CN110724921A - Intermittent magnetron sputtering method for improving disorder of amorphous material - Google Patents
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- CN110724921A CN110724921A CN201910969641.0A CN201910969641A CN110724921A CN 110724921 A CN110724921 A CN 110724921A CN 201910969641 A CN201910969641 A CN 201910969641A CN 110724921 A CN110724921 A CN 110724921A
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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
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron 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
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Abstract
The invention discloses an intermittent magnetron sputtering method for improving the disorder of an amorphous material, which comprises the following steps: cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity; polishing and cleaning a target material to be sputtered, and then placing the target material on a direct-current sputtering target position of the sputtering cavity; vacuumizing the sputtering cavity to a set vacuum degree; setting condition parameters in the sputtering process; and carrying out intermittent magnetron sputtering on the target material to be sputtered, stopping sputtering for the first time in the sputtering process under the condition of keeping the sputtering environment unchanged, then sputtering for the first time, stopping sputtering for the second time, then sputtering for the first time, stopping sputtering for the third time, and sequentially carrying out sputtering, wherein the time of each pause is sequentially prolonged until the required thickness of the film is sputtered. The intermittent magnetron sputtering method of the invention is more beneficial to the formation of the amorphous performance of the film while keeping the improvement of the disorder degree of the film.
Description
Technical Field
The invention belongs to the technical field of magnetron sputtering, and particularly relates to an intermittent magnetron sputtering method for improving the disorder of an amorphous material.
Background
Compared with a crystalline material, the amorphous material has a unique atomic arrangement mode and has the characteristics of short-range order and long-term disordered atomic arrangement. Thus, amorphous materials exhibit different and unique chemical and structural properties from crystalline materials, such as isotropy, high concentration of unsaturated coordination active sites, widely adjustable compositional components, and the like. Because of the unique chemical and structural characteristics, the amorphous material shows far better catalytic performance than the corresponding crystalline material in the fields of chemical production, energy conversion, environmental remediation and the like, thereby being widely concerned.
For amorphous materials, the disorder degree of the materials has a remarkable effect on the improvement of the film performance, and the traditional method for improving the disorder degree of the materials by a doping method is complex in process, easy to change the characteristics of the materials and easy to increase the preparation cost.
Chinese patent CN107043914A discloses an intermittent DC magnetron sputtering preparation method of an amorphous cobalt-based magnetic film, but the method aims to prepare the amorphous cobalt-based magnetic film and mainly adopts a gradient temperature rise mode to solve the problem that the temperature rise of DC magnetron sputtering is faster at low temperature.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides an intermittent magnetron sputtering method for improving the disorder of an amorphous material, so that an interface effect and a similar heterostructure are generated between layers sputtered by a film, the pause time is sequentially prolonged, and the amorphous performance of the film is more favorably formed while the disorder of the film is kept.
In order to achieve the above object, the present invention provides an intermittent magnetron sputtering method for improving disorder of an amorphous material, comprising the steps of:
cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
polishing and cleaning a target material to be sputtered, and then placing the target material on a direct-current sputtering target position of the sputtering cavity;
under the conditions of set vacuum degree, target base distance and target sputtering power, carrying out intermittent magnetron sputtering on the target to be sputtered in the sputtering cavity;
keeping the temperature of the substrate below 80 ℃ in the sputtering process, sputtering for a first time in the sputtering process, stopping sputtering for the first time under the condition of keeping the sputtering environment unchanged, sputtering for the first time again, stopping sputtering for a second time, sputtering for the first time again, and stopping sputtering for a third time; after the first time of sputtering, the process of stopping sputtering is a period, and the time for stopping sputtering in each period is sequentially prolonged until the required film thickness is sputtered;
the first time is 4-6 min, the second time is 2 times of the first time, the third time is 3 times of the first time, the first time is sequentially prolonged according to the rule, the nth time is n times of the first time, n is a natural number, and the value is related to the required film thickness.
Further, the degree of vacuum was 1X 10-4Pa～4×10-4Pa。
Furthermore, the target base distance is 60 mm-120 mm.
Further, the sputtering power of the target is 20W-80W.
Further, the sputtering cavity is filled with inert gas for protection.
Further, the inert gas is N2Ar or He.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the intermittent magnetron sputtering method for improving the disorder of the amorphous material adopts the intermittent magnetron sputtering method, and the pause in the sputtering process causes an interface effect and a similar heterostructure to be generated between layers sputtered by the film, so that the disorder degree of the film is improved. And the dwell time is prolonged in sequence, so that the amorphous performance of the film is more favorably formed while the disorder degree of the film is improved.
(2) The intermittent magnetron sputtering method for improving the disorder of the amorphous material prevents the surface crystallization of the film in the sputtering process because the crystallization temperature of most phase-change materials is quite low.
(3) The intermittent magnetron sputtering method for improving the disorder of the amorphous material, disclosed by the invention, not only can effectively improve the disorder of the material, but also is simple and convenient in operation process, and compared with the method for improving the disorder by doping in the traditional process, the intermittent magnetron sputtering method can greatly save raw materials and cost.
Drawings
FIG. 1 is an AC magnetic susceptibility diagram of an intermittent magnetron sputtering film according to an embodiment of the present invention;
FIG. 2 is a graph of the alternating magnetic susceptibility of a mass according to an embodiment of the present invention;
FIG. 3 is a DC susceptibility diagram of an intermittent magnetron sputtering film according to an embodiment of the present invention;
FIG. 4 is a graph of DC magnetic susceptibility of a bulk material according to an embodiment of the present invention;
FIG. 5 is a diagram of an MFM film according to an embodiment of the present invention;
fig. 6 is a diagram of a bulk MFM according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The intermittent magnetron sputtering method for improving the disorder of the amorphous material comprises the following steps:
cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
polishing and cleaning a target material to be sputtered, and then placing the target material on a direct current sputtering target position of a sputtering cavity;
turning on the power supply, vacuumizing the sputtering cavity to a vacuum degree of 1 × 10-4Pa～4×10-4Pa；
Setting condition parameters in the sputtering process, wherein the target base distance is 60-120 mm, and the sputtering power of the target is 20-80W; inert gas N is filled into the sputtering cavity2；
Keeping the temperature of the substrate below 80 ℃ in the sputtering process, sputtering for the first time in the sputtering process, stopping sputtering for the first time under the condition of keeping the sputtering environment unchanged, sputtering for the first time again, stopping sputtering for the second time, then sputtering for the first time again, and stopping sputtering for the third time; after the first time of sputtering, the process of stopping sputtering is a period, and the time for stopping sputtering in each period is sequentially prolonged until the required film thickness is sputtered;
the first time is 4-6 min, the second time is 2 times of the first time, the third time is 3 times of the first time, the first time is sequentially prolonged according to the rule, the nth time is n times of the first time, n is a natural number, and the value of n is related to the required thickness of the film.
Specifically, because the target material is placed in the air and has an oxidation reaction, the surface of the target material to be sputtered needs to be polished before sputtering to remove surface oxides, and sputtering the target material which is not polished can affect the components of the target material and the performance of a sputtered film; the vacuum degree of the sputtering cavity is 1 multiplied by 10-4Pa～4×10-4Pa, if the vacuum degree is exceeded, the element composition sputtered to the substrate by the target material cannot be controlled; the target base distance is 60 mm-120 mm, the element components sputtered by the target material beyond the range can not be controlled, and the roughness of the surface of the film is very large; the sputtering power of the target is 20W-80W, the target cannot glow when the sputtering power is lower than 20W, and the target has the risk of cracking when the sputtering power is higher than 80W.
Further, the sputtering process is performed for the first time, the sputtering is stopped for the first time under the condition that the sputtering environment is kept unchanged, the sputtering is stopped for the first time again, the sputtering is stopped for the second time, then the sputtering is performed for the first time again, the sputtering is stopped for the third time, the sputtering is performed in sequence, the time of each pause is prolonged in sequence, and the temperature of the substrate is controlled better. For some phase-change materials, the crystallization temperature is 80-100 ℃ due to the fact that the crystallization temperature is too low, heat is generated on the surface of a sputtered film due to impact of target atoms in the sputtering process, the temperature of the surface of the sputtered film is increased, and the intermittent magnetron sputtering method with the sequentially prolonged pause time is more beneficial to heat dissipation and cooling of the surface of the film. Under the condition of not crystallizing the film, the amorphous film with high disorder degree is sputtered, which is more beneficial to the preparation of amorphous materials. The film prepared by intermittent magnetron sputtering is non-continuous sputtering, so that a structure similar to an interface effect and a heterojunction can be generated in the middle of the film, and the disorder degree of the material is increased.
The nth time is n times of the first time, n is a natural number, and the value of n is directly related to the thickness of the film to be sputtered.
The intermittent magnetron sputtering method is to prepare the material by intermittent sputtering through direct current or alternating current magnetron sputtering. The sputtering target can be a metal, nonmetal or rare earth material. Wherein the interruption time is 1min or more, and inert gas such as N can be introduced into the reaction chamber for protection in order to prevent oxidation of the material2Ar, He, etc., and the amount of the inert gas to be charged is related to the size of the sputtering chamber and the kind of the sputtering target.
In conclusion, compared with the common magnetron sputtering method, the intermittent magnetron sputtering method is more beneficial to the preparation of the amorphous film. The amorphous film material is disordered due to the short-range ordered long layer, so that the amorphous film material is disordered, and the increase of the disorder degree of the amorphous material is beneficial to improving the performances of the amorphous material in various aspects and increasing the application range of the material. The intermittent magnetron sputtering method ensures that an interface effect and a similar heterostructure are generated between layers sputtered by the film due to pause in the sputtering process, so that the disorder degree of the film is improved. The dwell time is sequentially prolonged, and the amorphous performance of the film is more favorably formed while the disorder degree of the film is kept to be improved. Because the crystallization temperature of most phase-change materials is quite low, the intermittent magnetron sputtering method which sequentially prolongs the pause time prevents the surface crystallization of the film in the sputtering process.
Example 1
S1: cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
s2: polishing and cleaning a target material to be sputtered, and then placing the target material on a direct current sputtering target position of a sputtering cavity;
s3: turning on the power supply, vacuumizing the sputtering cavity to a vacuum degree of 1 × 10-4Pa；
S4: setting condition parameters in the sputtering process, wherein the target base distance is 60mm, and the sputtering power of the target is 20W; inert gas N is filled into the sputtering cavity2；
S5: the method comprises the steps of performing intermittent magnetron sputtering on a target material to be sputtered in a sputtering cavity, keeping the temperature of a substrate below 80 ℃ in the sputtering process, stopping sputtering for a first time in the sputtering process under the condition that the sputtering environment is kept unchanged, stopping sputtering for the first time, then sputtering for a second time, then sputtering for the first time, stopping sputtering for a third time, sequentially performing sputtering, and sequentially prolonging the time of each pause, wherein the first time is 4min, the second time is 8min, and the third time is 12min times of the first time, and sequentially prolonging the first time until the thickness of a sputtered film is 300 nm.
Example 2
S1: cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
s2: polishing and cleaning a target material to be sputtered, and then placing the target material on a direct current sputtering target position of a sputtering cavity;
s3: turning on the power supply, vacuumizing the sputtering cavity to 2 × 10-4Pa；
S4: setting condition parameters in the sputtering process, wherein the target base distance is 80mm, and the sputtering power of the target is 40W; inert gas N is filled into the sputtering cavity2；
S5: the method comprises the steps of performing intermittent magnetron sputtering on a target material to be sputtered in a sputtering cavity, keeping the temperature of a substrate below 80 ℃ in the sputtering process, stopping sputtering for a first time in the sputtering process under the condition that the sputtering environment is kept unchanged, stopping sputtering for the first time, then sputtering for a second time, then sputtering for the first time, stopping sputtering for a third time, sequentially performing sputtering, sequentially prolonging the pause time of each time, wherein the first time is 5min, the second time is 10min, and the third time is 15min, and sequentially prolonging the pause time until the thickness of a sputtered film is 200 nm.
Example 3
S1: cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
s2: polishing and cleaning a target material to be sputtered, and then placing the target material on a direct current sputtering target position of a sputtering cavity;
s3: turning on the power supply, vacuumizing the sputtering cavity to a vacuum degree of 3 × 10-4Pa；
S4: setting condition parameters in the sputtering process, wherein the target base distance is 100mm, and the sputtering power of the target is 60W; filling inert gas Ar into the sputtering cavity;
s5: the method comprises the steps of performing intermittent magnetron sputtering on a target material to be sputtered in a sputtering cavity, keeping the temperature of a substrate below 80 ℃ in the sputtering process, stopping sputtering for a first time in the sputtering process under the condition that the sputtering environment is kept unchanged, stopping sputtering for the first time, then sputtering for a second time, then sputtering for the first time, stopping sputtering for a third time, sequentially performing sputtering, sequentially prolonging the pause time of each time, wherein the first time is 5.5min, the second time is 11min, and the third time is 16.5min, and sequentially prolonging the pause time until the thickness of a sputtered film is 200 nm.
Example 4
S1: cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
s2: polishing and cleaning a target material to be sputtered, and then placing the target material on a direct current sputtering target position of a sputtering cavity;
s3: turning on the power supply, vacuumizing the sputtering cavity to a vacuum degree of 4 × 10-4Pa；
S4: setting condition parameters in the sputtering process, wherein the target base distance is 120mm, and the sputtering power of the target is 80W; filling inert gas He into the sputtering cavity;
s5: the method comprises the steps of performing intermittent magnetron sputtering on a target material to be sputtered in a sputtering cavity, keeping the temperature of a substrate below 80 ℃ in the sputtering process, stopping sputtering for a first time in the sputtering process under the condition that the sputtering environment is kept unchanged, stopping sputtering for the first time, then sputtering for a second time, then sputtering for the first time, stopping sputtering for a third time, sequentially performing sputtering, sequentially prolonging the time of each pause, wherein the first time is 6min, the second time is 12min, the third time is 18min, and sequentially prolonging the time until the thickness of a sputtered film is 100 nm.
FIG. 1 is an AC magnetic susceptibility diagram of an intermittent magnetron sputtering film according to an embodiment of the present invention; FIG. 2 is a graph of the alternating magnetic susceptibility of a mass according to an embodiment of the present invention; FIG. 3 is a DC susceptibility diagram of an intermittent magnetron sputtering film according to an embodiment of the present invention; FIG. 4 is a graph of DC magnetic susceptibility of a bulk material according to an embodiment of the present invention; with reference to fig. 1 to 4, it can be seen that the freezing temperature of the thin film material prepared by the intermittent magnetron sputtering method is greatly increased.
FIG. 5 is a diagram of an MFM film according to an embodiment of the present invention; fig. 6 is a diagram of a bulk MFM according to an embodiment of the present invention. It can be seen that the magnetic moment is more disordered by the film of intermittent magnetron sputtering.
The intermittent magnetron sputtering method for improving the disorder of the amorphous material, disclosed by the invention, not only can effectively improve the disorder of the material, enhance the improvement of the disorder of the material and contribute to the improvement of the performance of the material and devices, but also is simple and convenient in operation process, and compared with the method for improving the disorder by doping in the traditional process, the intermittent magnetron sputtering method can greatly save raw materials and cost.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. An intermittent magnetron sputtering method for improving the disorder of an amorphous material is characterized by comprising the following steps:
cleaning a substrate to be sputtered, and placing the substrate on a tray of a sputtering cavity;
polishing and cleaning a target material to be sputtered, and then placing the target material on a direct-current sputtering target position of the sputtering cavity;
under the conditions of set vacuum degree, target base distance and target sputtering power, carrying out intermittent magnetron sputtering on the target to be sputtered in the sputtering cavity;
keeping the temperature of the substrate below 80 ℃ in the sputtering process, sputtering for a first time in the sputtering process, stopping sputtering for the first time under the condition of keeping the sputtering environment unchanged, sputtering for the first time again, stopping sputtering for a second time, sputtering for the first time again, and stopping sputtering for a third time; after the first time of sputtering, the process of stopping sputtering is a period, and the time for stopping sputtering in each period is sequentially prolonged until the required film thickness is sputtered;
the first time is 4-6 min, the second time is 2 times of the first time, the third time is 3 times of the first time, the first time is sequentially prolonged according to the rule, the nth time is n times of the first time, n is a natural number, and the value is related to the required film thickness.
2. The intermittent magnetron sputtering method for improving disorder of amorphous material as claimed in claim 1, wherein the degree of vacuum is 1 x 10-4Pa～4×10-4Pa。
3. An intermittent magnetron sputtering method for improving the disorder of amorphous material as claimed in claim 1 or 2 wherein the target base distance is 60mm to 120 mm.
4. The intermittent magnetron sputtering method according to claim 3, wherein the sputtering power of the target material is 20W-80W.
5. An intermittent magnetron sputtering method for improving the disorder of amorphous material as claimed in claim 1 or 3 wherein the sputtering chamber is filled with inert gas for protection.
6. The intermittent magnetron sputtering method for improving the disorder of the amorphous material as claimed in claim 5, wherein the inert gas is N2Ar or He.
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Cited By (1)
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