CN114836805A - Aluminum alloy surface treatment method - Google Patents
Aluminum alloy surface treatment method Download PDFInfo
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- CN114836805A CN114836805A CN202210454762.3A CN202210454762A CN114836805A CN 114836805 A CN114836805 A CN 114836805A CN 202210454762 A CN202210454762 A CN 202210454762A CN 114836805 A CN114836805 A CN 114836805A
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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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
- 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
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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Abstract
An aluminum alloy surface treatment method comprises the following steps: the method comprises the following steps of matrix surface pretreatment, micro-arc oxidation electrolyte preparation, micro-arc oxidation treatment and hole sealing, wherein the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and ethylene diamine tetraacetic acid disodium salt, and a steeping fluid used in the hole sealing process comprises sodium acetate, nano titanium powder, nano graphene and sodium silicate; by changing the components of the micro-arc oxidation electrolyte and the impregnation liquid, a composite structure layer is formed on the surface of the matrix, and the wear resistance and corrosion resistance of the surface of the matrix are improved.
Description
Technical Field
The invention relates to the technical field of material surface processing, in particular to an aluminum alloy surface treatment method.
Background
Micro-arc oxidation, which is a method for enhancing and activating the reaction generated on an anode by utilizing arc discharge on the basis of common anodic oxidation so as to form a high-quality strengthened ceramic membrane on the surface of a workpiece made of metals such as aluminum, titanium, silicon and the like and alloys thereof, is characterized in that a special micro-arc oxidation power supply is used for applying voltage on the workpiece, so that the metal on the surface of the workpiece interacts with an electrolyte solution to form micro-arc discharge on the surface of the workpiece, and the ceramic membrane is formed on the surface of the metal under the action of factors such as high temperature, electric field and the like, thereby achieving the purpose of strengthening the surface of the workpiece.
The traditional preparation process of the micro-arc oxidation ceramic layer is to prepare the micro-arc oxidation ceramic layer by micro-arc oxidation under the condition of constant current or constant voltage, although the micro-arc oxidation ceramic layer can protect a substrate to a certain extent, the performance of the obtained coating cannot reach the optimal performance, and the ceramic layer still has better corrosion resistance and wear resistance by improving the preparation process.
Disclosure of Invention
In order to solve the above problems, the present application provides a method for treating an aluminum alloy surface, comprising the steps of: the method comprises the steps of matrix surface pretreatment, micro-arc oxidation electrolyte preparation, micro-arc oxidation treatment and hole sealing, wherein the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and ethylene diamine tetraacetic acid disodium salt, and a steeping fluid used in the hole sealing process comprises sodium acetate, nano titanium powder, nano graphene and sodium silicate.
Further, the method sequentially comprises the following steps:
(1) pretreatment of the surface of a substrate: polishing, impurity removal and degreasing treatment are carried out on the surface of the aluminum alloy substrate;
the surface of the matrix is pretreated to remove burrs on the surface of the aluminum alloy matrix and remove surface pollution and oil stains caused by the smelting process;
(2) preparing micro-arc oxidation electrolyte: adding silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and ethylene diamine tetraacetic acid disodium salt into deionized water, and performing ultrasonic dispersion;
the ultrasonic dispersion time is at least 3 hours, so that substances in the micro-arc oxidation electrolyte are fully dispersed;
(3) micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte for micro-arc oxidation;
in the micro-arc oxidation process, the nano graphene plays a conductive role;
disodium ethylene diamine tetraacetate is used as a complexing agent;
sodium hydroxide provides an alkaline environment;
(4) hole sealing: putting the material subjected to micro-arc oxidation treatment into a leaching solution for leaching, and then cleaning and drying;
in the hole sealing process, the nano graphene plays a role in loading, tiny holes and cracks generated by the ceramic membrane in the micro-arc oxidation process are filled, and the corrosion resistance is improved.
Further, the micro-arc oxidation electrolyte comprises 1.5-1.8 parts of silicate, 2.5-3.2 parts of manganese powder, 3.5-5.5 parts of silicon powder, 2-4 parts of silicon carbide particles, 0.4-0.8 part of nano graphene, 0.5-0.6 part of sodium hydroxide and 1.2-1.3 parts of disodium ethylene diamine tetraacetate.
Further, the silicate is sodium silicate, the particle size of the sodium silicate is 50-80 nm, the particle size of the silicon carbide particles is 10-20 microns, the particle size of the manganese powder is 2-10 microns, and the particle size of the silicon powder is 2-10 microns.
During the micro-arc oxidation process, silicon carbide particles, manganese powder and silicon powder with larger particle sizes can be precipitated to a certain degree and are precipitated on the surface of the aluminum alloy substrate, and due to the high temperature of micro-arc oxidation, all the components are fused and mixed together.
Further, the micro-arc oxidation is carried out, wherein the substrate material is used as an anode and is connected with a lead, the voltage of the micro-arc oxidation is 300-350V, the forward duty ratio is less than 25%, and the total time of the micro-arc oxidation is 3 min.
Further, during micro-arc oxidation, the temperature of the micro-arc oxidation electrolyte is 5-10 ℃.
The micro-arc oxidation time is short, and the stable formation of the ceramic layer is more facilitated due to the low temperature of the electrolyte.
Further, the impregnation liquid comprises 1.0-1.5 parts of sodium acetate, 0.3-0.5 part of nano titanium powder, 0.3-0.8 part of nano graphene and 1.0-1.2 parts of sodium silicate.
Further, the dipping temperature is 50 ℃, the dipping time is 5-7 hours, the drying temperature is 60-65 ℃, and the drying time is 20-24 hours.
Further, a composite structure layer is formed on the surface of the aluminum alloy substrate, and the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
Furthermore, the thickness of the prepared composite structure layer is less than 30 μm.
The micro-arc oxidation time is short, the formed composite structure layer is thin, but the formed composite structure layer is uniform in component and stable in performance.
This application can bring following beneficial effect:
1. according to the method, the components of the micro-arc oxidation electrolyte and the impregnation liquid are changed, so that a composite structure layer is formed on the surface of the matrix, and the wear resistance and corrosion resistance of the surface of the matrix are improved.
2. According to the method, the nano graphene is added into the micro-arc oxidation electrolyte, and the electrochemical performance of the electrolyte is improved by utilizing the conductivity of the nano graphene.
3. According to the micro-arc oxidation electrolyte, silicon carbide particles are added into the micro-arc oxidation electrolyte, so that the silicon carbide particles enter the ceramic layer, and the wear resistance is improved.
4. According to the method, in the hole sealing process, the tiny holes and cracks of the ceramic membrane are filled by utilizing the loading property of the nano graphene, the filling effect is better, and the performance of the composite structure layer is improved.
5. The ceramic layer formed by the method is stable by using low-temperature electrolyte and shorter micro-arc oxidation time, and the generated micro holes and cracks are fewer.
6. According to the method, the instantaneous high temperature generated during micro-arc oxidation is utilized, so that silicon and manganese are doped into the aluminum alloy, and a composite structure layer is formed by matching the generated ceramic layer, so that the wear resistance and corrosion resistance of the surface of the aluminum alloy substrate are improved.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present application will be explained in detail through the following embodiments.
In a specific embodiment of the present application, the base material used is 5052 aluminum alloy.
Example 1:
the composite structure layer is produced according to the following steps, which sequentially comprise the following steps:
(1) pretreatment of the surface of a substrate: polishing the surface of the substrate by using abrasive paper, and cleaning the surface of the substrate by using absolute ethyl alcohol and deionized water after the treatment is finished;
(2) preparing micro-arc oxidation electrolyte: adding 1.5 parts of sodium silicate with the particle size of 50nm, 0.5 part of sodium hydroxide, 0.4 part of nano graphene, 2.5 parts of manganese powder with the particle size of 2-10 microns, 3.5 parts of silicon powder with the particle size of 2-10 microns, 2 parts of silicon carbide particles with the particle size of 10-20 microns and 1.2 parts of disodium ethylenediamine tetraacetic acid into 1000 parts of deionized water, and ultrasonically dispersing for 3 hours;
(3) micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte, connecting the substrate material serving as an anode with a lead, wherein the temperature of the micro-arc oxidation electrolyte is 5 ℃, the voltage of micro-arc oxidation is 300V, the forward duty ratio is less than 25%, and the total micro-arc oxidation time is 3 min;
(4) hole sealing: and (3) putting the material subjected to micro-arc oxidation treatment into a soaking solution containing 1000 parts of deionized water, 1.0 part of sodium acetate, 0.3 part of nano titanium powder, 0.3 part of nano graphene and 1.0 part of sodium silicate, soaking at the temperature of 50 ℃ for 5 hours, and then cleaning and drying at the temperature of 60 ℃ for 20 hours.
It can be understood that a composite structure layer is formed on the surface of the aluminum alloy substrate, and the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structure layer produced is less than 30 μm thick.
Example 2:
the composite structure layer is produced according to the following steps, which sequentially comprise the following steps:
(1) pretreatment of the surface of a substrate: polishing the surface of the substrate by using abrasive paper, and cleaning the surface of the substrate by using absolute ethyl alcohol and deionized water after the treatment is finished;
(2) preparing micro-arc oxidation electrolyte: adding 1.6 parts of sodium silicate with the diameter of 70nm, 0.55 part of sodium hydroxide, 0.6 part of nano graphene, 3 parts of manganese powder with the particle size of 2-10 microns, 4 parts of silicon powder with the particle size of 2-10 microns, 3 parts of silicon carbide particles with the particle size of 10-20 microns and 1.25 parts of ethylene diamine tetraacetic acid disodium salt into 1000 parts of deionized water, and ultrasonically dispersing for 3 hours;
(3) micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte, connecting the substrate material serving as an anode with a lead, wherein the temperature of the micro-arc oxidation electrolyte is 8 ℃, the voltage of micro-arc oxidation is 320V, the forward duty ratio is less than 25%, and the total micro-arc oxidation time is 3 min;
(4) hole sealing: and (3) putting the material subjected to micro-arc oxidation treatment into a soaking solution containing 1000 parts of deionized water, 1.25 parts of sodium acetate, 0.4 part of nano titanium powder, 0.5 part of nano graphene and 1.1 part of sodium silicate, soaking at the temperature of 50 ℃ for 6 hours, cleaning and drying at the temperature of 62 ℃ for 22 hours.
It can be understood that a composite structure layer is formed on the surface of the aluminum alloy substrate, and the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structure layer produced is less than 30 μm thick.
Example 3:
the composite structure layer is produced according to the following steps, which sequentially comprise the following steps:
(1) pretreatment of the surface of a matrix: polishing the surface of the substrate by using abrasive paper, and cleaning the surface of the substrate by using absolute ethyl alcohol and deionized water after the treatment is finished;
(2) preparing micro-arc oxidation electrolyte: adding 1.8 parts of sodium silicate with the particle size of 80nm, 0.6 part of sodium hydroxide, 0.8 part of nano graphene, 3.2 parts of manganese powder with the particle size of 2-10 microns, 5.5 parts of silicon powder with the particle size of 2-10 microns, 4 parts of silicon carbide particles with the particle size of 10-20 microns and 1.3 parts of disodium ethylenediamine tetraacetic acid into 1000 parts of deionized water, and ultrasonically dispersing for 3 hours;
(3) micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte, connecting the substrate material serving as an anode with a lead, wherein the temperature of the micro-arc oxidation electrolyte is 10 ℃, the voltage of micro-arc oxidation is 350V, the forward duty ratio is less than 25%, and the total micro-arc oxidation time is 3 min;
(4) hole sealing: and (3) putting the material subjected to micro-arc oxidation treatment into a soaking solution containing 1000 parts of deionized water, 1.5 parts of sodium acetate, 0.5 part of nano titanium powder, 0.8 part of nano graphene and 1.2 parts of sodium silicate, soaking at the temperature of 50 ℃ for 7 hours, cleaning and drying at the temperature of 65 ℃ for 24 hours.
It can be understood that a composite structure layer is formed on the surface of the aluminum alloy substrate, and the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structure layer produced is less than 30 μm thick.
Comparative example:
comparative example the setup was carried out with reference to example 1, except that the other conditions were the same as in example 1.
TABLE 1
And (3) detecting data:
(1) test of Corrosion resistance
The test means is as follows: the electrochemical workstation was used to test the tafel curves of the samples.
And (3) testing conditions are as follows: a three-electrode system is adopted, an auxiliary electrode is a platinum electrode, a reference electrode is a saturated calomel electrode, a sample to be tested is taken as a research electrode, and a test medium is a 3% NaCl aqueous solution.
Because the adopted treatment modes are approximately the same, the corrosion currents of all the materials are approximately the same, and the corrosion resistance of the materials is mainly reflected on the corrosion potential under the condition that the corrosion currents are not different, and the higher the corrosion potential is, the better the corrosion resistance of the materials is.
TABLE 2
(2) Abrasion resistance test
The test means is as follows: an MXD-02 friction coefficient instrument of Labthink blue light is adopted.
And (3) testing conditions are as follows: the test was carried out according to GB/T10006-1988 to test the coefficient of friction.
The test means is as follows: a PHASE II micro vickers hardness tester was used.
And (3) testing conditions are as follows: the hardness of the alloy is tested according to the GB/T4340.3-2012 standard and tested according to the Vickers hardness.
TABLE 3
(3) Stability test
The test means is as follows: the method is carried out by adopting an MRH-2 type high-speed ring block abrasion tester.
And (3) testing conditions are as follows: the temperature is room temperature, the relative humidity is 50%, the rotating speed is 200r/min, the load is 100N, after 2 hours, 4 hours and 6 hours of friction, the test is carried out according to the method used in the corrosion resistance test (1) and the wear resistance test (2).
TABLE 4
From the result of the test data, in the micro-arc oxidation process, the corrosion resistance of the composite structure layer can be improved by adding the silicon powder and the manganese powder, and the wear resistance of the composite structure layer can be improved by adding the silicon carbide and the nano graphene.
In the dipping process, the corrosion resistance can be improved by adding the nano graphene and the titanium powder, and the wear resistance can be improved by adding the sodium silicate.
Comparative example 9 is an original aluminum alloy, and the original aluminum alloy without surface treatment has a very low corrosion potential and a very low vickers hardness as compared to the other treated examples or comparative examples.
When the friction coefficient of the comparative example 9 is tested, the tested data is the friction coefficient of the original aluminum alloy, the influence factor is mainly the roughness of the surface of the original aluminum alloy, and the reference value of the experimental data is not large.
Compared with the comparative example 5 and the example 1, the performance of the obtained composite structure layer is reduced due to overlong electrolysis time, the electrolysis time is overlong, so that the micro holes and cracks in the formed ceramic layer are increased, after the composite structure layer with a certain thickness is formed, the components are reduced in the subsequently formed structure, the comprehensive performance is reduced, and due to the defects in the micro-arc oxidation process, the performance of the subsequently formed film layer cannot reach the required standard easily.
In the stability test, the composite structure layer formed on the surface of the base material is abraded after long-time friction in the embodiment 1 and the comparative example 5, and the composite structure layer formed in the embodiment 1 is thin, so that the composite structure layer in the embodiment 1 is basically damaged after 6 hours of abrasion, and the performances of the composite structure layer are not greatly different from those of the aluminum alloy base material.
Comparative example 5 is long in micro-arc oxidation time, the formed composite structure layer is thick, but the micro-arc oxidation time is too long, the formed composite structure layer has increased micro holes and cracks, the obtained composite structure layer has poor performance, after a period of abrasion, part of the composite structure layer with poor external comprehensive performance of the composite structure layer is ground away, the composite structure layer with fewer internal holes and cracks and excellent performance is exposed, so that after 6 hours of an abrasion experiment in comparative example 5, the measured experimental data is better than the initially measured data, and various performances are excellent.
The steps used in the present application are indispensable and have an effect on the properties of the final composite structure layer, as seen by comparative examples 9 and 10 and example 1.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. The aluminum alloy surface treatment method is characterized by comprising the following steps: pretreating the surface of a substrate, preparing a micro-arc oxidation electrolyte, carrying out micro-arc oxidation treatment, and sealing holes;
the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano-graphene, silicon powder, manganese powder, silicon carbide particles and ethylene diamine tetraacetic acid disodium salt, and the impregnation liquid used in the hole sealing process comprises sodium acetate, nano-titanium powder, nano-graphene and sodium silicate.
2. The aluminum alloy surface treatment method according to claim 1, comprising the steps of, in order:
(1) pretreatment of the surface of a substrate: polishing, impurity removal and degreasing treatment are carried out on the surface of the aluminum alloy substrate;
(2) preparing micro-arc oxidation electrolyte: adding silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and ethylene diamine tetraacetic acid disodium salt into deionized water, and performing ultrasonic dispersion;
(3) micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte for micro-arc oxidation;
(4) hole sealing: and (3) putting the material subjected to micro-arc oxidation treatment into a leaching solution for leaching, and then cleaning and drying.
3. The surface treatment method for an aluminum alloy according to claim 1, characterized in that: the micro-arc oxidation electrolyte comprises 1.5-1.8 parts of silicate, 2.5-3.2 parts of manganese powder, 3.5-5.5 parts of silicon powder, 2-4 parts of silicon carbide particles, 0.4-0.8 part of nano graphene, 0.5-0.6 part of sodium hydroxide and 1.2-1.3 parts of ethylene diamine tetraacetic acid disodium salt.
4. The surface treatment method of an aluminum alloy according to claim 1, characterized in that: the silicate is sodium silicate, the particle size of the sodium silicate is 50-80 nm, the particle size of the silicon carbide particles is 10-20 microns, the particle size of the manganese powder is 2-10 microns, and the particle size of the silicon powder is 2-10 microns.
5. The surface treatment method of an aluminum alloy according to claim 1, characterized in that: and in the micro-arc oxidation, the substrate material is used as an anode and is connected with a wire, the voltage of the micro-arc oxidation is 300-350V, the forward duty ratio is less than 25%, and the total time of the micro-arc oxidation is 3 min.
6. The surface treatment method of an aluminum alloy according to claim 1, characterized in that: during micro-arc oxidation, the temperature of the micro-arc oxidation electrolyte is 5-10 ℃.
7. The surface treatment method of an aluminum alloy according to claim 1, characterized in that: the impregnation liquid comprises 1.0-1.5 parts of sodium acetate, 0.3-0.5 part of nano titanium powder, 0.3-0.8 part of nano graphene and 1.0-1.2 parts of sodium silicate.
8. The surface treatment method of an aluminum alloy according to claim 1, characterized in that: the dipping temperature is 50 ℃, the dipping time is 5-7 h, the drying temperature is 60-65 ℃, and the drying time is 20-24 h.
9. The surface treatment method of an aluminum alloy according to any one of claims 1 to 8, characterized in that: and forming a composite structure layer on the surface of the aluminum alloy substrate, wherein the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
10. The surface treatment method of an aluminum alloy according to claim 9, characterized in that: the thickness of the prepared composite structure layer is less than 30 mu m.
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