CN113514011A - Method for rapidly judging roughness of metal film - Google Patents
Method for rapidly judging roughness of metal film Download PDFInfo
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- CN113514011A CN113514011A CN202110661647.9A CN202110661647A CN113514011A CN 113514011 A CN113514011 A CN 113514011A CN 202110661647 A CN202110661647 A CN 202110661647A CN 113514011 A CN113514011 A CN 113514011A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/30—Measuring arrangements characterised by the use of optical techniques for measuring roughness or irregularity of surfaces
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a method for rapidly judging the roughness of a metal film. The rapid discrimination method comprises the following steps: (1) performing direct-current magnetron sputtering under inert gas by using metal as a target and glass as a substrate to obtain a metal film; (2) and (3) testing the mirror image glossiness of the back surface of the metal film obtained in the step (1) and identifying the roughness. By testing the mirror image glossiness of the back surface of the metal film, the roughness of the metal film in the direct current magnetron sputtering deposition process can be judged, and whether a prepared product is qualified or not can be rapidly screened; and the roughness of a product prepared under a specific direct current magnetron sputtering parameter can be judged to further guide the optimization of the direct current magnetron sputtering parameter, so that the prepared metal film has the characteristics of high purity, low oxidation degree and low roughness. The method is favorable for reducing the probability of poor products caused by abnormal roughness of the surface and the interior of the metal film and shortening the quality inspection time of the metal film.
Description
Technical Field
The invention belongs to the technical field of target roughness identification, and particularly relates to a method for rapidly judging the roughness of a metal film.
Background
The metal indium has the excellent characteristics of good ductility, strong plasticity, low melting point, high boiling point, low resistance, corrosion resistance and the like, has better light permeability and electrical conductivity, and is widely applied to the fields of aerospace, radio and electronic industries, medical treatment, national defense, high and new technology, energy sources and the like.
The direct current magnetron sputtering is adopted to grow the metallic indium film, and the surface of the deposited film is not smooth and has no metallic luster. The reason for the roughness of the film may be that the film is oxidized due to impure sputtering gas, or the film has high surface roughness, large crystal grains, and much grain boundary scattering, and forms surface scattering light, which affects the light transmission performance of the film. The prior art determines whether the film is oxidized or not by performing a sheet resistance test on the film, but when the film is thick, the sheet resistance test cannot determine whether the film is oxidized only on the surface or all deposited films.
In summary, under the current test conditions, how to simply and rapidly determine whether the metal film is oxidized or not and determine whether the surface of the metal film is rough or not still needs to be overcome.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention provides a method for rapidly determining the roughness of a metal film.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for rapidly judging the roughness of a metal film comprises the following steps:
(1) performing direct-current magnetron sputtering under inert gas by using metal as a target and glass as a substrate to obtain a metal film;
(2) and (3) testing the mirror image glossiness of the back surface of the metal film obtained in the step (1) and identifying the roughness.
In the method of the direct current magnetron sputtering, the roughness of the metal film is caused by two factors, one is that the roughness is increased because the metal is oxidized into the metal oxide, and the other is that the metal film is deposited layer by layer in the direct current magnetron sputtering, and the longer the film deposition time is, the thicker the film thickness is, the larger the metal particles on the surface layer of the metal film are, and the roughness is increased. The roughness of the metal film is rapidly judged by testing the mirror image glossiness of the back surface of the metal film, and the technical problems that when the film is thick, the roughness can not be determined only by the surface of the film or all deposited film layers by using a sheet resistance test, and the roughness in the film can not be tested by using the roughness test in the prior art are solved. By testing the mirror image glossiness of the back surface of the metal film, the roughness of the first layer of metal deposition film of the metal film in the direct-current magnetron sputtering deposition process can be judged, and whether the prepared product is qualified or not can be rapidly screened; and the roughness of a product prepared under a specific direct current magnetron sputtering parameter can be judged to further guide the optimization of the direct current magnetron sputtering parameter, so that the prepared metal film has the characteristics of high purity, low oxidation degree and low roughness.
In a preferred embodiment of the present invention, the back surface of the metal thin film is a substrate surface of the metal thin film.
The substrate surface of the metal film is glass, the surface of the glass substrate is smooth and has excellent light transmittance, the mirror image glossiness of the back surface of the glass substrate is from the first layer of metal film sputtered and deposited on the substrate, the mirror image glossiness of the back surface of the metal film is measured at an incident angle of 60 degrees, and if the mirror image glossiness of the back surface of the glass substrate is larger than or equal to G0If the roughness of the metal film is lower, the internal roughness of the metal film is qualified; if the mirror gloss of the reverse side of the glass substrate is less than G0And if the roughness of the metal film is larger, the internal roughness of the metal film is unqualified.
The gloss G0In order to obtain an average gloss of a metal thin film prepared by the following metal thin film preparation method, the metal thin film preparation method comprises the steps of:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass, the alkali element content in the glass is 0.05 wt%, and the room-temperature thermal expansion coefficient of the glass is 35.5 multiplied by 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 10cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 2.0W/cm2Sputtering pressure of 0.2Pa, growth temperature of 25 deg.C to obtainThe thickness of the metal thin film was 500 nm.
The roughness of the metal film is judged by testing the mirror image glossiness of the back surface of the metal film obtained in the step (1) and the roughness of the front surface of the metal film.
The front surface of the metal film is a metal deposition surface of the metal film.
As a preferred embodiment of the present invention, the thickness of the metal thin film is 500-2000 nm.
The metal film is thick, so that whether the roughness exists on the surface or inside of the metal film can not be determined only by using a sheet resistance test, and the roughness inside the metal film can not be determined by using a roughness detection instrument in a matching manner.
In a preferred embodiment of the present invention, in the step (1), the glass is alkali-free ultrathin glass, and the glass has a thermal expansion coefficient at room temperature of 35.5X 10 or less-7K, thickness of 0.2-0.6 mm; the content of alkali element in the glass is less than or equal to 0.05 wt%.
In a preferred embodiment of the present invention, in the step (1), the metal is one of metal indium, metal palladium, metal nickel and metal chromium, and the purity of the metal is not less than 99.97%.
Preferably, the metal is metallic indium, and the density of the metallic indium is more than or equal to 7.31g/cm3。
In a preferred embodiment of the present invention, the inert gas is one of nitrogen, argon and helium, and the purity of the inert gas is 99.999% or more.
The purity of the inert gas influences the oxidation degree of the metal film in the direct current magnetron sputtering process, and the inert gas with the purity of over 99.999 percent is selected to ensure that the oxidation degree and the roughness of the metal film are lower and meet the qualified standard of products.
In the step (1), the distance between the target and the substrate is 6-10cm, and the target sputtering power density is 0.5-2.0W/cm2Sputtering ofThe pressure is 0.2-0.8Pa, and the growth temperature of the metal film is 25-32 ℃.
More preferably, in the step (1), in the direct current magnetron sputtering, the distance between the target and the center of the substrate is 7cm, and the target sputtering power density is 0.78W/cm2The sputtering pressure is 0.6Pa, and the growth temperature of the metal film is 25 ℃.
As a preferred embodiment of the present invention, before performing dc magnetron sputtering on a substrate and a target, the substrate is cleaned, and the cleaning specifically comprises the following steps: and ultrasonically cleaning the substrate in acetone, ethanol and water for 5-15min respectively in sequence, and then drying by using high-purity nitrogen.
The high-purity nitrogen has a nitrogen purity of more than 99.999 percent.
Compared with the prior art, the invention has the beneficial effects that:
(1) the roughness of the metal film is rapidly judged by testing the mirror image glossiness of the back surface of the metal film, and the technical problems that when the thickness of the film is thicker, the roughness can not be determined only by the surface of the film or all deposited film layers by using a sheet resistance test, and the roughness in the film can not be tested by using the roughness test in the prior art are solved. By testing the mirror image glossiness of the back surface of the metal film, the roughness of the metal film in the direct current magnetron sputtering deposition process can be judged, and whether a prepared product is qualified or not can be rapidly screened; and the roughness of a product prepared under a specific direct current magnetron sputtering parameter can be judged to further guide the optimization of the direct current magnetron sputtering parameter, so that the prepared metal film has the characteristics of high purity, low oxidation degree and low roughness.
(2) The rapid discrimination method is beneficial to reducing the probability of poor products caused by abnormal roughness of the surface and the interior of the metal film, shortens the quality inspection time of the metal film prepared by the direct current magnetron sputtering method, and saves the cost and the time.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The inventionThe purity of the metallic indium target materials described in the examples and the comparative examples is more than or equal to 99.97 percent, and the density is more than or equal to 7.31g/cm3。
Example 1
The embodiment of the method for rapidly judging the oxidation degree of the metal film comprises the following specific steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 7cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 0.78W/cm2Sputtering pressure is 0.6Pa, growth temperature is 25 ℃, and the thickness of the obtained metal film is 1500 nm;
example 2
The embodiment of the method for rapidly judging the oxidation degree of the metal film comprises the following specific steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 7cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 0.52W/cm2Sputtering pressure is 0.4Pa, growth temperature is 25 ℃, and the thickness of the obtained metal film is 1200 nm;
example 3
The embodiment of the method for rapidly judging the oxidation degree of the metal film comprises the following specific steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is selected fromAlkali ultrathin glass with 0.05 wt% alkali element content and 35.5X 10 of room temperature thermal expansion coefficient-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 6cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 0.5W/cm2Sputtering pressure is 0.8Pa, growth temperature is 32 ℃, and the thickness of the obtained metal film is 2000 nm;
example 4
The embodiment of the method for rapidly judging the oxidation degree of the metal film comprises the following specific steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 10cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 2.0W/cm2Sputtering pressure is 0.2Pa, growth temperature is 25 ℃, and the thickness of the obtained metal film is 500 nm;
comparative example 1
The invention relates to a comparison example of a method for rapidly judging the oxidation degree of a metal film, which comprises the following steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target material and the center of the substrate is 7cm, the purity of argon is 99 percent, and the sputtering power density of the target material isIs 0.78W/cm2Sputtering pressure is 0.6Pa, growth temperature is 25 ℃, and the thickness of the obtained metal film is 1500 nm;
comparative example 2
The invention relates to a comparison example of a method for rapidly judging the oxidation degree of a metal film, which comprises the following steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 7cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 2.5W/cm2The sputtering pressure is 0.6Pa, the growth temperature is 25 ℃, and the thickness of the obtained metal film is 1500 nm.
Comparative example 3
The invention relates to a comparison example of a method for rapidly judging the oxidation degree of a metal film, which comprises the following steps:
(1) mounting a metal indium target on the cathode target;
(2) the substrate is alkali-free ultrathin glass with alkali element content of 0.05 wt% and room temperature thermal expansion coefficient of 35.5 × 10-7K, the thickness is 0.4mm, ultrasonic cleaning is carried out in acetone, absolute ethyl alcohol and deionized water respectively for 10 minutes in sequence, and then high-purity nitrogen is used for blow-drying;
(3) growing a metal indium film on a substrate by adopting direct current magnetron sputtering, wherein the distance between a metal indium target and the center of the substrate is 7cm, the purity of argon is 99.999 percent, and the sputtering power density of the target is 0.78W/cm2The sputtering pressure is 0.6Pa, the growth temperature is 35 ℃, and the thickness of the obtained metal film is 1500 nm.
Examples of effects
Test samples: examples 1 to 4 and comparative examples 1 to 5.
The surface roughness Ra of the metal thin film was measured using a zygo interferometer.
The resistivity rho test method comprises the following steps: the sheet resistance is measured by a four-probe tester, and then the resistivity is calculated according to the formula Rs ═ rho/t, wherein t is the thickness and Rs is the sheet resistance.
Mirror image gloss test of the reverse side of the metal film: with the result G of example 40As a standard, the test specimens had a specular gloss > G0If the result is A; mirror gloss G0Then is A-; mirror gloss < G0If the result is B; a and A-are qualified, B is unqualified.
And (3) manual judgment: the mirror reflection effect is observed by naked eyes, and the substrate on the reverse side of the metal film displays clear portrait, which is strong gloss; if the substrate on the reverse side of the metal film shows blurred human images, the images are weak in gloss.
The results are shown in table 1, and the front surface roughness, the front surface resistivity, the mirror image gloss of the back surface of the metal film and the value of manually judged back surface metallic gloss of each test item in table 1 are average values of 5 test sample tests.
TABLE 1 Performance test results of the Metal films
The metal film prepared in the embodiment 1 of the present invention has the highest mirror image glossiness, which is calculated as a +, on the reverse side, which means that the metal film prepared by the dc magnetron sputtering process described in the embodiment has the smallest internal and surface roughness and the smallest front resistivity. From the results in Table 2, it can be seen that the measured gloss of the instrument is consistent with the manual judgment level, i.e., A +, A and A-are strong gloss, and B is weak gloss. When the surface roughness of the front surface of the metal film is less than 15nm, the front surface resistivity is less than 1 to 10-3Omega cm, and when the mirror image glossiness of the back surface of the metal film is A +, A or A-, the metal film is a qualified product. Comparative example 1 in comparison with the results of example 1, the metal is not pure due to the inert gas in the DC magnetron sputtering processThe metal portions inside and on the surface of the film are oxidized to result in high roughness. The method for rapidly judging the roughness of the metal film solves the problem that the metal film is unqualified due to the fact that only the metal roughness of the front surface is judged and the roughness of the inner part of the metal film is neglected in the prior art, is favorable for reducing the probability of poor products due to the abnormal roughness of the surface and the inner part of the metal film, and shortens the quality inspection time of the metal film.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A method for rapidly judging the roughness of a metal film is characterized by comprising the following steps:
(1) performing direct-current magnetron sputtering under inert gas by using metal as a target and glass as a substrate to obtain a metal film;
(2) and (3) testing the mirror image glossiness of the back surface of the metal film obtained in the step (1) to judge the roughness.
2. The method for rapidly judging the roughness of the metal film as claimed in claim 1, wherein the reverse surface of the metal film is a substrate surface of the metal film.
3. The method as claimed in claim 1, wherein the thickness of the metal film is 500-2000 nm.
4. The method for rapidly judging the roughness of a metal thin film according to claim 1, wherein in the step (1), the glass is alkali-free ultra-thin glass, and the thermal expansion coefficient at room temperature of the glass is less than or equal to 35.5 x 10-7K, thickness of 0.2-0.6 mm; the content of alkali element in the glass is less than or equal to 0.05 wt%.
5. The method for rapidly judging the roughness of a metal film as claimed in claim 1, wherein in the step (1), the metal is one of indium, palladium, nickel and chromium, and the purity of the metal is not less than 99.97%.
6. The method for rapidly judging the roughness of a metal film according to claim 1, wherein the inert gas is one of nitrogen, argon and helium, and the purity of the inert gas is more than 99.999%.
7. The method for rapidly judging the roughness of a metal film as claimed in claim 1, wherein in the step (1), the distance between the center of the target and the center of the substrate in the direct current magnetron sputtering is 6-10cm, and the sputtering power density of the target is 0.5-2.0W/cm2The sputtering pressure is 0.2-0.8Pa, and the growth temperature of the metal film is 25-32 ℃.
8. The method for rapidly judging the roughness of a metal film according to claim 1, wherein in the step (1), in the direct current magnetron sputtering, the distance between the target and the center of the substrate is 7cm, and the sputtering power density of the target is 0.78W/cm2The sputtering pressure is 0.6Pa, and the growth temperature of the metal film is 25 ℃.
9. The method for rapidly judging the roughness of the metal film as claimed in claim 1, wherein the substrate is cleaned before the substrate and the target material are subjected to the direct current magnetron sputtering, and the cleaning comprises the following specific steps: and ultrasonically cleaning the substrate in acetone, ethanol and water for 5-15min respectively in sequence, and then drying by using high-purity nitrogen.
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Cited By (1)
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| CN116497334A (en) * | 2023-06-21 | 2023-07-28 | 潍坊坤祥包装材料有限公司 | Automatic production process for silver plating of thin film |
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| CN116497334B (en) * | 2023-06-21 | 2024-04-19 | 潍坊坤祥包装材料有限公司 | Automatic production process for silver plating of thin film |
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