CN111344836B - Anodic oxidation aluminum-containing member having excellent corrosion resistance and insulating properties, and method for forming oxide film thereof - Google Patents

Anodic oxidation aluminum-containing member having excellent corrosion resistance and insulating properties, and method for forming oxide film thereof Download PDF

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CN111344836B
CN111344836B CN201880072917.9A CN201880072917A CN111344836B CN 111344836 B CN111344836 B CN 111344836B CN 201880072917 A CN201880072917 A CN 201880072917A CN 111344836 B CN111344836 B CN 111344836B
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oxide film
aluminum
semiconductor
corrosion resistance
manufacturing apparatus
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CN111344836A (en
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刘贤喆
郑彩钟
高贤哲
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Komico Ltd
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    • H—ELECTRICITY
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    • 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
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Abstract

The present invention relates to a method for forming an anodized film having excellent corrosion resistance and insulating properties on the surface of an aluminum or aluminum alloy member and an aluminum or aluminum alloy member formed with the anodized film manufactured by the method, and more particularly, to a method for forming an anodized film having high hardness and excellent corrosion resistance and insulating properties without internal defects of an anodized coating, and an internal member for a semiconductor or display manufacturing apparatus coated with the anodized film manufactured by the method.

Description

Anodic oxidation aluminum-containing member having excellent corrosion resistance and insulating properties, and method for forming oxide film thereof
Technical Field
The present invention relates to a method for forming an anodized film having excellent corrosion resistance and insulating properties on the surface of an aluminum or aluminum alloy member and an aluminum or aluminum alloy member formed with the anodized film produced by the method, and more particularly, to a method for forming an anodized film having high hardness and excellent corrosion resistance and insulating properties without internal defects of an anodized coating, and an internal member for a semiconductor and display production apparatus coated with the anodized film produced by the method.
Background
In the field of processes for embodying semiconductor elements and other ultrafine shapes, vacuum plasma equipment is widely used. Examples of the vacuum plasma equipment include PECVD (PLASMA ENHANCED CHEMICAL vapor deposition) equipment for forming a deposition film on a substrate by a chemical vapor deposition method using plasma, sputtering equipment for forming a deposition film by a physical method, dry etching equipment for etching a substrate or a coating substance on a substrate into a desired pattern, and the like, and the vacuum plasma equipment uses high-temperature plasma to embody etching or ultrafine shape of a semiconductor element.
Therefore, a high-temperature plasma is generated inside the vacuum plasma equipment, and the chamber and its internal components are damaged, and specific elements and contaminant particles are generated from the surfaces of the chamber and its components, so that the possibility of contamination inside the chamber is high.
On the other hand, since halogen such as Cl, F, br, or an etchant gas containing O, N, H, S, C elements is introduced as a reaction gas used in a semiconductor manufacturing apparatus, corrosion resistance to the gas is required for a chamber or a member in the chamber, and plasma of halogen is also generated in a process of the semiconductor or liquid crystal manufacturing apparatus, and plasma resistance is also required.
Further, in some parts of the chamber such as the semiconductor etching step, the high-voltage power supply is connected to some parts, and when the insulating property is weak, an arc action occurs, so that excellent non-conductivity is required.
On the other hand, aluminum is mainly used as a material used for semiconductor equipment due to conductivity, ease of manufacture, and availability at a reasonable price.
However, aluminum readily reacts with halogens such as chlorine, fluorine and bromine to form AlCl3, al2Cl6, alF3 or AlBr3. The aluminum-fluorine compound, which is peeled from the surface of the processing apparatus component and induces corrosion of the component itself, can act as a source of particulate contamination of the processing chamber (and components fabricated within the chamber).
In addition, many compounds containing aluminum and chlorine, many compounds containing aluminum and bromine are volatile, and gases are generated under semiconductor processing conditions, which leave the aluminum substrate. Thus, spaces are formed within the structure that cause structural instability, creating a surface with problematic integrity.
Therefore, as a preferred means for protecting the aluminum surface in the semiconductor device, there is an anodic aluminum oxide coating method, which is an electrolytic oxidation step of forming a monolithic coating layer composed of a relatively porous aluminum oxide on the aluminum surface.
As a method of forming the anodic oxide film, a method of controlling an electrolyte at a low temperature or a method of performing electrolysis with a high current density is used, but if the anodic oxide film is formed by these methods, there is a tendency that occurrence of cracks of the anodic oxide film increases, and there is a problem that these methods require high energy consumption.
As a conventional technique for forming an anodic oxide film, japanese patent publication No. 4660760 (1/14/2011) proposes a method for forming a highly hard anodic oxide film using a sulfuric acid-based electrolyte to which ethanol is added. However, the above-mentioned conventional document has a problem in that the control of the change in the concentration of ethanol in the electrolyte solution due to the anodic oxidation treatment is complicated.
In addition, korean patent publication No. 10-0664900 (1.4.2007) proposes a method of anodizing a surface treatment using an electrolyte in which oxalic acid is added to sulfuric acid in a small amount. However, the above-mentioned conventional document is an anodizing treatment condition for obtaining an oxide film thickness of 50 μm to 60 μm in a semiconductor manufacturing apparatus, but a high current is applied to form a film of a desired thickness, and thus there is a problem that defects occur in a plurality of places in a coating layer, and corrosion resistance is lowered.
Accordingly, although there is a technical development as described above, there is still a strong need to continuously develop a surface treatment method of an aluminum or aluminum alloy material semiconductor device capable of improving corrosion resistance and insulation properties of the semiconductor device.
Disclosure of Invention
Technical problem
The main object of the present invention is to provide a method for producing an anodized aluminum or aluminum alloy member excellent in corrosion resistance and insulating properties of a gas used in a semiconductor production process, and a surface-treated semiconductor device.
Technical proposal
In order to achieve the above object, the present invention provides a method for forming an oxide film of an aluminum-containing member of a semiconductor or display manufacturing apparatus, as a method for forming an oxide film of an aluminum-containing member of a semiconductor or display manufacturing apparatus having an anodic oxide film formed on a surface thereof, comprising: a) A step of mixing sulfuric acid, oxalic acid and tartaric acid to produce an electrolyte; and b) a step of forming an anodic oxide film on the surface of the aluminum or aluminum alloy member using the electrolyte produced in the step a).
According to one embodiment, in the step a, the content of the sulfuric acid, oxalic acid and tartaric acid may be 9 to 11:2.5 to 3.5:0.3 to 0.7.
In addition, according to one embodiment, the concentration of the electrolyte may be 1wt% to 10wt%.
In addition, according to one embodiment, when the anodic oxide film is formed in the b), the current may be supplied at 0.8A/dm2 to 1.7A/dm2, and the temperature of the electrolyte may be 8 ℃ to 22 ℃.
In addition, according to one embodiment, the anodic oxide film thickness may be 50 μm to 60 μm.
In another aspect, the present invention provides an aluminum or aluminum alloy member of a semiconductor or display manufacturing apparatus manufactured by the oxide film forming method of the member including aluminum of the semiconductor or display manufacturing apparatus.
The present invention can provide a member containing aluminum for a semiconductor or display manufacturing apparatus coated with an anodic oxide film having a hardness of 370 to 425Hv and a withstand voltage of 1500 to 2000V, which can have a corrosion resistance of 120 minutes or more.
The present invention can provide not only a member containing aluminum for a semiconductor or display manufacturing apparatus coated with an anodic oxide film having a hardness of 370 to 425Hv and a corrosion resistance of 120 minutes or more, but also a member containing aluminum for a semiconductor or display manufacturing apparatus coated with an anodic oxide film having a withstand voltage of 1500 to 2000V and a corrosion resistance of 120 minutes or more.
Advantageous effects
The method for forming an anodized film on the surface of an aluminum or aluminum alloy member, which is excellent in corrosion resistance and insulation properties, has the effect of enabling the formation of a coating thickness of 50 μm or more without internal defects of the anodized coating.
Further, the gas used in the semiconductor manufacturing apparatus has an effect of excellent corrosion resistance and excellent insulating property against high voltage in the chamber of the semiconductor manufacturing apparatus.
Drawings
Fig. 1 is a cross-sectional view showing a schematic structure of forming an anodic oxide film on the surface of an aluminum or aluminum alloy member.
Fig. 2 is SEM images of example 3 and comparative example 7, (a) is an image of a cross section of the oxide film of comparative example 7, and (b) is an image of a cross section of the oxide film of example 3.
Symbol description
1: Electrolyte 4: aluminum-containing member
7: Membrane cell 2: porous layer interface
5: Porous layer 3: air holes
6: Barrier layer
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Generally, nomenclature used in this specification is well known and commonly employed in the art.
In the present application, when a certain component is referred to as "comprising" in the present specification, unless otherwise specified, it means that other components are not excluded and other components may be included.
The present invention relates to a method for manufacturing an aluminum or aluminum alloy member of a semiconductor or display manufacturing apparatus having an anodized film formed on a surface thereof, the method comprising the steps of: a) A step of mixing sulfuric acid, oxalic acid and tartaric acid to produce an electrolyte; and b) a step of forming an anode on the surface of the aluminum or aluminum alloy member using the electrolyte produced in the step a).
In order to produce the anodized film-formed aluminum or aluminum alloy member of the present invention, an electrolyte solution in which sulfuric acid, oxalic acid, tartaric acid are mixed is used, and the anodized film can be formed to 50 μm or more even if a low current is applied thereto, as compared with a conventional sulfuric acid solution using a mixed solution in which sulfuric acid, oxalic acid, an organic substance, etc. are added, and internal defects of the anodized film are not generated by using a current applied thereto, and corrosion resistance is improved.
Further, an oxalic acid solution to which a mixed solution of oxalic acid, tartaric acid, an organic substance, and the like is added is used, and a low current is applied unlike sulfuric acid solution, so that a film which does not cause internal defects of an anodic oxide film is formed, and the anodic oxide film has high corrosion resistance, but has low hardness and insulation characteristics due to a low thickness. In contrast, in the present invention, although a low current is applied, a coating layer having a thickness of 50 μm or more can be formed, and the present invention has excellent effects such as corrosion resistance, hardness, and insulating properties as compared with the conventional anodic oxide film forming method.
Therefore, the anodized film-formed aluminum or aluminum alloy member of the present invention can be formed by mixing sulfuric acid, oxalic acid, and tartaric acid at a predetermined ratio, and thus can be coated with a coating layer having a thickness of 50 μm or more at a low current, can have improved corrosion resistance, can have an extended product life, and can be reduced in the occurrence of arcing in a semiconductor device or a display manufacturing device connected to a high-voltage power supply unit due to excellent insulating properties.
In addition, according to one embodiment, in the step a, the content of the sulfuric acid, oxalic acid and tartaric acid may be 9 to 11:2.5 to 3.5:0.3 to 0.7, and the concentration of the electrolyte may be 1wt% to 10wt%.
Wherein when sulfuric acid, oxalic acid and tartaric acid are different from the above ratios, it is difficult to coat an anodized film of 50 μm or more excellent in corrosion resistance and withstand voltage characteristics at a low current.
When the content of sulfuric acid is more than the above ratio, high current and low electrolyte temperature are required for coating 50 μm or more, but corrosion resistance characteristics are low, and when the content of oxalic acid and tartaric acid is more than the above ratio, it is difficult to coat an anodic oxide film of 50 μm or more at low current, and although coating excellent in corrosion resistance can be achieved, withstand voltage and hardness are low.
On the other hand, when the anodic oxide film is formed in the step b), the current is preferably 0.8A/dm 2 to 1.7A/dm 2, and the temperature of the electrolyte may be 8℃to 22 ℃.
When the current is less than 0.8A/dm 2, it is difficult to form a coating thickness of 50 μm or more, and the hardness, voltage resistance and corrosion resistance of the coating layer are low, and when it exceeds 1.7A/dm 2, the voltage resistance and corrosion resistance of the coating layer are low.
In addition, when the temperature of the electrolyte exceeds 8 ℃ to 22 ℃, the problem of low withstand voltage and corrosion resistance of the coating occurs.
In addition, according to an embodiment of the present invention, the anodic oxide film thickness may be 50 μm or more, and more preferably, may be 50 μm to 60 μm.
The structure of the present invention in which an anodic oxide film is formed on the surface of an aluminum or aluminum alloy member can be examined in more detail with reference to fig. 1.
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.
If the member 4 containing aluminum is immersed in the electrolyte 1 and a current is applied, a Barrier layer 6 free of pores 3 is formed first. If a current is continuously supplied to the member 4 containing aluminum on which the barrier layer 6 is formed, the porous layer 5 having pores 3 is grown, and at this time, the composition, temperature, and current supply of the electrolyte solution become factors of the growth structure of the pores 3 and the membrane cells 7 of the porous layer 5 due to the generation and erosion in the uppermost porous layer interface 2 and the barrier layer 6 which are in contact with the electrolyte solution 1.
Accordingly, the present invention is directed to solving the problems occurring in the prior art, and can provide an anodized film having excellent corrosion resistance and insulating properties for a semiconductor or display manufacturing apparatus by growing the pores 3 and cells 7 of the oxide film without defects in an electrolyte solution prepared by mixing sulfuric acid, oxalic acid and tartaric acid at a predetermined ratio.
The present invention also provides an aluminum or aluminum alloy member for a semiconductor or display manufacturing apparatus manufactured by the method for manufacturing an aluminum or aluminum alloy member for a semiconductor or display manufacturing apparatus, in which the anodized film is formed on the surface thereof.
Further, according to the present invention, a member containing aluminum of a semiconductor or display manufacturing apparatus coated with an anodic oxide film having a hardness of 370 to 425Hv and a withstand voltage of 1500 to 2000V can be manufactured, and in this case, the corrosion resistance of the member containing aluminum may be 120 minutes or more.
In addition, not only an anodic oxide film having a hardness of 370 to 425Hv and a corrosion resistance of 120 minutes or more may be applied to a member of a semiconductor or display manufacturing apparatus, but also an anodic oxide film having a withstand voltage of 1500 to 2000V and a corrosion resistance of 120 minutes or more may be applied to a member of a semiconductor or display manufacturing apparatus.
The present invention will be described in more detail with reference to examples. The following examples are merely illustrative of the present invention and are not intended to limit the scope of the present invention.
[ Example ]
In the embodiment, an anodic oxide film is formed on the surface of the aluminum alloy of the present invention.
Example 1 ]
First, an aluminum alloy (Al 6061) test piece was cut into a size of 50mm in the longitudinal direction, 50mm in the transverse direction, and 5mm in the height, and then the surface of the test piece was polished to a predetermined surface roughness. In this case, a Scotch tape (Scotch tape) (# 400) is used for polishing, but other known techniques may be used. At the time of the high grinding wheel (Scotch brite) treatment, the surface roughness of the test piece was adjusted to ra=0.28 μm to 0.64 μm.
Then, the weight ratio of sulfuric acid (95% sulfuric acid), oxalic acid (100% oxalic acid) and tartaric acid (99% tartaric acid) was 10:3: the anodic oxidation treatment was carried out in a mixed amperometric solution (solvent: deionized water (DI water)) having a concentration of 5wt% at a ratio of 0.5 at a temperature of 20℃under a current of 1A/dm 2 to obtain an anodic oxide film, and at this time, aluminum was used as an anode (+) and lead was used as a cathode (-).
< Example 2 to example 8>
The anodic oxide films of examples 2 to 8 were obtained in the same manner as in example 1 except that the weight ratio of the electrolyte and the time of the anodic oxidation treatment process were the same, and the anodic oxide film formation conditions were as shown in table 1 below.
Comparative examples 1 to 8 ]
The anodic oxide films of comparative examples 1 to 8 were obtained in the same manner as in example 1 except that the weight ratio of the electrolyte and the time of the anodic oxidation treatment step were the same, and the anodic oxide film formation conditions were as shown in table 1 below.
[ Example 1]
In order to confirm the physical properties of the anodized 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, a thickness gauge (Positector 6000, diefshi (DeFelsko)), a wegener's hardness tester (HM 810-124K, three-quarter corporation), and a withstand voltage gauge (HIPOT TESTER 19052, chroma) were used.
Further, a hydrochloric acid bubble test (bubble test) was performed in which a PVC tube having a diameter of 2mm was attached to a test piece using a sealant, diluted to 5wt% with hydrochloric acid, and 2ml was added to measure the time for initial bubble generation.
The anodizing conditions and physical property analysis results of examples 1 to 8 and comparative examples 1 to 8 are shown in the following tables 1 and 2.
TABLE 1
Physical property analysis experimental results of the examples 1 to 8 and the comparative examples 1 to 8, wherein the weight ratio of sulfuric acid, oxalic acid and tartaric acid was fixed to 10 in the examples 1 to 4: 3:0.5, it was confirmed that when the process time was 150 minutes, a coating thickness of 50 μm or more was obtained, and the hardness, withstand voltage and corrosion resistance were excellent.
In contrast, when the process time is less than 150 minutes, although the hardness is high and the corrosion resistance is good, the desired coating thickness cannot be obtained, and it is found that the withstand voltage is also low. In the case where the process time exceeds 150 minutes, although a thicker coating thickness can be obtained, it is known that the hardness, voltage resistance and corrosion resistance are similar to those of a test piece which is subjected to 150 minutes.
In addition, as is clear from comparative examples 1 to 8, if the content of sulfuric acid is increased, the hardness is good, but the withstand voltage and corrosion resistance characteristics are low, and when the content of sulfuric acid is smaller than the weight ratio of the present invention, it is confirmed that the hardness is similar but the withstand voltage and corrosion resistance characteristics are slightly lowered.
In addition, when the oxalic acid content was decreased, it was confirmed that the corrosion resistance was low, whereas when the oxalic acid and tartaric acid contents were more than the weight ratio of the present invention, it was confirmed that the corrosion resistance was improved, but the hardness was low due to the relative decrease in the sulfuric acid content.
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 to 11:2.5 to 3.5: from 0.3 to 0.7, an anodized film having a coating thickness of 50 μm or more, and suitable hardness, voltage resistance and corrosion resistance can be obtained.
Fig. 2 is an SEM image of example 3 and comparative example 7, (a) is an image of a cross section of the oxide film of comparative example 7, and (b) is an image of a cross section of the oxide film of example 3. (a) The anodic oxide film was formed under the same conditions as in the conventional sulfuric acid method, and it was confirmed that there were many defects, and in (b), it was confirmed that there were almost no defects.
The specific portions of the present invention are described in detail above, and are not limited to the exemplary illustrations of the drawings, and the technical description is only a preferred embodiment, and the scope of the present invention is not limited thereto, as will be apparent to those of ordinary skill in the art. Accordingly, the substantial scope of the invention is defined by the appended claims and equivalents thereof.

Claims (5)

1. An oxide film forming method of an aluminum-containing member of a semiconductor or display manufacturing apparatus, comprising:
a) A step of mixing sulfuric acid, oxalic acid and tartaric acid to produce an electrolyte; and
B) A step of forming an anodic oxide film on the surface of the aluminum or aluminum alloy member using the electrolyte produced in the step a):
In the step a), the weight ratio of the content of sulfuric acid, oxalic acid and tartaric acid is 9-11 when the concentration of the electrolyte is 1wt% to 10 wt%: 2.5 to 3.5:0.3 to 0.7 percent of the total weight of the composite,
When the anodic oxide film is formed in the step b), the current is connected between 0.8A/dm 2 and 1.7A/dm 2,
Wherein the anodic oxide film is formed for 150 minutes or longer,
In the method of forming the anodic oxide film, the content ratio of the electrolytic solution, the on-current, and the formation time are simultaneously satisfied.
2. The method for forming an oxide film of an aluminum-containing member of a semiconductor or display manufacturing apparatus according to claim 1, wherein,
The temperature of the electrolyte is 8 ℃ to 22 ℃.
3. The method for forming an oxide film of an aluminum-containing member of a semiconductor or display manufacturing apparatus according to claim 1, wherein,
The anodic oxide film has a thickness of 50 μm to 60 μm.
4. A member comprising aluminum for a semiconductor or display manufacturing apparatus having an anodized film formed on a surface thereof by the method of any one of claims 1 to 3.
5. The member containing aluminum of the semiconductor or display manufacturing apparatus having an anodized film formed on the surface thereof according to claim 4, wherein the member containing aluminum of the semiconductor or display manufacturing apparatus is coated with an anodized film having a hardness of 370 to 425Hv, a withstand voltage of 1500 to 2000V, and a corrosion resistance of 120 minutes or more.
CN201880072917.9A 2017-12-11 2018-07-17 Anodic oxidation aluminum-containing member having excellent corrosion resistance and insulating properties, and method for forming oxide film thereof Active CN111344836B (en)

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