TWI772489B - Aluminium-containing member and manufacturing method of oxide film thereof - Google Patents
Aluminium-containing member and manufacturing method of oxide film thereof Download PDFInfo
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- TWI772489B TWI772489B TW107128081A TW107128081A TWI772489B TW I772489 B TWI772489 B TW I772489B TW 107128081 A TW107128081 A TW 107128081A TW 107128081 A TW107128081 A TW 107128081A TW I772489 B TWI772489 B TW I772489B
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 52
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 48
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004411 aluminium Substances 0.000 title 1
- 239000004065 semiconductor Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000005260 corrosion Methods 0.000 claims abstract description 40
- 230000007797 corrosion Effects 0.000 claims abstract description 40
- 239000010407 anodic oxide Substances 0.000 claims abstract description 38
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 23
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 44
- 235000006408 oxalic acid Nutrition 0.000 claims description 20
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 16
- 239000003792 electrolyte Substances 0.000 claims description 16
- 235000002906 tartaric acid Nutrition 0.000 claims description 16
- 239000011975 tartaric acid Substances 0.000 claims description 16
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 14
- 239000008151 electrolyte solution Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 8
- 238000009413 insulation Methods 0.000 abstract description 6
- 239000011247 coating layer Substances 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 57
- 238000000576 coating method Methods 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 13
- 239000010410 layer Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000007743 anodising Methods 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910052794 bromium Inorganic materials 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- -1 aluminum-fluorine compounds Chemical class 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/28008—Making conductor-insulator-semiconductor electrodes
- H01L21/28017—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon
- H01L21/28158—Making the insulator
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
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Abstract
本發明涉及在鋁或鋁合金構件表面形成耐腐蝕性及絕緣性佳的陽極氧化膜的方法及形成有以該方法製造的陽極氧化膜的鋁或鋁合金構件，更詳細而言，涉及一種無陽極氧化塗層內部缺陷且具高硬度的氧化膜且耐腐蝕性及絕緣性佳的陽極氧化膜的形成方法以及塗佈有以該方法製造的陽極氧化膜的半導體或顯示裝置製造裝置用內構件。 The present invention relates to a method for forming an anodic oxide film with good corrosion resistance and insulation on the surface of an aluminum or aluminum alloy member, and an aluminum or aluminum alloy member formed with the anodic oxide film produced by the method. A method for forming an anodic oxide film with internal defects in anodized coating layer, high hardness oxide film and excellent corrosion resistance and insulating properties, and internal member for semiconductor or display device manufacturing device coated with the anodic oxide film produced by the method .
Description
本發明涉及在鋁或鋁合金構件的表面形成耐腐蝕性及絕緣性佳的陽極氧化膜的方法及形成有以該方法製造的陽極氧化膜的鋁或鋁合金構件，更詳細而言，涉及一種無陽極氧化塗層內部缺陷且具高硬度的氧化膜且耐腐蝕性及絕緣性佳的陽極氧化膜的形成方法以及塗佈有以該方法製造的陽極氧化膜的半導體或顯示裝置製造裝置用內構件。 The present invention relates to a method for forming an anodic oxide film with good corrosion resistance and insulation on the surface of an aluminum or aluminum alloy member, and an aluminum or aluminum alloy member having the anodic oxide film produced by the method. More specifically, it relates to a A method for forming an anodized film having no internal defects in an anodized coating, having a high hardness oxide film, and having good corrosion resistance and insulating properties, and an interior for a semiconductor or display device manufacturing device coated with the anodized film produced by the method member.
在用於實現半導體元件或其他超微細形狀的製程領域中，正在廣泛使用真空電漿體裝備。作為使用真空電漿體裝備的示例，有以利用了電漿體的化學氣相沉積法而在基板上形成沉積膜的PECVD(plasma enhanced chemical vapor deposition，化學氣相沉積)裝備、以物理方法形成沉積膜的濺射裝備及用於將基板或基板上的塗佈物質蝕刻成所需圖案的乾式蝕刻裝備等，真空電漿體裝備利用高溫的電漿體，實現半導體元件的蝕刻或超微細形狀。 In the field of processes for realizing semiconductor elements or other ultra-fine shapes, vacuum plasma equipment is being widely used. As an example of equipment using vacuum plasma, there are PECVD (plasma enhanced chemical vapor deposition) equipment that forms a deposition film on a substrate by a chemical vapor deposition method using plasma, and a physical method. Sputtering equipment for depositing films and dry etching equipment for etching substrates or coating substances on substrates into desired patterns, etc. Vacuum plasma equipment utilizes high-temperature plasma to achieve etching of semiconductor elements or ultra-fine shapes .
因此，在真空電漿體裝備的內部，發生高溫的電漿體，因而腔室及其內部部件被損傷，從腔室及其部件的表面發生特定元素及污染顆粒，使腔室內部被污染的可能性增大。 Therefore, a high-temperature plasma is generated inside the vacuum plasma equipment, so that the chamber and its internal components are damaged, and specific elements and contaminant particles are generated from the surface of the chamber and its components, so that the interior of the chamber is polluted. possibility increases.
另一方面，作為半導體製造裝置中使用的反應氣體，導入Cl、F、Br等鹵素元素或包括O、N、H、S、C等元素的腐蝕性氣體，因而腔室或腔室內的構件要求對該氣體的耐腐蝕性，在半導體或液晶製造裝置的製程中，也發生鹵素類的電漿體，因而還要求耐電漿體性。 On the other hand, halogen elements such as Cl, F, and Br, or corrosive gases including elements such as O, N, H, S, C, etc. are introduced as reaction gases used in semiconductor manufacturing apparatuses, so the chamber or the members in the chamber are required to be With regard to the corrosion resistance of this gas, a halogen-based plasma is also generated in the manufacturing process of a semiconductor or liquid crystal manufacturing apparatus, and therefore, plasma resistance is also required.
不僅如此，半導體蝕刻製程等一部分腔室內的一部分構件，與高電壓電源部連接，當絕緣性脆弱時，發生電弧作用，因而還要求佳的非導電性。 In addition, some components in a part of the chamber, such as a semiconductor etching process, are connected to a high-voltage power supply, and when the insulation is weak, arcing occurs, and thus excellent non-conductivity is also required.
另一方面，作為半導體製造裝置中使用的材料，由於導電性、製造的容易性及合理價格下的利用可能性，主要使用鋁。 On the other hand, as a material used in a semiconductor manufacturing apparatus, aluminum is mainly used because of electrical conductivity, ease of manufacture, and availability at a reasonable price.
但是，鋁容易與諸如氯、氟及溴的鹵素反應，生成AlCl3、Al2Cl6、AlF3或AlBr3。鋁-氟化合物從處理裝置部件的表面剝離而會誘發部件本身的腐蝕，可以發生處理腔室(及在腔室內製造的部件)的微粒污染源作用。 However, aluminum readily reacts with halogens such as chlorine, fluorine and bromine to form AlCl 3 , Al 2 Cl 6 , AlF 3 or AlBr 3 . The peeling of aluminum-fluorine compounds from the surfaces of processing equipment components induces corrosion of the components themselves, and can act as a source of particulate contamination of the processing chamber (and the components manufactured in the chamber).
另外，含有鋁和氯的許多化合物、含有鋁和溴的許多化合物具有揮發性，在半導體處理條件下生成氣體，這些氣體離開鋁基板。因此，在結構內形成空間，使得該空間結構不穩定，生成完整性有問題的表面。 Additionally, many compounds containing aluminum and chlorine, and many compounds containing aluminum and bromine are volatile and generate gases under semiconductor processing conditions that leave the aluminum substrate. Consequently, a space is created within the structure, making the space structure unstable, creating a surface with questionable integrity.
因此，作為在半導體製造裝置內保護鋁表面的較佳手段，有陽極氧化氧化鋁塗佈方法，陽極氧化處理法是在鋁表面形成由相對多孔性的鋁氧化物構成的一體型塗佈的電解氧化製程。 Therefore, as a preferable means for protecting the aluminum surface in a semiconductor manufacturing apparatus, there is an anodized aluminum oxide coating method. Oxidation process.
作為形成陽極氧化膜的方法，採用將形成陽極氧化膜時的電解液控制為低溫的方法或利用高電流密度進行電解的方法，但如果利用這些方法形成陽極氧化膜，則存在使陽極氧化膜發生裂紋增加的趨勢，另外，這些方法還存在需要高耗能的問題。 As a method of forming the anodic oxide film, a method of controlling the electrolyte solution at the time of forming the anodic oxide film to a low temperature or a method of performing electrolysis with a high current density are used. The tendency for cracks to increase, in addition, these methods also have the problem of requiring high energy consumption.
作為形成陽極氧化膜的方法的先前技術，日本授權專利公報第4660760號(2011.01.14.)提出一種利用添加了乙醇的硫酸類電解液形成高硬質的陽極氧化膜的方法。但是，該現有文獻存在的問題是，陽極氧化處理導致的電解液中的乙醇濃度變化管理煩雜。 As a prior art for a method of forming an anodic oxide film, Japanese Patent Laid-Open No. 4660760 (2011.01.14.) proposes a method of forming a highly rigid anodic oxide film using a sulfuric acid-based electrolyte to which ethanol is added. However, this prior literature has a problem in that it is complicated to manage changes in the ethanol concentration in the electrolytic solution due to anodization treatment.
另外，韓國授權專利公報第10-0664900號(2007.01.04.)提出一種利用在硫酸中少量添加乙二酸的電解液進行陽極氧化表面處理的方法。但是，該現有文獻雖然是用於在半導體製造裝置中獲得50~60μm氧化膜厚度的陽極氧化處理條件，但為了形成希望厚度的薄膜，應施加較高的通入電流，因而在塗層內發生多處缺陷，存在降低耐腐蝕性的問題。 In addition, Korean Patent Publication No. 10-0664900 (2007.01.04.) proposes a method for anodizing surface treatment using an electrolytic solution obtained by adding a small amount of oxalic acid to sulfuric acid. However, this prior literature is anodizing treatment conditions for obtaining an oxide film thickness of 50 to 60 μm in a semiconductor manufacturing apparatus, but in order to form a thin film with a desired thickness, a relatively high current should be applied, so that the formation of There are many defects, and there is a problem of reducing corrosion resistance.
因此，儘管有如上所述的技術開發，但依然迫切需要持續開發能夠提高半導體製造裝置的耐腐蝕性及絕緣性的鋁或鋁合金材料半導體製造裝置的表面處理方法。 Therefore, despite the technical development as described above, there is still an urgent need to continuously develop a surface treatment method for a semiconductor manufacturing apparatus made of aluminum or an aluminum alloy material that can improve the corrosion resistance and insulation properties of the semiconductor manufacturing apparatus.
(現有技術文獻) (Prior Art Literature)
(專利文獻) (patent literature)
(專利文獻0001)日本授權專利公報第4660760號(2011.01.14.) (Patent Document 0001) Japanese Patent Publication No. 4660760 (2011.01.14.)
(專利文獻0002)韓國授權專利公報第10-0664900號(2007.01.04.) (Patent Document 0002) Korean Patent Publication No. 10-0664900 (2007.01.04.)
本發明的主要目的在於提供一種對半導體製造製程中使用的氣體的耐腐蝕性及絕緣性佳的陽極氧化鋁或鋁合金構件的製造方法及經表面處理的半導體製造裝置。 The main object of the present invention is to provide a method for manufacturing anodized aluminum or aluminum alloy members with good corrosion resistance and insulating properties to gases used in the semiconductor manufacturing process, and a surface-treated semiconductor manufacturing apparatus.
為了達成如上所述的目的，本發明提供一種半導體或顯示裝置製造裝置的包含鋁的構件的氧化膜形成方法，作為在其表面形成有陽極氧化膜的半導體或顯示裝置製造裝置的包含鋁的構件的氧化膜形成方法，包括：a)步驟，混合硫酸、乙二酸及酒石酸而製造電解液的步驟；及b)步驟，利用該a)步驟中製造的電解液，在鋁或鋁合金構件表面形成陽極氧化膜的步驟。 In order to achieve the above-mentioned object, the present invention provides a method for forming an oxide film of a member containing aluminum of a semiconductor or display device manufacturing device, as a member containing aluminum of a semiconductor or display device manufacturing device having an anodic oxide film formed on the surface thereof. The oxide film forming method comprises: a) step, the step of mixing sulfuric acid, oxalic acid and tartaric acid to manufacture electrolyte; and b) step, utilizing the electrolyte manufactured in this a) step, on the surface of aluminum or aluminum alloy components The step of forming an anodized film.
根據一個實施例，在該a)步驟中，該硫酸、乙二酸及酒石酸的含量按重量比可以為9~11：2.5~3.5：0.3~0.7。 According to one embodiment, in step a), the content of sulfuric acid, oxalic acid and tartaric acid may be 9~11:2.5~3.5:0.3~0.7 by weight.
另外，根據一個實施例，該電解液的濃度可以為1至10wt%。 In addition, according to one embodiment, the concentration of the electrolyte may be 1 to 10 wt %.
另外，根據一個實施例，在該b)步驟中形成陽極氧化膜時，通入電流可以為0.8至1.7A/dm2，電解液的溫度可以為8至22℃。 In addition, according to one embodiment, when the anodic oxide film is formed in the step b), the passing current may be 0.8 to 1.7 A/dm 2 , and the temperature of the electrolyte may be 8 to 22°C.
另外，根據一個實施例，該陽極氧化膜厚度可以為50μm至60μm。 In addition, according to one embodiment, the thickness of the anodized film may be 50 μm to 60 μm.
另一方面，本發明提供一種以該半導體或顯示裝置製造裝置的包含鋁的構件的氧化膜形成方法而製造的半導體或顯示裝置製造裝置的鋁或鋁合金構件。 On the other hand, the present invention provides an aluminum or aluminum alloy member of a semiconductor or display device manufacturing device manufactured by the method for forming an oxide film of a member containing aluminum of the semiconductor or display device manufacturing device.
本發明提供一種塗佈有硬度為370~425Hv、耐電壓為1500~2000V的陽極氧化膜的半導體或顯示裝置製造裝置的包含鋁的構件，其耐腐蝕性可以為120分鐘以上。 The present invention provides an aluminum-containing member of a semiconductor or display device manufacturing device coated with an anodic oxide film having a hardness of 370-425Hv and a withstand voltage of 1500-2000V, and its corrosion resistance can be 120 minutes or more.
另外，本發明不僅可以提供一種塗佈有硬度為370~425Hv、耐腐蝕性為120分鐘以上的陽極氧化膜的半導體或顯示裝置製造裝置的包含鋁的構 件，而且還可以提供一種塗佈有耐電壓為1500~2000V、耐腐蝕性為120分鐘以上的陽極氧化膜的半導體或顯示裝置製造裝置的包含鋁的構件。 In addition, the present invention can provide not only an aluminum-containing structure of a semiconductor or display device manufacturing device coated with an anodized film having a hardness of 370 to 425 Hv and a corrosion resistance of 120 minutes or more It is also possible to provide an aluminum-containing member of a semiconductor or display device manufacturing device coated with an anodized film having a withstand voltage of 1500 to 2000 V and a corrosion resistance of 120 minutes or more.
本發明的在鋁或鋁合金構件表面形成耐腐蝕性及絕緣性佳的陽極氧化膜的方法，具有可以無陽極氧化塗層內部缺陷地形成50μm以上塗層厚度的效果。 The method for forming an anodic oxide film having excellent corrosion resistance and insulating properties on the surface of an aluminum or aluminum alloy member of the present invention has the effect that a coating thickness of 50 μm or more can be formed without internal defects in the anodic oxide coating.
另外，具有的效果是，對半導體製造裝置中使用的氣體的耐腐蝕性佳，對半導體製造裝置腔室內的高電壓的絕緣性佳。 In addition, there is an effect of excellent corrosion resistance to the gas used in the semiconductor manufacturing apparatus, and excellent insulating properties against the high voltage in the chamber of the semiconductor manufacturing apparatus.
1:電解液 1: Electrolyte
2:多孔質層界面 2: Porous layer interface
3:氣孔 3: Stomata
4:構件 4: Components
5:多孔質層 5: Porous layer
6:阻擋層 6: Barrier layer
7:池 7: Pool
第1圖是顯示在鋁或鋁合金構件表面形成有陽極氧化膜的概略結構的剖面圖。 FIG. 1 is a cross-sectional view showing a schematic structure in which an anodic oxide film is formed on the surface of an aluminum or aluminum alloy member.
第2圖是實施例3及比較例7的SEM圖像。(a)是測量形成有比較例7的氧化膜的剖面的圖像，(b)是測量形成有實施例3的氧化膜的剖面的圖像。 FIG. 2 is an SEM image of Example 3 and Comparative Example 7. FIG. (a) is an image obtained by measuring the cross section where the oxide film of Comparative Example 7 was formed, and (b) is an image obtained by measuring the cross section where the oxide film of Example 3 was formed.
只要未以其他方式定義，本說明書中使用的所有技術性及科學性術語具有與本發明所屬技術領域的具有通常知識者通常所理解的內容相同的意義。一般而言，本說明書中使用的命名法是本技術領域習知和常用的。 Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In general, the nomenclature used in this specification is known and commonly used in the art.
在本申請全部說明書中，當提到某部分「包括」某種構成要素時，只要沒有特別相反的記載，則意味著不排除其他構成，可以還包括其他構成要素。 In the entire specification of the present application, when it is mentioned that a certain part "includes" a certain constituent element, unless otherwise stated, it means that other constituent elements are not excluded, and other constituent elements may also be included.
本發明涉及在其表面上形成有陽極氧化膜的半導體或顯示裝置製造裝置的鋁或鋁合金構件的製造方法，其技術特徵在於，包括：a)步驟，混合硫酸、乙二酸及酒石酸而製造電解液的步驟；及b)步驟，利用該a)步驟中製造的電解液，在鋁或鋁合金構件表面形成陽極氧化膜的步驟。 The present invention relates to a method for manufacturing an aluminum or aluminum alloy member of a semiconductor or display device manufacturing device having an anodic oxide film formed on the surface thereof. The step of electrolytic solution; and the step of b), the step of forming an anodic oxide film on the surface of aluminum or aluminum alloy member by using the electrolytic solution produced in the a) step.
為了製造本發明的形成有陽極氧化膜的鋁或鋁合金構件，使用混合了硫酸、乙二酸及酒石酸的電解液，這與以往的利用添加了硫酸、乙二酸、有機物等的混合浴的硫酸浴相比，即使使用較低的通入電流，也可以形成50μm以上的陽極氧化膜，藉由使用比該硫酸浴低的通入電流，從而不發生陽極氧化膜的內部缺陷，可以提高耐腐蝕性。 In order to manufacture the aluminum or aluminum alloy member on which the anodic oxide film of the present invention is formed, an electrolytic solution mixed with sulfuric acid, oxalic acid, and tartaric acid is used, which is different from the conventional method using a mixed bath to which sulfuric acid, oxalic acid, organic matter, and the like are added. Compared with the sulfuric acid bath, an anodic oxide film of 50 μm or more can be formed even if a lower current is used. Improve corrosion resistance.
另外，利用添加了乙二酸、酒石酸、有機物等的混合浴的乙二酸浴，不同於硫酸浴，施加較低的通入電流，形成不發生陽極氧化膜內部缺陷的薄膜，具有高耐腐蝕性，但由於厚度低，因而硬度及絕緣性低。相反，在本發明中雖然使用較低的通入電流，但可以形成50μm以上厚度的塗層，與以往的陽極氧化膜形成方法相比，具有耐腐蝕性、硬度、絕緣性等佳的效果。 In addition, the oxalic acid bath, which is a mixed bath of oxalic acid, tartaric acid, organic substances, etc., is used. Unlike the sulfuric acid bath, a lower current is applied to form a thin film that does not cause internal defects in the anodic oxide film, and has high corrosion resistance. However, due to the low thickness, the hardness and insulating properties are low. On the contrary, in the present invention, although a relatively low current is used, a coating layer having a thickness of 50 μm or more can be formed, and compared with the conventional anodic oxide film forming method, it has better effects such as corrosion resistance, hardness, and insulating properties.
因此，本發明的形成有陽極氧化膜的鋁或鋁合金構件，由於按預定比例混合硫酸、乙二酸、酒石酸而形成陽極氧化膜，因而可以使用較低的通入電流，形成50μm以上厚度的塗層，塗層的耐腐蝕性可以提高，製品使用壽命可以延長，由於絕緣性佳，因而可以減小連接於高電壓電源部的半導體裝置或顯示裝置製造裝置的電弧現象的發生率。 Therefore, the anodic oxide film-formed aluminum or aluminum alloy member of the present invention forms an anodic oxide film by mixing sulfuric acid, oxalic acid, and tartaric acid in a predetermined ratio, so that a relatively low current can be used to form a thickness of 50 μm or more. The coating can improve the corrosion resistance of the coating, prolong the service life of the product, and reduce the occurrence of arc phenomenon in the semiconductor device or the display device manufacturing device connected to the high-voltage power supply because of the good insulation.
另外，根據一個實施例，在該a)步驟中，該硫酸、乙二酸及酒石酸的含量按重量比可以為9~11：2.5~3.5：0.3~0.7，該電解液的濃度可以為1至10wt%。 In addition, according to one embodiment, in this a) step, the content of sulfuric acid, oxalic acid and tartaric acid can be 9~11:2.5~3.5:0.3~0.7 by weight, and the concentration of this electrolyte can be 1 to 0.7 10wt%.
其中，當硫酸、乙二酸及酒石酸與該比例相異時，在低電流下難以塗佈耐蝕性及耐電壓性佳的50μm以上的陽極氧化膜。 Among them, when the ratio of sulfuric acid, oxalic acid and tartaric acid is different from this ratio, it is difficult to coat an anodic oxide film of 50 μm or more with good corrosion resistance and withstand voltage at low current.
當硫酸的含量比該比例多時，為了塗佈50μm以上，需要高電流及低電解液溫度，但耐腐蝕性特性會降低，當乙二酸及酒石酸的含量比該比例多時，在低電流下也難以塗佈50μm以上的陽極氧化膜，雖然能夠實現耐腐蝕性佳的塗佈，但耐電壓及硬度會降低。
When the content of sulfuric acid is more than this ratio, in order to
另一方面，當在該b)步驟中形成陽極氧化膜時，通入電流較佳為0.8至1.7A/dm2，電解液的溫度可以為8至22℃。 On the other hand, when the anodic oxide film is formed in this b) step, the passing current is preferably 0.8 to 1.7 A/dm 2 , and the temperature of the electrolytic solution may be 8 to 22°C.
其中，在通入電流不足0.8A/dm2的情況下，難以形成50μm以上的塗佈厚度，塗層的硬度、耐電壓及耐腐蝕性會降低，在超過1.7A/dm2的情況下，塗層的耐電壓及耐腐蝕性會降低。 Among them, when the passing current is less than 0.8A/dm 2 , it is difficult to form a coating thickness of 50 μm or more, and the hardness, withstand voltage and corrosion resistance of the coating layer will decrease, and when it exceeds 1.7A/dm 2 , the The withstand voltage and corrosion resistance of the coating will decrease.
另外，在電解液的溫度超出8℃至22℃的情況下，會發生塗層的耐電壓及耐腐蝕性降低的問題。 In addition, when the temperature of the electrolytic solution exceeds 8°C to 22°C, problems arise in that the withstand voltage and corrosion resistance of the coating layer are lowered.
另外，根據本發明的一個實施例，該陽極氧化膜厚度可以為50μm以上，較佳地，可以為50μm至60μm。 In addition, according to an embodiment of the present invention, the thickness of the anodized film may be 50 μm or more, preferably, 50 μm to 60 μm.
本發明的在鋁或鋁合金構件的表面形成有陽極氧化膜的結構，可以藉由第1圖進行更詳細考查。 The structure in which the anodic oxide film is formed on the surface of the aluminum or aluminum alloy member of the present invention can be examined in more detail with reference to FIG. 1 .
第1圖是顯示出在鋁或鋁合金構件表面形成有陽極氧化膜的概略結構的剖面圖。 FIG. 1 is a cross-sectional view showing a schematic structure in which an anodized film is formed on the surface of an aluminum or aluminum alloy member.
如果將鋁或鋁合金構件4浸於電解液1並通入電流，則最先形成無氣孔3的阻擋(Barrier)層6。如果向形成有阻擋層6的構件4持續通入電流，則使有氣孔3的多孔質層5生長，此時，在與電解液1相接的最上部多孔質層界面2和阻擋層6中，電解液的組分、溫度、通入電流成為左右因生長及侵蝕導致的多孔質層5的氣孔3及池(cell)7的生長結構的因素。
When the aluminum or aluminum alloy member 4 is immersed in the electrolytic solution 1 and an electric current is passed, a
因此，本發明針對先前技術發生的問題，在由硫酸、乙二酸及酒石酸按既定比例混合的電解液中，使氧化膜的氣孔3及池7無缺陷地生長，可以提供半導體或顯示裝置製造裝置的具有佳的耐腐蝕性及絕緣性的陽極氧化膜。
Therefore, the present invention is aimed at the problems that occur in the prior art. In the electrolyte solution mixed by sulfuric acid, oxalic acid and tartaric acid in a predetermined ratio, the
另外，本發明提供一種在其表面上形成有該陽極氧化膜的、以半導體或顯示裝置製造裝置的鋁或鋁合金構件的製造方法而製造的半導體或顯示裝置製造裝置的鋁或鋁合金構件。 In addition, the present invention provides an aluminum or aluminum alloy member of a semiconductor or display device manufacturing device manufactured by a method of manufacturing an aluminum or aluminum alloy member of a semiconductor or display device manufacturing device having the anodized film formed on the surface thereof.
而且，根據本發明，可以製造塗佈有硬度為370~425Hv、耐電壓為1500~2000V的陽極氧化膜的半導體或顯示裝置製造裝置的包含鋁的構件，此時，包含鋁的構件的耐腐蝕性也可以為120分鐘以上。 Furthermore, according to the present invention, it is possible to manufacture an aluminum-containing member of a semiconductor or display device manufacturing apparatus coated with an anodized film having a hardness of 370 to 425 Hv and a withstand voltage of 1500 to 2000 V. In this case, the corrosion resistance of the aluminum-containing member can be produced. Sex can also be more than 120 minutes.
另外，不僅硬度為370~425Hv、耐腐蝕性為120分鐘以上的陽極氧化膜可以塗佈於半導體或顯示裝置製造裝置的構件，而且，耐電壓為1500~2000V、耐腐蝕性為120分鐘以上的陽極氧化膜也可以塗佈於半導體或顯示裝置製造裝置的構件。 In addition, not only an anodized film with a hardness of 370 to 425 Hv and a corrosion resistance of 120 minutes or more can be applied to the components of semiconductor or display device manufacturing equipment, but also a withstand voltage of 1500 to 2000 V and corrosion resistance of 120 minutes or more. The anodic oxide film can also be applied to a member of a semiconductor or display device manufacturing apparatus.
下面根據實施例，更詳細地說明本發明。但是，下述實施例只是對本發明的示例，並非本發明由該實施例所限定。 Hereinafter, the present invention will be described in more detail based on examples. However, the following examples are merely examples of the present invention, and the present invention is not limited by the examples.
[實施例] [Example]
實施例是在本發明的鋁合金表面形成陽極氧化膜者。 Examples are those in which an anodized film is formed on the surface of the aluminum alloy of the present invention.
<實施例1> <Example 1>
首先，將鋁合金(Al6061)試片截斷成縱向50mm*橫向50mm*高度5mm大小而做好準備後，對該試片的表面進行研磨(polishing)，形成既定的表面粗糙度。此時，研磨利用了思高研磨輪(Scotch bright)(#400)，但也可以利用習知的其他技術。在思高研磨輪(Scotch bright)處理時，將試片的表面粗糙度調節為Ra=0.28~0.64μm。 First, an aluminum alloy (Al6061) test piece was cut into a size of 50 mm in length, 50 mm in width, and 5 mm in height to prepare, and then the surface of the test piece was polished to a predetermined surface roughness. At this time, a Scotch bright wheel (#400) was used for grinding, but other known techniques may also be used. During the Scotch bright treatment, the surface roughness of the test piece was adjusted to Ra=0.28~0.64 μm.
然後，在將硫酸(95%硫酸)、乙二酸(100%乙二酸)及酒石酸(99%酒石酸)的重量比按10：3：0.5比例混合的濃度為5wt%電解液(溶劑：DI Water)中，按溫度20℃、通入電流1A/dm2進行陽極氧化處理，獲得了陽極氧化膜，此時，將鋁合金當作陽極(+)，將鉛當作負極(-)。 Then, the concentration of sulfuric acid (95% sulfuric acid), oxalic acid (100% oxalic acid) and tartaric acid (99% tartaric acid) mixed in a ratio of 10:3:0.5 is 5wt% electrolyte (solvent: DI Water), anodizing was carried out at a temperature of 20°C and a current of 1A/dm 2 to obtain an anodized film. At this time, the aluminum alloy was used as the anode (+), and the lead was used as the negative electrode (-).
<實施例2至實施例8> <Example 2 to Example 8>
實施例2至實施例8的陽極氧化膜，除電解液的重量比及陽極氧化處理製程時間之外的其餘條件相同，藉由與該實施例1相同的方法獲得，陽極氧化膜生成條件如下表1記載所示。 The anodic oxide films of Examples 2 to 8, except for the weight ratio of the electrolyte and the anodizing treatment process time, are the same as the remaining conditions, obtained by the same method as in Example 1, and the production conditions of the anodic oxide films are as follows 1 as shown in the record.
<比較例1至比較例8> <Comparative Example 1 to Comparative Example 8>
比較例1至比較例8的陽極氧化膜，除電解液重量比及陽極氧化處理製程時間之外的其餘條件相同，藉由與該實施例1相同的方法獲得，陽極氧化膜生成條件如下表1記載所示。 The anodic oxide films of Comparative Examples 1 to 8, except for the electrolyte weight ratio and the anodizing treatment process time, are the same as the remaining conditions, obtained by the same method as in Example 1, and the production conditions of the anodic oxide films are as follows in Table 1 record shown.
[實驗例1] [Experimental Example 1]
為了確認實施例1至實施例8、比較例1至比較例8的陽極氧化膜的物性，在如下條件下執行了物性分析。物性分析裝備使用了外電流式的厚度測量儀(Positector 6000，Defelsko)、威格士硬度計(HM 810-124K，Mitutoyo)、耐電壓測量儀(HIPOT TESTER 19052，Chroma)。 In order to confirm the physical properties of the anodic oxide films of Examples 1 to 8 and Comparative Examples 1 to 8, physical property analysis was performed under the following conditions. As the physical property analysis equipment, an external current type thickness measuring instrument (Positector 6000, Defelsko), a Vickers hardness tester (HM 810-124K, Mitutoyo), and a withstand voltage measuring instrument (HIPOT TESTER 19052, Chroma) were used.
另外，耐蝕性測試進行了鹽酸氣泡試驗(bubble test)，該鹽酸氣泡試驗使用密封劑將直徑2mm的PVC管附著於試片，以鹽酸5wt%稀釋，加入2ml，測量了最初發生氣泡的時間。 In addition, for the corrosion resistance test, a hydrochloric acid bubble test was performed. In the hydrochloric acid bubble test, a PVC pipe having a diameter of 2 mm was attached to a test piece using a sealant, diluted with 5 wt % hydrochloric acid, and 2 ml was added, and the time until bubbles first occurred was measured.
該實施例1至實施例8、比較例1至比較例8的陽極氧化條件及物性分析結果顯示於表1及第2圖中。 The anodic oxidation conditions and physical property analysis results of Examples 1 to 8 and Comparative Examples 1 to 8 are shown in Table 1 and Figure 2 .
【表1】
從該實施例1至實施例8及比較例1至比較例8的物性分析實驗結果確認，實施例1至實施例4作為將硫酸、乙二酸、酒石酸的重量比固定為10：3：0.5，只變化製程時間的情形，當以150分鐘的製程時間進行時，獲得50μm以上的塗層厚度，硬度、耐電壓及耐腐蝕性佳的。 From the experimental results of physical property analysis of Examples 1 to 8 and Comparative Examples 1 to 8, it was confirmed that the weight ratio of sulfuric acid, oxalic acid, and tartaric acid in Examples 1 to 4 was fixed to 10:3:0.5 , In the case of only changing the process time, when the process time is 150 minutes, a coating thickness of more than 50 μm is obtained, and the hardness, voltage resistance and corrosion resistance are good.
相反，在製程時間不足150分鐘的情況下，可知雖然硬度高，耐腐蝕性好，但無法獲得希望的塗層厚度，耐電壓也降低。在製程時間超過150分鐘的情況下，雖然可以獲得較厚的塗層厚度，但可知硬度、耐電壓及耐腐蝕性與進行150分鐘的試片類似。 Conversely, when the process time was less than 150 minutes, it was found that although the hardness was high and the corrosion resistance was good, the desired coating thickness could not be obtained, and the withstand voltage was also lowered. When the process time exceeds 150 minutes, although a thicker coating thickness can be obtained, it can be seen that the hardness, withstand voltage and corrosion resistance are similar to those of the test piece performed for 150 minutes.
另外，如果比較比較例1至比較例8則可知，如果硫酸的含量增加，則硬度好，但耐電壓及耐腐蝕性特性降低，當硫酸的含量比本發明的重量比小時，確認了硬度雖然類似，但耐電壓及耐腐蝕性特性小幅下降。 In addition, when Comparative Examples 1 to 8 are compared, it can be seen that when the content of sulfuric acid is increased, the hardness is good, but the withstand voltage and corrosion resistance characteristics are reduced. Similar, but the withstand voltage and corrosion resistance characteristics are slightly reduced.
另外，在乙二酸含量減小的情況下，確認了耐腐蝕性降低，相反，當乙二酸及酒石酸的含量比本發明的重量比多時，確認了雖然耐腐蝕性變好，但由於硫酸的含量相對減小，因而硬度降低。 In addition, when the content of oxalic acid was reduced, it was confirmed that the corrosion resistance decreased. On the contrary, when the content of oxalic acid and tartaric acid was larger than the weight ratio of the present invention, it was confirmed that the corrosion resistance was improved, but due to The content of sulfuric acid is relatively reduced, and thus the hardness is reduced.
因此，確認了用於形成陽極氧化膜所需的電解液的硫酸、乙二酸及酒石酸的重量比較佳為9~11：2.5~3.5：0.3~0.7，可以獲得能夠具有50μm以上塗層厚度、適宜的硬度、耐電壓及耐腐蝕性的陽極氧化膜。 Therefore, it was confirmed that the weight ratio of sulfuric acid, oxalic acid, and tartaric acid of the electrolyte required for forming the anodic oxide film is preferably 9~11:2.5~3.5:0.3~0.7, and it is possible to obtain a coating thickness of 50 μm or more, Anodized film with suitable hardness, voltage resistance and corrosion resistance.
另外，第2圖作為實施例3及比較例7的SEM圖像，(a)是測量形成有比較例7的氧化膜的剖面的圖像，(b)是測量形成有實施例3的氧化膜的剖面的圖像。(a)以與原有硫酸法相同的條件形成陽極氧化膜，確認了存在多處缺陷，在(b)中確認了幾乎不存在缺陷。 In addition, FIG. 2 is an SEM image of Example 3 and Comparative Example 7, (a) is an image of a cross section where the oxide film of Comparative Example 7 is formed, and (b) is a measurement of the oxide film of Example 3 formed thereon. image of the cross section. (a) The anodic oxide film was formed under the same conditions as the conventional sulfuric acid method, and it was confirmed that there were many defects, and in (b), it was confirmed that almost no defects were present.
以上詳細記述了本發明內容的特定部分，並非限定於圖式中的例示，這種具體記述只是較佳的實施態樣，並非本發明的範圍限定於此，這是所屬技術領域中具有通常知識者不言而喻的。因此，本發明的實質性範圍由附加的申請專利範圍及其等價物所定義。 The specific part of the content of the present invention is described in detail above, and it is not limited to the illustration in the drawings. This specific description is only a preferred embodiment, and the scope of the present invention is not limited to this, which is a common knowledge in the technical field. is self-evident. Accordingly, the substantial scope of the invention is defined by the appended claims and their equivalents.
1:電解液 1: Electrolyte
2:多孔質層界面 2: Porous layer interface
3:氣孔 3: Stomata
4:構件 4: Components
5:多孔質層 5: Porous layer
6:阻擋層 6: Barrier layer
7:池 7: Pool
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