on a carbon material via a primer layer. It is in.
図１は、本発明に係る精密機械用耐食性部材の構造断面図であり、その構造は、炭素材料（１）と、炭素材料（１）上に形成されたプライマー層（２）と、プライマー層（２）上に形成されたフッ素樹脂皮膜（３）とから成る。 FIG. 1 is a structural sectional view of a corrosion-resistant member for precision machinery according to the present invention. The structure includes a carbon material (1), a primer layer (2) formed on the carbon material (1), and a primer layer. (2) It consists of a fluororesin film (3) formed thereon.
炭素材料（１）として等方性黒鉛を使用する。等方性黒鉛は従来の異方性黒鉛と異なり、切り出し方向による特性差がないことから加工が容易であるため、本発明において好適に使用される。かさ密度は１．４〜１．７Ｍｇ／ｍ３程度が好ましい。
You use the isotropic black lead as charcoal material fee (1). Isotropic graphite is preferably used in the present invention because it is easy to process because there is no difference in properties depending on the cutting direction, unlike conventional anisotropic graphite. The bulk density is preferably about 1.4 to 1.7 Mg / m 3 .
フッ素樹脂皮膜（３）と炭素材料（１）との密着性を向上させるために、両者の間にプライマー層（２）を設ける。プライマー層（２）を構成するプライマーとしては、チタネート系プライマー又はクロム酸系プライマーを使用する。
この発明において使用するクロム酸系プライマーとしてフッ素樹脂とクロム酸及びリン酸を含む混合物を好適に用いることができ、具体的には８５０Ｇ−３１４（Ｄｕｐｏｎｔ社製）と８５０−７７９９（Ｄｕｐｏｎｔ社製）の重量比３：１混合液が挙げられる。
この発明において使用するチタネート系プライマーとして特許公開２０１１−２０２０３４に開示のプライマーが挙げられる。具体的には、チタニウムジイソプロポキシビス（トリエタノールアミネート）とフッ素樹脂の混合物等が挙げられる。
この発明においてチタネート系プライマー又はクロム酸系プライマーを用いることにより、炭素材料（１）とフッ素樹脂皮膜（３）との密着性がより優れたものとなる。
この発明において、チタネート系プライマーはクロム酸系プライマーと比べて毒性がより低いため、チタネート系プライマーが好適に使用される。何故ならチタネート系プライマーを用いることにより、環境に悪影響を及ぼすことがないからである。
プライマー層（２）の膜厚は３〜１５μｍの範囲内であることが好ましい。プライマー層（２）の膜厚が３μｍ未満だとフッ素樹脂皮膜（３）と炭素材料（１）とを密着させる力が小さくなるため好ましくなく、１５μｍより大きいと発泡などが発生し加工不良となるため好ましくない。
In order to improve the adhesion between the fluororesin film (3) and the carbon material (1), a primer layer (2) is provided between them. As a primer constituting the primer layer (2), a titanate primer or a chromic acid primer is used.
A mixture containing a fluororesin, chromic acid and phosphoric acid can be suitably used as the chromic acid-based primer used in the present invention. Specifically, 850G-314 (manufactured by Dupont) and 850-7799 (manufactured by Dupont) A 3: 1 weight ratio liquid mixture is mentioned.
Examples of titanate-based primers used in the present invention include the primers disclosed in Japanese Patent Publication No. 2011-202034. Specifically, a mixture of titanium diisopropoxybis (triethanolamate) and a fluororesin can be used.
In this invention, by using a titanate primer or a chromic acid primer, the adhesion between the carbon material (1) and the fluororesin film (3) becomes more excellent.
In this invention, since titanate primers are less toxic than chromate primers, titanate primers are preferably used. This is because the use of titanate primers does not adversely affect the environment.
The thickness of the primer layer (2) is preferably in the range of 3 to 15 μm. If the film thickness of the primer layer (2) is less than 3 μm, it is not preferable because the force for adhering the fluororesin film (3) and the carbon material (1) decreases, and if it is greater than 15 μm, foaming or the like occurs, resulting in processing defects. Therefore, it is not preferable.
フッ素樹脂皮膜（３）におけるフッ素樹脂の種類は特に限定されず、例えば、ポリテトラフルオロエチレン・エチレン共重合体（ＰＴＥＥ）、ポリテトラフルオロエチレン（ＰＴＦＥ）、テトラフルオロエチレン・パーフルオロアルキルビニルエーテル共重合体（ＰＦＡ）、テトラフルオロエチレン・ヘキサフルオロプロピレン共重合体（ＦＥＰ）、フッ化ビニリデン樹脂（ＶＦ２）等を使用することができる。
本発明においては、ＰＦＡ、ＦＥＰが好適に使用される。何故ならピンホールがないフッ素樹脂皮膜を形成するのに適しており、耐薬品性が良いからである。
フッ素樹脂皮膜（３）の膜厚は１００〜２０００μｍの範囲内であることが好ましい。フッ素樹脂皮膜（３）の膜厚が１００μｍ未満だと耐熱性や耐酸性度が低くなるため好ましくなく、２０００μｍより大きいと皮膜の収縮力が大きくなり、耐食性部材の歪みが増すため好ましくない。
The kind of fluororesin in the fluororesin film (3) is not particularly limited. For example, polytetrafluoroethylene / ethylene copolymer (PTEE), polytetrafluoroethylene (PTFE), tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer A polymer (PFA), a tetrafluoroethylene / hexafluoropropylene copolymer (FEP), a vinylidene fluoride resin (VF2), or the like can be used.
In the present invention, PFA and FEP are preferably used. This is because it is suitable for forming a fluororesin film having no pinholes and has good chemical resistance.
The film thickness of the fluororesin film (3) is preferably in the range of 100 to 2000 μm. When the film thickness of the fluororesin film (3) is less than 100 μm, the heat resistance and acid resistance are low, which is not preferable. When the film thickness is more than 2000 μm, the film contraction force increases and the corrosion-resistant member increases, which is not preferable.
２．精密機械用耐食性部材の製造方法
次に、本発明の精密機械用耐食性部材の製造方法について説明する。
まず、炭素材料（１）表面のゴミやホコリを取り除く。次に、コーティングの施工温度で熱分解するような有機物等を取り除くため必要に応じて有機溶剤等で脱脂処理を行なうか４００℃程度で空焼きする。接着のための表面積を増やすため、炭素材料（１）の表面をブラスト処理によって粗面化する。ブラスト処理の方法は特に限定されない。
上記したプライマーを用いて炭素材料の上にプライマー層（２）を形成する。プライマーはエアスプレー等の方法で塗布し、乾燥させる。乾燥させる方法は特に限定されない。プライマーを塗布する際、１回塗布しても良いし、複数回塗布しても良い。
プライマー層（２）の上にフッ素樹脂皮膜（３）を静電粉体塗装法等によって１〜２０回塗布し、３２０〜３８０℃で１〜５時間焼成する。
2. Method for Producing Corrosion-Resistant Member for Precision Machine Next, a method for producing a corrosion-resistant member for precision machine according to the present invention will be described.
First, dust and dust on the surface of the carbon material (1) are removed. Next, in order to remove organic substances that are thermally decomposed at the coating application temperature, degreasing treatment is performed with an organic solvent or the like as necessary, or baking is performed at about 400 ° C. In order to increase the surface area for adhesion, the surface of the carbon material (1) is roughened by blasting. The method of blasting is not particularly limited.
A primer layer (2) is formed on the carbon material using the above-described primer. The primer is applied by a method such as air spray and dried. The method for drying is not particularly limited. When applying the primer, it may be applied once or a plurality of times.
On the primer layer (2), the fluororesin film (3) is applied 1 to 20 times by electrostatic powder coating or the like, and baked at 320 to 380 ° C. for 1 to 5 hours.
本発明の耐食性部材の使用用途は特に限定されず、原子力、航空宇宙分野などの環境・エネルギー関連、半導体製造用、熱交換器、イオン注入装置用や高周波素子製造用などのエレクトロニクス関連、各種工業炉部材、光ファイバー等幅広い分野に使用することができる。
本発明においては、半導体製造装置及び熱交換器に好適に使用される。
特に半導体製造装置のウエハ洗浄工程を行う部分に使用される部材として好適に使用される。
The use of the corrosion-resistant member of the present invention is not particularly limited, and is related to the environment and energy in the fields of nuclear power, aerospace, etc., electronics related to semiconductor manufacturing, heat exchanger, ion implantation equipment and high frequency device manufacturing, and various industries. It can be used in a wide range of fields such as furnace members and optical fibers.
In this invention, it uses suitably for a semiconductor manufacturing apparatus and a heat exchanger.
In particular, it is suitably used as a member used in a part for performing a wafer cleaning process of a semiconductor manufacturing apparatus.
以下、本発明に係る精密機械用耐食性部材に関する実施例を示すことにより、本発明の効果をより明確なものとする。但し、本発明は以下の実施例に限定されるものではない。 Hereinafter, the effects of the present invention will be made clearer by showing examples of the corrosion-resistant member for precision machinery according to the present invention. However, the present invention is not limited to the following examples.
１．精密機械用耐食性部材の製造
（実施例１）
等方性黒鉛であるＩＧ−１１（東洋炭素株式会社製）のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上にスプレー法によってチタネート系プライマーチタニウムジイソプロポキシビス（トリエタノールアミネート）とフッ素樹脂混合物を塗布し、その上に静電粉体塗装法によってフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを実施例１とした。
1. Production of corrosion-resistant materials for precision machinery (Example 1)
A titanate-based primer titanium diisopropoxybis (triethanolaminate) and a fluororesin mixture are sprayed on a plate (200 mm × 200 mm × thickness 5 mm) of IG-11 (made by Toyo Tanso Co., Ltd.) which is isotropic graphite. The coating was applied, and a fluororesin film (NFX-3650A: manufactured by Nippon Fuso Kogyo Co., Ltd.) with a thickness of 300 μm was coated thereon by an electrostatic powder coating method. This was designated Example 1.
（実施例２）
ＩＧ−１１の高純度製品であるＩＧ−１１０（東洋炭素株式会社製）のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に、実施例１と同様の方法によりチタネート系プライマーを塗布し、その上に実施例１と同様の方法によりフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを実施例２とした。
(Example 2)
A titanate primer was applied on the plate (200 mm × 200 mm × thickness 5 mm) of IG-110 (manufactured by Toyo Tanso Co., Ltd.), which is a high-purity product of IG-11, in the same manner as in Example 1. A fluororesin film (NFX-3650A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated at a thickness of 300 μm by the same method as in Example 1. This was designated Example 2.
（実施例３）
ＩＧ−１１（東洋炭素株式会社製）のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によってクロム酸系プライマー８５０Ｇ−３１４（Ｄｕｐｏｎｔ社製）と８５０−７７９９（Ｄｕｐｏｎｔ社製）の重量比３：１混合液を塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを実施例３とした。
(Example 3)
Chromic acid primers 850G-314 (Dupont) and 850-7799 (Dupont) on the plate (200 mm x 200 mm x thickness 5 mm) of IG-11 (made by Toyo Tanso Co., Ltd.) by the same method as Example 1. The 3: 1 weight ratio liquid mixture was apply | coated, and the fluororesin membrane | film | coat (NF-240A: Nihon Fluoro Kogyo Co., Ltd. product) was coated by thickness 500 micrometers by the same method as Example 1 on it. This was designated as Example 3.
（実施例４）
ＩＧ−１１０（東洋炭素株式会社製）のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によってクロム酸系プライマーを塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを実施例４とした。
Example 4
A chromic primer was applied on the plate (200 mm × 200 mm × thickness 5 mm) of IG-110 (manufactured by Toyo Tanso Co., Ltd.) by the same method as in Example 1, and a fluororesin film was applied thereon by the same method as in Example 1. (NF-240A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated with a thickness of 500 μm. This was designated Example 4.
（比較例１）
ステンレス（ＳＵＳ３０４）のプレート（２００ｍｍ×２００ｍｍ×厚み６ｍｍ）上に実施例１と同じ方法によってチタネート系プライマーを塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを比較例１とした。
(Comparative Example 1)
A titanate primer was applied on a stainless steel (SUS304) plate (200 mm × 200 mm × thickness 6 mm) by the same method as in Example 1, and then a fluororesin film (NFX-3650A: Nippon Fluoro) was applied by the same method as in Example 1. Kogyo Co., Ltd.) was coated with a thickness of 300 μm. This was designated as Comparative Example 1.
（比較例２）
ステンレス（ＳＵＳ３０４）のプレート（２００ｍｍ×２００ｍｍ×厚み６ｍｍ）上に実施例１と同じ方法によってクロム酸系プライマーを塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを比較例２とした。
(Comparative Example 2)
A chromic acid-based primer was applied to a stainless steel (SUS304) plate (200 mm × 200 mm × thickness 6 mm) by the same method as in Example 1, and then a fluororesin film (NF-240A: Japan) by the same method as in Example 1. Co., Ltd.) was coated with a thickness of 500 μm. This was designated as Comparative Example 2.
（比較例３）
石英ガラスのプレート（１６５ｍｍ×１６５ｍｍ×厚み３ｍｍ）上に実施例１と同じ方法によってチタネート系プライマーを塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを比較例３とした。
(Comparative Example 3)
A titanate primer was applied on a quartz glass plate (165 mm × 165 mm × thickness 3 mm) by the same method as in Example 1, and a fluororesin film (NFX-3650A: Nippon Fluoro Industries, Ltd.) was applied by the same method as in Example 1. Co., Ltd.) was coated with a thickness of 300 μm. This was designated as Comparative Example 3.
（比較例４）
石英ガラスのプレート（１６５ｍｍ×１６５ｍｍ×厚み３ｍｍ）上に実施例１と同じ方法によってクロム酸系プライマーを塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを比較例４とした。
(Comparative Example 4)
A chromic primer was applied on a quartz glass plate (165 mm × 165 mm × thickness 3 mm) by the same method as in Example 1, and then a fluororesin film (NF-240A: Nippon Fluoro Industries, Ltd.) was applied by the same method as in Example 1. Co., Ltd.) was coated with a thickness of 500 μm. This was designated as Comparative Example 4.
（比較例５）
ＩＧ−１１のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によって樹脂系プライマー４２０−７０６（Ｄｕｐｏｎｔ社製）を塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを比較例５とした。
(Comparative Example 5)
Resin primer 420-706 (manufactured by Dupont) was applied on the IG-11 plate (200 mm × 200 mm × thickness 5 mm) by the same method as in Example 1, and a fluororesin film was applied thereon by the same method as in Example 1. (NFX-3650A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated with a thickness of 300 μm. This was designated as Comparative Example 5.
（比較例６）
ＩＧ−１１０のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によって樹脂系プライマー４２０−７０６（Ｄｕｐｏｎｔ社製）を塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦＸ−３６５０Ａ：日本フッソ工業株式会社製）を厚み３００μｍでコーティングした。これを比較例６とした。
(Comparative Example 6)
Resin primer 420-706 (manufactured by Dupont) was applied on an IG-110 plate (200 mm × 200 mm × thickness 5 mm) by the same method as in Example 1, and a fluororesin film was applied thereon by the same method as in Example 1. (NFX-3650A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated with a thickness of 300 μm. This was designated as Comparative Example 6.
（比較例７）
ＩＧ−１１のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によって樹脂系プライマー４２０−７０６（Ｄｕｐｏｎｔ社製）を塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを比較例７とした。
(Comparative Example 7)
Resin primer 420-706 (manufactured by Dupont) was applied on the IG-11 plate (200 mm × 200 mm × thickness 5 mm) by the same method as in Example 1, and a fluororesin film was applied thereon by the same method as in Example 1. (NF-240A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated with a thickness of 500 μm. This was designated as Comparative Example 7.
（比較例８）
ＩＧ−１１０のプレート（２００ｍｍ×２００ｍｍ×厚み５ｍｍ）上に実施例１と同じ方法によって樹脂系プライマー４２０−７０６（Ｄｕｐｏｎｔ社製）を塗布し、その上に実施例１と同じ方法によってフッ素樹脂皮膜（ＮＦ−２４０Ａ：日本フッソ工業株式会社製）を厚み５００μｍでコーティングした。これを比較例８とした。
(Comparative Example 8)
Resin primer 420-706 (manufactured by Dupont) was applied on an IG-110 plate (200 mm × 200 mm × thickness 5 mm) by the same method as in Example 1, and a fluororesin film was applied thereon by the same method as in Example 1. (NF-240A: manufactured by Nippon Fuso Kogyo Co., Ltd.) was coated with a thickness of 500 μm. This was designated as Comparative Example 8.
２．精密機械用耐食性部材の評価方法
次に、精密機械用耐食性部材の評価方法を説明する。
本評価においては山崎式ライニングテスターＬＡ−１５（山崎精機研究所製）を使用した。図２は、本実施例及び比較例の精密機械用耐食性部材を評価する際の様子を示す。
山崎式ライニングテスターＬＡ−１５において、上記実施例及び比較例の耐食性部材プレート（４）を５％塩酸中に下半分を浸潤させ、密閉することで上半分を揮発した５％塩酸に曝した。
５％塩酸に直接浸かる耐食性部材の下半分を液相部分、５％塩酸に直接浸からない上半分を気相部分とし、二つの部分を合わせて浸漬部分（５）とした。これを１００℃下で４週間放置し、１週間ごとに以下の評価を行った。
2. Evaluation Method for Corrosion Resistant Member for Precision Machinery Next, an evaluation method for the corrosion resistant member for precision machinery will be described.
In this evaluation, a Yamazaki lining tester LA-15 (manufactured by Yamazaki Seiki Laboratories) was used. FIG. 2 shows a state when evaluating the corrosion-resistant members for precision machines of this example and the comparative example.
In the Yamazaki type lining tester LA-15, the corrosion-resistant member plate (4) of the above-mentioned Examples and Comparative Examples was exposed to 5% hydrochloric acid in which the lower half was infiltrated in 5% hydrochloric acid and the upper half was volatilized by sealing.
The lower half of the corrosion-resistant member immersed directly in 5% hydrochloric acid was the liquid phase portion, the upper half not directly immersed in 5% hydrochloric acid was the gas phase portion, and the two portions were combined to form the immersion portion (5). This was left at 100 ° C. for 4 weeks, and the following evaluation was performed every week.
外観評価
皮膜の変色、劣化、ブリスターの発生等の異常の有無を含む外観の変化の目視並びに拡大鏡での観察を１週間ごとに行った。
Appearance evaluation The appearance change including the presence / absence of abnormalities such as discoloration, deterioration and occurrence of blisters was visually observed and observed with a magnifier every week.
ブリスターの最大径、発生面積の評価
ブリスターの最大径、発生面積を１週間ごとに測定した。
Evaluation of the maximum diameter and generation area of blisters The maximum diameter and generation area of blisters were measured every week.
重量変化の評価
重量変化の評価を１週間ごとに測定した。重量測定の結果より、皮膜の単位面積当たりの重量変化（ΔＷ／Ｓ、重量変化（ｍｇ）／表面積（１２３ｃｍ２））を求め、その結果を表１乃至４に示す。
Evaluation of Weight Change Evaluation of weight change was measured every week. The weight change per unit area of the film (ΔW / S, weight change (mg) / surface area (123 cm 2 )) was determined from the results of the weight measurement, and the results are shown in Tables 1 to 4.
密着力の評価
図３は、本発明に係る精密機械用耐食性部材の密着力を評価する際の様子を示す。実施例１乃至４と比較例１乃至８を５％塩酸に浸漬させ、１００℃下で４週間評価した後、皮膜を５ｍｍ幅でカットし９０°方向に皮膜を剥がし、剥がす際に必要な力（Ｎ／５ｍｍ幅）を図３に示すＡ乃至Ｅ点でそれぞれ測定した。
測定値には炭素材料等の基材との密着力以外に、皮膜を曲げるのに要する力も含まれ、測定値は膜厚に影響される。本実施例及び比較例では、剥がす際に必要な力が２４．５Ｎ／５ｍｍ以上または皮膜が測定時に破断すれば密着力の低下は認めないと判断した。
また、Ａ点は浸漬部分ではないため５％塩酸や１００℃に曝された影響を受けておらず、Ｂ乃至Ｅ点の測定値をＡ点と比較することで密着力が維持されているかどうかを判断した。その結果を表５に示す。
Evaluation of Adhesion Strength FIG. 3 shows a state when evaluating the adhesion strength of the corrosion resistant member for precision machinery according to the present invention. Examples 1 to 4 and Comparative Examples 1 to 8 were immersed in 5% hydrochloric acid and evaluated at 100 ° C. for 4 weeks. Then, the film was cut to a width of 5 mm, and the film was peeled off in the 90 ° direction. (N / 5 mm width) was measured at points A to E shown in FIG.
The measured value includes the force required to bend the film in addition to the adhesion force with the base material such as a carbon material, and the measured value is influenced by the film thickness. In this example and the comparative example, it was judged that a decrease in the adhesion force was not recognized if the force required for peeling was 24.5 N / 5 mm or more or the film was broken during the measurement.
In addition, since point A is not an immersion part, it is not affected by exposure to 5% hydrochloric acid or 100 ° C, and whether the adhesion is maintained by comparing the measured values of points B to E with point A Judged. The results are shown in Table 5.
上記の評価の結果、ブリスターを含む外観、重量及び密着力に変化がないものほど耐熱性、耐酸性度の高い、優れた精密機械用耐食性部材であるとすることができる。 As a result of the above evaluation, a material having no change in appearance, weight and adhesion including blisters can be considered to be an excellent corrosion-resistant member for precision machines having higher heat resistance and acid resistance.
以上の実施例及び比較例における評価試験の結果は下記の通りである。 The results of the evaluation tests in the above examples and comparative examples are as follows.
＜評価＞
外観評価の結果、実施例１乃至４にはブリスターの発生、皮膜の変色、劣化等の異常は認められなかった（図４参照）。
比較例１では、試験開始後２週間後から液相部分にブリスターの発生が確認され、試験期間の経過とともにブリスターの面積の増加が確認されたことから（図５参照）、皮膜が５％塩酸浸透の影響を受けていると考えられる。
比較例２では、試験開始１週間後から液相部分にブリスターの発生が確認された。試験開始２週間後からは気相、液相部分共にブリスター発生を確認し、試験期間の経過とともにブリスターの面積の増加が確認されたことから（図６参照）、５％塩酸浸透の影響を受けていると考えられる。
また、比較例３及び４では、試験開始後２週間後から気相、液相部分共にブリスターの発生が確認され、試験期間の経過とともにブリスターの面積の増加が確認されたことから（図７参照）、皮膜が５％塩酸浸透の影響を受けていると考えられる。
<Evaluation>
As a result of the appearance evaluation, Examples 1 to 4 showed no abnormalities such as blistering, discoloration and deterioration of the film (see FIG. 4).
In Comparative Example 1, since the occurrence of blister was confirmed in the liquid phase portion after 2 weeks from the start of the test, and the increase in the area of the blister was confirmed with the passage of the test period (see FIG. 5), the film was 5% hydrochloric acid. It is thought to be affected by penetration.
In Comparative Example 2, the occurrence of blisters was confirmed in the liquid phase part one week after the start of the test. Two weeks after the start of the test, the occurrence of blistering was confirmed in both the gas phase and the liquid phase, and the increase in the area of the blister was confirmed over the course of the test period (see Fig. 6). It is thought that.
In Comparative Examples 3 and 4, the occurrence of blisters was confirmed in both the gas phase and the liquid phase part after 2 weeks from the start of the test, and the increase in the area of the blisters was confirmed with the passage of the test period (see FIG. 7). ), The film is considered to be affected by 5% hydrochloric acid penetration.
また、重量変化の評価の結果、比較例２の重量変化の値が１．８７ｍｇ／ｃｍ２となり、他の実施例及び比較例に比べて５％塩酸の浸透が進んでいることを示した。
比較例２には及ばないものの、比較例１、３、４の重量変化の値はそれぞれ０．５７ｍｇ／ｃｍ２、０．８１ｍｇ／ｃｍ２、１．５４ｍｇ／ｃｍ２であり、浸透が進んでいることを示した。
Further, as a result of the evaluation of the weight change, the value of the weight change of Comparative Example 2 was 1.87 mg / cm 2 , indicating that 5% hydrochloric acid permeation was advanced as compared with other Examples and Comparative Examples.
Although not inferior to Comparative Example 2, respectively 0.57 mg / cm 2 is the value of the weight change of the comparative example 1, 3,4, 0.81 mg / cm 2, was 1.54 mg / cm 2, penetration willing Showed that.
表１乃至４の結果から、ステンレスや石英ガラスを基材とする耐食性部材と比較して炭素材料を基材とする耐食性部材はブリスターの発生が見られず、重量変化もほとんどなかったことから耐熱性、耐酸性共に優れていた。
また、実施例１及び２、実施例３及び４を比較すると、ＩＧ−１１とＩＧ−１１０との間に差異は認められなかった。
さらに実施例１、３と比較例５、７、及び実施例２、４と比較例６、８を比較すると、炭素材料を基材とした時、チタネート系プライマー、クロム酸系プライマー及び樹脂系プライマーとの間に耐熱性及び耐酸性については大きな差異は認められなかった。
From the results of Tables 1 to 4, the corrosion resistant member based on the carbon material showed no blistering and hardly changed in weight compared to the corrosion resistant member based on stainless steel or quartz glass. Both acidity and acid resistance were excellent.
Moreover, when Example 1 and 2 and Example 3 and 4 were compared, the difference was not recognized between IG-11 and IG-110.
Further, when Examples 1 and 3 are compared with Comparative Examples 5 and 7, and Examples 2 and 4 are compared with Comparative Examples 6 and 8, when a carbon material is used as a base material, a titanate primer, a chromic acid primer, and a resin primer There was no significant difference in heat resistance and acid resistance.
密着力の評価の結果、炭素材料を基材とし、樹脂系プライマーを使用している比較例５乃至８は、Ａ点において、この比較例５乃至８とはチタネート系プライマーまたはクロム酸系プライマーを使用している点のみ異なる実施例１乃至４と比較して低い測定値が得られた。
つまり、比較例５乃至８は実施例１乃至４と比較して、１００℃、５％塩酸に曝す前の初期密着力が低いことが確認された。
また、実施例１乃至４は密着力が強いため皮膜の破断が見られた。実施例１乃至４のＢ乃至Ｅ点の測定値は目安値（２４．５Ｎ／５ｍｍ）よりも低いものの、浸漬していないＡ点と測定値がほとんど変わらないことから、気相、液相部分共に浸漬前の密着力を維持していることが確認された（図８参照）。
As a result of the evaluation of adhesion, Comparative Examples 5 to 8 using a carbon material as a base material and using a resin-based primer are different from those of Comparative Examples 5 to 8 in that a titanate-based primer or a chromic acid-based primer is used. Compared with Examples 1 to 4 which differ only in the points used, low measured values were obtained.
That is, it was confirmed that Comparative Examples 5 to 8 had a lower initial adhesion before exposure to 100 ° C. and 5% hydrochloric acid than Examples 1 to 4.
Moreover, since Examples 1 to 4 had strong adhesion, the film was broken. Although the measured values of points B to E in Examples 1 to 4 are lower than the standard value (24.5 N / 5 mm), the measured values are almost the same as those of the point A that is not immersed. It was confirmed that the adhesion before dipping was maintained (see FIG. 8).
表５の結果から、同じ炭素材料を基材とする耐食性部材でも樹脂系プライマーを用いた場合、チタネート系プライマーまたはクロム酸系プライマーを用いた場合と比べて１００℃、５％塩酸に曝す前の初期密着力が低いことが確認された。
炭素材料を基材とする耐食性部材にチタネート系プライマーまたはクロム酸系プライマーを用いた場合、浸漬しても気相、液相部分共に浸漬前の密着力を維持していた。
これらの結果から、樹脂系プライマーからなるプライマー層を有する炭素材料を基材とする耐食性部材よりも、チタネート系プライマーまたはクロム酸系プライマーからなるプライマー層を有する炭素材料を基材とする耐食性部材の方が密着性に優れているといえる。
From the results of Table 5, when using a resin-based primer even with a corrosion-resistant member made of the same carbon material as a base material, it was before exposure to 100 ° C. and 5% hydrochloric acid as compared with the case of using a titanate-based primer or a chromic acid-based primer. It was confirmed that the initial adhesion was low.
When a titanate-based primer or chromic acid-based primer was used for a corrosion-resistant member having a carbon material as a base material, the adhesion before dipping was maintained in both the gas phase and the liquid phase even when immersed.
From these results, the corrosion-resistant member based on a carbon material having a primer layer composed of a titanate-based primer or a chromic acid-based primer rather than a corrosion-resistant member based on a carbon material having a primer layer composed of a resin-based primer. It can be said that is better in adhesion.
炭素材料を基材とする耐食性部材のＡ乃至Ｅ点全ての密着力がステンレスを基材とする耐食性部材よりも低かった。
密着力評価後の耐食性部材の状態を観察すると、プライマー層と炭素材料の層が混在していることから、密着力評価の際に炭素材料の表層が破壊されながら皮膜が剥がれていたと推測される。
つまり、炭素材料を基材とする耐食性部材のＡ乃至Ｅ点全ての密着力がステンレスを基材とする耐食性部材よりも低かったのは、炭素材料の物性が影響していると考えられる。
The adhesion strength at all points A to E of the corrosion resistant member based on the carbon material was lower than that of the corrosion resistant member based on stainless steel.
When the state of the corrosion-resistant member after the adhesion evaluation is observed, it is presumed that since the primer layer and the carbon material layer are mixed, the film was peeled off while the surface layer of the carbon material was destroyed during the adhesion evaluation. .
That is, it is considered that the physical properties of the carbon material influence the reason why the adhesion strength of all points A to E of the corrosion resistant member based on the carbon material is lower than that of the corrosion resistant member based on the stainless steel.
以上の結果から、炭素材料を基材とし、プライマー層がチタネート系プライマー又はクロム酸系プライマーからなる耐食性部材は、耐熱性、耐酸性、密着力全てにおいて優れた部材であることがわかる。 From the above results, it can be seen that a corrosion-resistant member having a carbon material as a base material and having a primer layer made of a titanate-based primer or a chromic acid-based primer is an excellent member in all of heat resistance, acid resistance, and adhesion.
本発明である耐食性部材は、半導体製造装置及び熱交換器に好適に利用される。 The corrosion-resistant member according to the present invention is suitably used for a semiconductor manufacturing apparatus and a heat exchanger.
１ 炭素材料
２ プライマー層
３ フッ素樹脂皮膜
４ 耐食性部材プレート
５ 浸漬部分
DESCRIPTION OF SYMBOLS 1 Carbon material 2 Primer layer 3 Fluororesin film | membrane 4 Corrosion-resistant member plate 5 Immersion part
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