CN108149206B - ZnSnN 2 film and preparation method thereof - Google Patents
ZnSnN 2 film and preparation method thereof Download PDFInfo
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- CN108149206B CN108149206B CN201711330330.7A CN201711330330A CN108149206B CN 108149206 B CN108149206 B CN 108149206B CN 201711330330 A CN201711330330 A CN 201711330330A CN 108149206 B CN108149206 B CN 108149206B
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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
- C23C14/3464—Sputtering using more than one target
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
The invention discloses a ZnSnN 2 film and a preparation method thereof, wherein the method comprises the steps of carrying out radio frequency sputtering on metal zinc and carrying out direct current sputtering on metal tin in flowing nitrogen and argon atmosphere, and depositing the metal tin on a substrate by a co-sputtering method to obtain the ZnSnN 2 film.
Description
Technical Field
The invention relates to the technical field of semiconductor film materials, in particular to a ZnSnN 2 film and a preparation method thereof.
Background
The ZnSnN 2 film is very suitable for being used as an absorption layer of a next-generation solar cell due to the advantages of rich element reserves, no toxicity, low cost, high absorption coefficient, capability of enabling an energy band of the ZnSnN 2 film to be adjustable in 1.0-2.0eV according to disorder of cations and the like.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a ZnSnN 2 film and a preparation method thereof, and aims to solve the problem that the carrier mobility of the ZnSnN 2 film prepared by the existing method is not high.
The technical scheme of the invention is as follows:
A method for preparing a znsn 2 thin film, comprising the steps of:
In the atmosphere of nitrogen and argon, metal zinc is subjected to radio frequency sputtering, metal tin is subjected to direct current sputtering, and the metal tin is deposited on the substrate by a co-sputtering method, so that the ZnSnN 2 film is obtained.
the preparation method of the ZnSnN 2 film comprises the following steps:
Fixing a zinc target on a radio frequency target, fixing a tin target on a direct current target, vacuumizing a sputtering system, continuously introducing nitrogen and argon, keeping the pressure stable, and simultaneously depositing zinc and tin on a silicon chip or a glass substrate by a co-sputtering method to obtain the ZnSnN 2 film.
The preparation method of the ZnSnN 2 film comprises the steps of using 99.999 percent of high-purity nitrogen as the nitrogen, and using 99.995 percent of high-purity argon as the argon.
The preparation method of the ZnSnN 2 film comprises the steps of enabling the flow rate of nitrogen to be 4 ~ 8sccm and enabling the flow rate of argon to be 15 ~ 25 sccm.
The preparation method of the ZnSnN 2 film comprises the steps of enabling the radio frequency sputtering power to be 30 ~ 50w and enabling the direct current sputtering power to be 15 ~ 20 w.
The preparation method of the ZnSnN 2 film comprises the step of carrying out radio frequency sputtering and direct current sputtering at the air pressure of 3 ~ 7 Pa.
The preparation method of the ZnSnN 2 film is characterized in that the substrate needs to be cleaned in advance.
In the preparation method of the ZnSnN 2 film, the substrate needs to be cleaned by acetone, alcohol and deionized water in advance.
The preparation method of the ZnSnN 2 film is characterized in that the substrate is heated to 300 ~ 400 ℃ before film deposition.
A znsn 2 film, prepared by the process as described above.
The preparation method has the beneficial effects that in the flowing nitrogen and argon atmosphere, the metal zinc is subjected to radio frequency sputtering, the metal tin is subjected to direct current sputtering, and the metal tin is deposited on the substrate simultaneously by a co-sputtering method, so that the ZnSnN 2 film with low carrier concentration and high carrier mobility reaching 24.3cm 2/V-S is prepared, other subsequent treatment is not needed, and the problem of low carrier mobility of the ZnSnN 2 film prepared by the existing method is solved.
drawings
FIG. 1 is an X-ray diffraction test chart of a sample prepared in example 1 of the present invention;
FIG. 2 is an X-ray diffraction test chart of a sample prepared in example 2 of the present invention;
FIG. 3 is an X-ray diffraction test chart of a sample prepared in example 3 of the present invention.
Detailed Description
the present invention provides a method for preparing ZnSnN 2 film, which is further described in detail below for the purpose of making the objects, technical solutions and effects of the present invention clearer and clearer.
The invention relates to a preparation method of a ZnSnN 2 film, which comprises the following steps:
in the flowing nitrogen and argon atmosphere, metal zinc is subjected to radio frequency sputtering, metal tin is subjected to direct current sputtering, and the metal tin is deposited on the substrate through a co-sputtering method, so that the ZnSnN 2 film is obtained.
Different from the traditional mode of preparing the ZnSnN 2 film by performing single sputtering deposition on a zinc-tin alloy on a substrate, the method takes flowing nitrogen as reaction gas and flowing argon as bombardment particles to perform radio frequency sputtering on metal zinc and direct current sputtering on metal tin, and then simultaneously deposits the metal zinc and the metal tin on the substrate to prepare the ZnSnN 2 film with low carrier concentration and high carrier mobility.
The preparation method of the ZnSnN 2 film comprises the steps of fixing a zinc target on a radio frequency target, fixing a tin target on a direct current target, vacuumizing the whole sputtering system to the vacuum degree of 6 x 10 -4 Pa so as to ensure that no oxygen and other impurity gases exist, continuously introducing nitrogen and argon and keeping the pressure stable, namely discharging the nitrogen and the argon at a certain speed while ensuring that the whole co-sputtering system is kept in a certain pressure environment, and simultaneously depositing zinc and tin on a silicon chip or a glass substrate by a co-sputtering method so as to obtain the ZnSnN 2 film.
Preferably, the substrate is cleaned in advance, for example, sequentially cleaned by acetone, alcohol and deionized water in an ultrasonic environment to remove oil stains, impurities and the like on the surface of the substrate, so as to facilitate film deposition, and then the substrate is dried for standby use, wherein the substrate can be monocrystalline silicon, or cheap silicon wafers or glass such as Si (100) or K9 glass and the like, and can be used for manufacturing the ZnSnN 2 film in the invention.
Preferably, in the present invention, the substrate is heated and maintained at 300 ~ 400 c, more preferably 350 c, in advance before the thin film deposition, and impurities are easily generated due to an excessively high temperature, while the thin film is easily amorphized due to an excessively low temperature.
The zinc target and the tin target can be pre-sputtered for a period of time (e.g., 3 ~ 15 minutes) before the film is deposited, so as to remove oxides and impurities on the surface of the target, and avoid depositing the oxides or impurities on the substrate, which finally causes the pollution and even the rejection of the ZnSnN 2 film.
The zinc target is metal zinc with the purity of 99.999 percent, the tin target is metal tin with the purity of 99.999 percent, the power for carrying out radio frequency sputtering on the zinc target is 30 ~ 50w, and the power for carrying out direct current sputtering on the tin target is 15 ~ 20w, and the power proportion not only can realize the radio frequency sputtering on the zinc and the direct current sputtering on the tin, but also can ensure that the zinc and the direct current sputtering on the tin are simultaneously deposited on a substrate to form a ZnSnN 2 film.
In the preparation method of the ZnSnN 2 film, the nitrogen is high-purity nitrogen with the purity of 99.999 percent, the argon is high-purity argon with the purity of 99.995 percent, so that the interference of impurity gases on sputtering reaction is avoided as far as possible, the quality of the ZnSnN 2 film is improved, the air pressure of the whole system is ensured to be stabilized at 3 ~ 7Pa, namely the sputtering air pressure is 3 ~ 7Pa, the N content in the atmosphere is high at the air pressure, the N position occupied by residual O can be reduced, the Zn position occupied by Sn can be reduced, the deposition rate is slow, the compactness of the deposited film is good, the crystallinity of the film is good, the transmission of carrier electrons is facilitated, the mobility of the film is improved, if the air pressure strength is too high, the deposition is not only good, but also the too small film is not tight enough, the transmission of the carrier electrons is not facilitated, meanwhile, the residual O easily occupies the N position, the Sn position is reduced, the Zn position easily occupied by Sn, the carrier concentration is increased violently, and if the air pressure of the reaction system is too high, the deposition rate of Sn and Zn can be caused seriously.
Preferably, the flow rate of the nitrogen is 4 ~ 8sccm, the flow rate of the argon is 15 ~ 25sccm, and the ZnSnN 2 thin film prepared under the flowing nitrogen and argon with the flow rate is low in carrier concentration, high in mobility and particularly good in quality.
The invention also provides a ZnSnN 2 film, wherein the ZnSnN 2 film is prepared by the method.
The present invention will be described in detail below with reference to examples.
Example 1
the method comprises the steps of taking Si (100) and K9 glass as substrates, sequentially utilizing acetone, alcohol and deionized water to carry out ultrasonic cleaning on the substrates, fixing a zinc target with the purity of 99.999% on a radio frequency target, fixing a tin target with the purity of 99.999% on a direct current target, then vacuumizing the background of a sputtering system to 6.0 x 10 -4 Pa, introducing high-purity nitrogen with the flow of 6sccm and high-purity argon with the flow of 20 sccm, carrying out pre-sputtering on the targets for 10min to remove oxides and impurities on the surfaces of the targets, heating the substrates to 350 ℃, carrying out radio frequency sputtering on the zinc target with the sputtering power of 40W under the working pressure of 3Pa, carrying out direct current sputtering on the tin target with the power of 17W for 60 min to obtain the ZnSnN 2 film, closing a sputtering source and an air inlet valve after the sputtering is finished, and sequentially closing a vacuum pump, a power supply and other switches when the temperature of the substrates is reduced to room temperature, and taking out a sample A.
The X-ray diffraction (XRD) test of sample a showed that fig. 1 shows that the thin film prepared according to the present invention has a hexagonal structure under the preparation conditions used in the present invention, as can be seen from fig. 1.
The Hall effect test was performed on sample A, and the results are shown in Table 1. from Table 1, it can be seen that when the operating gas pressure was 3Pa, the carrier concentration of the resulting thin film sample was 2.81X 10 20 cm -3, and the carrier mobility was 0.987cm 2/V-S.
Example 2
The method comprises the steps of taking Si (100) and K9 glass as substrates, sequentially utilizing acetone, alcohol and deionized water to carry out ultrasonic cleaning on the substrates, fixing a zinc target with the purity of 99.999% on a radio frequency target, fixing a tin target with the purity of 99.999% on a direct current target, then vacuumizing the background of a sputtering system to 6.0 x 10 -4 Pa, introducing high-purity nitrogen with the flow of 6sccm and high-purity argon with the flow of 20 sccm, carrying out pre-sputtering on the targets for 10min to remove oxides and impurities on the surfaces of the targets, heating the substrates to 350 ℃, carrying out radio frequency sputtering on the zinc target with the sputtering power of 40W under the working pressure of 5Pa, carrying out direct current sputtering on the tin target with the power of 17W for 60 min to obtain the ZnSnN 2 film, closing a sputtering source and an air inlet valve after the sputtering is finished, and sequentially closing a vacuum pump, a power supply and other switches when the temperature of the substrates is reduced to room temperature, and taking out a sample B.
The X-ray diffraction (XRD) test of sample B showed that the film had a hexagonal structure under the preparation conditions used in the present invention, as can be seen from fig. 2, as shown in fig. 2.
The Hall Effect test was performed on sample B, and the results are shown in Table 1:
TABLE 1
As can be seen from Table 1, when the operating gas pressure was 5Pa, the carrier concentration of the obtained thin film sample was 3.35X 10 19 cm -3, and the carrier mobility thereof was 11.5cm 2/V-S.
Example 3
The method comprises the steps of taking Si (100) and K9 glass as substrates, sequentially utilizing acetone, alcohol and deionized water to carry out ultrasonic cleaning on the substrates, fixing a zinc target with the purity of 99.999% on a radio frequency target, fixing a tin target with the purity of 99.999% on a direct current target, then vacuumizing the background of a sputtering system to 6.0 x 10 -4 Pa, introducing high-purity nitrogen with the flow of 6sccm and high-purity argon with the flow of 20 sccm, carrying out pre-sputtering on the targets for 10min to remove oxides and impurities on the surfaces of the targets, heating the substrates to 350 ℃, carrying out radio frequency sputtering on the zinc target with the sputtering power of 40W under the working pressure of 7Pa, carrying out direct current sputtering on the tin target with the power of 17W for 60 min to obtain the ZnSnN 2 film, closing a sputtering source and an air inlet valve after the sputtering is finished, and sequentially closing a vacuum pump, a power supply and other switches when the temperature of the substrates is reduced to room temperature, and taking out a sample C.
the X-ray diffraction (XRD) test of sample C showed the result of fig. 3, and it can be seen from fig. 3 that the prepared thin film has a hexagonal structure under the preparation conditions used in the present invention.
The Hall effect test was performed on sample C, and the results are shown in Table 1. from Table 1, it can be seen that when the operating gas pressure was 7Pa, the resulting thin film sample had a carrier concentration of 6.72X 10 19 cm -3 and a carrier mobility of 24.3cm 2/V-S.
In combination with the above example 1 ~ 3, it can be seen that, as the sputtering pressure increases, the crystallinity of the obtained film is better, and as the sputtering pressure increases, the carrier concentration decreases by an order of magnitude, and the carrier mobility increases by an order of magnitude, which can reach 24.3cm 2/V-S, and is much higher than that of the znsn 2 film prepared by the method in the prior art.
In conclusion, the invention provides the ZnSnN 2 film and the preparation method thereof, metal zinc is subjected to radio frequency sputtering and metal tin is subjected to direct current sputtering in flowing nitrogen and argon atmosphere, and the metal zinc and the metal tin are simultaneously deposited on the substrate by a co-sputtering method, so that the ZnSnN 2 film with low carrier concentration and high carrier mobility reaching 24.3cm 2/V-S is prepared, other subsequent treatment is not needed, and the problem of low carrier mobility of the ZnSnN 2 film prepared by the conventional method is solved.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of ZnSnN 2 film is characterized by comprising the following steps:
In the flowing nitrogen and argon atmosphere, performing radio frequency sputtering on metal zinc and performing direct current sputtering on metal tin, and depositing the metal tin on a substrate by a co-sputtering method to obtain a ZnSnN 2 film;
The air pressure of the radio frequency sputtering and the air pressure of the direct current sputtering are both 3-7 Pa.
2. The method of making a znsn 2 film as recited in claim 1, comprising the steps of:
Fixing a zinc target on a radio frequency target, fixing a tin target on a direct current target, vacuumizing a sputtering system, continuously introducing nitrogen and argon, keeping the pressure stable, and simultaneously depositing zinc and tin on a silicon chip or a glass substrate by a co-sputtering method to obtain the ZnSnN 2 film.
23. The method of claim 2, wherein the nitrogen gas is a high purity nitrogen gas of 99.999% and the argon gas is a high purity argon gas of 99.995%.
4. The method for preparing ZnSnN 2 thin film as claimed in claim 3, wherein a flow rate of said nitrogen gas is 4 to 8sccm and a flow rate of said argon gas is 15 to 25 sccm.
5. The method for preparing ZnSnN 2 film according to claim 1, wherein the RF sputtering power is 30-50 w and the DC sputtering power is 15-20 w.
6. The method of making a znsn 2 film as set forth in claim 1, wherein the substrate is previously cleaned.
27. The method as claimed in claim 1, wherein the substrate is previously cleaned with acetone, alcohol and deionized water.
8. The method for preparing ZnSnN 2 film according to claim 1, wherein said substrate is heated to 300 to 400 ℃ before film deposition.
9. A znsn 2 film prepared by the method of any one of claims 1 to 8.
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| CN201711330330.7A CN108149206B (en) | 2017-12-13 | 2017-12-13 | ZnSnN 2 film and preparation method thereof |
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| CN108149206B true CN108149206B (en) | 2019-12-10 |
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| EP2853518B1 (en) * | 2013-09-26 | 2019-01-02 | Türkiye Sise Ve Cam Fabrikalari A.S. | A low-e coated glass |
| CN104037267B (en) * | 2014-06-30 | 2016-07-06 | 电子科技大学 | A kind of method that copper-zinc-tin-selefilm film solar battery obsorbing layer is modified |
| CN104195514B (en) * | 2014-08-04 | 2017-01-11 | 中国科学院宁波材料技术与工程研究所 | Preparation method for zinc tin nitride polycrystalline film |
| CN105118884B (en) * | 2015-07-20 | 2017-07-25 | 中国科学院宁波材料技术与工程研究所 | One kind nitridation zinc-tin pn-junction and preparation method thereof |
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