CN109148267B - Preparation method of silver-doped copper-zinc-tin-sulfur film - Google Patents
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- CN109148267B CN109148267B CN201811013186.9A CN201811013186A CN109148267B CN 109148267 B CN109148267 B CN 109148267B CN 201811013186 A CN201811013186 A CN 201811013186A CN 109148267 B CN109148267 B CN 109148267B
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Abstract
The invention relates to the technical field of photoelectric materials, in particular to a preparation method of a silver-doped copper-zinc-tin-sulfur film. The invention discloses a preparation method of a silver-doped copper-zinc-tin-sulfur film, which comprises the following steps: step 1: circularly and vacuum sputtering zinc, tin and copper-silver alloy on a substrate in sequence to obtain a precursor; step 2: and vulcanizing the precursor to obtain the silver-doped copper-zinc-tin-sulfur film. The invention solves the technical problems of low compactness, low silver doping efficiency and poor process repeatability of the silver-doped copper-zinc-tin-sulfur film obtained by the existing preparation method.
Description
Technical Field
The invention relates to the technical field of photoelectric materials, in particular to a preparation method of a silver-doped copper-zinc-tin-sulfur film.
Background
Quaternary semiconductor compound copper zinc tin sulfide (Cu) with kesterite structure2ZnSnS4) The film has the advantages of rich component element reserves, no toxicity, low cost and high light absorption coefficient, and becomes a new generation of inorganic film solar cell absorption layer material with development potential.
In Cu2ZnSnS4In the thin film, since the ionic radii of Cu and Zn are close, Cu is likely to appear under high carrier concentrationZnThe inversion defect makes the defect formation energy of the prepared film very low. CuZnThe inversion defects cause surface defects or bulk defects, which are key factors affecting the open-circuit voltage and the conversion efficiency of the solar cell. Suppression of CuZnOne possible approach to dislocation defects is for Cu2ZnSnS4The film is doped with silver (Ag), and the ionic radius of silver ions is larger than that of copper ions, so that the formation energy of site defects can be improved, and Cu can be inhibitedZnAnd forming inverted defects. In addition, Ag doping can also increase Cu2ZnSnS4The grain size of the film, the crystallization quality and the band gap can be adjusted, thereby being beneficial to improving the open-circuit voltage of the solar cellThe conversion efficiency.
Existing preparation of Ag doped Cu2ZnSnS4Methods for thin films include solution methods, spray pyrolysis methods, and sputtering methods. Solution method in Cu2ZnSnS4And silver element is used for partially replacing copper element in the precursor solution to realize Ag doping. Preparing Ag doped Cu by adding Ag-containing compound to raw material by spray thermal decomposition2ZnSnS4The precursor solution is used for preparing a film by subsequent spray pyrolysis. In the two methods, impurities in the surrounding environment easily affect the film in the preparation process, so that the compactness of the film and the Ag doping efficiency are reduced, and the process repeatability is poor. The sputtering method is that firstly an Ag layer is deposited on a Mo-plated soda-lime glass substrate by a thermal evaporation method, then a Cu-Zn-Sn precursor is deposited by a co-sputtering technology, and finally the Ag-doped Cu is obtained by carrying out vulcanization treatment in a sulfur atmosphere2ZnSnS4The thin film has the defects of difficult effective control of doping amount and doping distribution, low doping efficiency and the like. Therefore, the Ag doped Cu obtained by the existing preparation method2ZnSnS4The film compactness and Ag doping efficiency are low, and the process repeatability is poor, so that the technical problem to be solved by the technical personnel in the field is solved.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a silver-doped copper zinc tin sulfide thin film, which solves the technical problems of low compactness and low silver doping efficiency of the silver-doped copper zinc tin sulfide thin film obtained by the existing preparation method.
The invention provides a preparation method of a silver-doped copper-zinc-tin-sulfur film, which comprises the following steps:
step 1: sequentially sputtering zinc, tin and copper-silver alloy on a substrate in vacuum to obtain a precursor;
the sputtering target material of the zinc is a zinc elementary substance target, the sputtering target material of the tin is a tin elementary substance target, and the sputtering target material of the copper-silver alloy is a copper-silver alloy target;
step 2: and vulcanizing the precursor to obtain the silver-doped copper-zinc-tin-sulfur film.
Preferably, after the step 1 and before the step 2, the method further comprises repeating the step 1 for 2-5 times.
More preferably, after the step 1 and before the step 2, the method further comprises repeating the step 1 4 times.
More preferably, before step 1, the method further comprises cleaning the substrate with acetone, absolute ethyl alcohol and deionized water in sequence.
Preferably, the substrate is soda-lime glass or molybdenum-coated soda-lime glass.
More preferably, the substrate is molybdenum-plated soda-lime glass.
It should be noted that, in each vacuum sputtering, the sputtering sequence is Zn, Sn, Cu-Ag, and since the precursor is of a periodic structure, the precursor is favorable for mutual diffusion of metals in the vulcanization process to generate a sufficient vulcanization reaction, and the vulcanization process can sufficiently release thermal stress and improve the crystallinity of the copper-zinc-tin-sulfide thin film.
Preferably, the background vacuum degree of the vacuum sputtering is 5 x 10-4Pa。
More preferably, argon is introduced as a working gas during the vacuum sputtering;
more preferably, the flow rate of the argon gas is 20 mL/min.
Preferably, the atomic ratio of silver to the copper-silver alloy in the copper-silver alloy target is 0.1-0.5.
More preferably, the atomic ratio of silver to copper-silver alloy in the copper-silver alloy target is 0.1 or 0.5.
It should be noted that the atomic ratio of the alloy affects the forbidden bandwidth of the copper-zinc-tin-sulfur thin film
Preferably, the sputtering power of the copper-silver alloy target is 30-50W.
More preferably, the sputtering power of the copper-silver alloy target is 40W.
More preferably, in the repeated vacuum sputtering, the total sputtering time of the copper-silver alloy target is 400-700 s.
Preferably, the sputtering power of the zinc simple substance target is 40-60W.
More preferably, the sputtering power of the zinc elementary substance target is 50W.
More preferably, in the repeated vacuum sputtering, the total sputtering time of the zinc simple substance target is 80-120 s.
Preferably, the sputtering power of the tin simple substance target is 40-60W.
More preferably, the sputtering power of the elementary tin target is 50W.
More preferably, in the repeated vacuum sputtering, the total sputtering time of the tin single substance target is 1300-1700 s.
Preferably, the working pressure of the vacuum sputtering is 0.5 Pa.
Preferably, the vulcanizing temperature is 500-580 ℃.
Nitrogen was introduced as a protective gas during vulcanization.
Compared with a solution method and a spray thermal decomposition method, the preparation method of the silver-doped copper-zinc-tin-sulfur film provided by the invention has the advantage that the sputtering method based on the vacuum condition is favorable for improving the crystallization quality of the film and the process repeatability of the film. Compared with the existing sputtering method of adding an Ag layer between a molybdenum (Mo) electrode and a Cu-Zn-Sn precursor, the method adopts the copper-silver alloy target material to sputter the precursor, so that the distribution of silver in the precursor is more uniform, the activation of silver doping in the vulcanization process is facilitated, and the Ag doping efficiency is improved.
The embodiment of the invention not only successfully prepares the Cu2ZnSnS4Film, and Ag has been doped to Cu2ZnSnS4In thin films, and Ag is doped with Cu2ZnSnS4The surface of the thin film is made of Cu2ZnSnS4Composition of particles, Cu2ZnSnS4The crystallization is good, which is beneficial to improving the carrier mobility and reducing the grain boundary.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is an X-ray diffraction spectrum of a silver-doped CZTS thin film prepared in example 1 of the present invention;
FIG. 2 is a Raman spectrum of a silver-doped CZTS film prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of a silver-doped CZTS film prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction spectrum of a silver-doped CZTS film prepared in example 2 of the present invention;
FIG. 5 shows a Raman spectrum of a silver-doped CZTS film prepared in example 2 of the present invention;
FIG. 6 is a scanning electron microscope image of a silver-doped CZTS film prepared in example 2 of the present invention;
FIG. 7 is an X-ray diffraction spectrum of a silver-doped CZTS film prepared in example 3 of the present invention;
FIG. 8 shows a Raman spectrum of a silver-doped CZTS film prepared in example 3 of the present invention;
FIG. 9 is a scanning electron microscope image of a silver-doped CZTS film prepared in example 3 of the present invention;
FIG. 10 is an X-ray diffraction spectrum of a silver-doped CZTS film prepared in example 4 of the present invention;
FIG. 11 shows a Raman spectrum of a silver-doped CZTS film prepared in example 4 of the present invention;
FIG. 12 is a scanning electron microscope image of a silver-doped CZTS film prepared in example 4 of the present invention.
Detailed Description
The invention provides a preparation method of a silver-doped copper-zinc-tin-sulfur film, which solves the technical problems of low compactness, low silver doping efficiency and poor process repeatability of the silver-doped copper-zinc-tin-sulfur film obtained by the conventional preparation method.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the silver-doped copper-zinc-tin-sulfur film provided by the embodiment of the invention is further explained below.
Example 1
Step 1: the method comprises the steps of selecting molybdenum (Mo) plated soda-lime glass as a substrate, carrying out ultrasonic cleaning on the substrate for 15min by using acetone, absolute ethyl alcohol and deionized water in sequence, and blow-drying by using nitrogen for later use. Putting the cleaned substrate into a magnetron sputtering vacuum chamber, and vacuumizing the vacuum chamber to the background vacuum degree of 5 multiplied by 10-4Pa, introducing argon as working gas, wherein the flow of the argon is 20mL/min, and the working pressure is 0.5 Pa; carrying out pre-sputtering on a zinc elementary substance target, a tin elementary substance target and a copper-silver alloy target for 5 minutes to remove impurities on the surface of the target before formal coating, wherein the atomic ratio of silver to copper-silver alloy in the copper-silver alloy target is 0.1; and then performing formal sputtering coating, wherein the sputtering period number is 4, the sputtering sequence is Zn, Sn and Cu-Ag in each sputtering period, the sputtering power of the zinc simple substance target, the sputtering power of the tin simple substance target and the sputtering time of the copper-silver alloy target are respectively 50W, 50W and 40W, and the sputtering time is respectively 23s, 390s and 135s, so as to prepare the precursor. In the precursor, the total sputtering deposition time of Zn, Sn and Cu-Ag is respectively 92s, 1560s and 540 s.
Step 2: vulcanizing the precursor, putting the precursor and sulfur powder into a quartz boat, and putting the quartz boat into a tube furnace to realize the vulcanization of the precursor; protective gas N is introduced in the vulcanization process2Wherein the vulcanizing temperature is 500 ℃, the vulcanizing time is 20min, and the film is naturally cooled to room temperature after the vulcanizing is finished to obtain the Ag-doped Cu-Zn-Sn-S film2ZnSnS4A film.
FIG. 1 is an X-ray diffraction spectrum of the Ag-doped CuZnSn sulfide thin film prepared in example 1, FIG. 2 is a Raman spectrum of the Ag-doped CuZnSn sulfide thin film prepared in example 1, the characteristic peaks of the diffraction peak and the Raman spectrum in the X-ray diffraction spectrum can be obtainedPhase Structure of the prepared film, Cu was generated from the film prepared in example 12ZnSnS4The structure does not show the X-ray diffraction peak and the Raman spectrum characteristic peak of simple substance Ag and Ag related compounds, which indicates that the Cu is successfully prepared2ZnSnS4Film, and Ag has been doped to Cu2ZnSnS4In the film.
FIG. 3 is a scanning electron microscope photograph of the Ag-doped CuZnSn-S thin film prepared in example 1, and it can be seen from FIG. 3 that the Ag-doped Cu prepared in example 12ZnSnS4The surface of the thin film is made of Cu2ZnSnS4Composition of particles, Cu2ZnSnS4The crystallization was good.
Example 2
Example 2 differs from example 1 in that the atomic ratio of silver to copper-silver alloy in the copper-silver alloy target in example 1 is 0.1, whereas the atomic ratio of silver to copper-silver alloy in the copper-silver alloy target in example 2 is 0.5.
Example 3
Example 3 differs from example 1 in that the vulcanization temperature in example 1 is 500 ℃ and the vulcanization temperature in example 3 is 540 ℃.
Example 4
Example 4 differs from example 1 in that the vulcanization temperature of example 1 is 500 ℃ and the vulcanization temperature of example 4 is 580 ℃.
In summary, fig. 1, 4, 7 and 10 are X-ray diffraction spectra of the silver-doped copper zinc tin sulfide thin films prepared in examples 1, 2, 3 and 4, respectively, and fig. 2, 5, 8 and 11 are raman spectra of the silver-doped copper zinc tin sulfide thin films prepared in the above examples, respectively, and it can be seen from the graphs that the phase structure of the prepared thin films can be obtained from the diffraction peak in the X-ray diffraction spectrum and the characteristic peak in the raman spectrum, and the thin films prepared in the above examples all generate Cu2ZnSnS4The structure does not have X-ray diffraction peak and Raman spectrum characteristic peak of simple substance Ag and Ag related compounds, which shows that the embodiment of the invention successfully prepares Cu2ZnSnS4Film, and Ag has been doped to Cu2ZnSnS4In the film.
FIG. 3FIGS. 6, 9 and 12 are SEM pictures of Ag-doped Cu-Zn-Sn-S thin films prepared in the above examples, and it can be seen that Ag-doped Cu films prepared in the examples of the present invention2ZnSnS4The surface of the thin film is made of Cu2ZnSnS4Composition of particles, Cu2ZnSnS4The crystallinity is good.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the silver-doped copper-zinc-tin-sulfur film is characterized by comprising the following steps of:
step 1: sequentially sputtering zinc, tin and copper-silver alloy on a substrate in vacuum to obtain a precursor;
the sputtering target material of the zinc is a zinc elementary substance target, the sputtering target material of the tin is a tin elementary substance target, and the sputtering target material of the copper-silver alloy is a copper-silver alloy target;
step 2: and vulcanizing the precursor to obtain the silver-doped copper-zinc-tin-sulfur film.
2. The method for preparing the silver-doped copper zinc tin sulfide thin film according to claim 1, wherein after the step 1 and before the step 2, the method further comprises repeating the step 1 for 2 to 5 times.
3. The method of claim 1, wherein the atomic ratio of silver to copper-silver alloy in the copper-silver alloy target is 0.1-0.5.
4. The method for preparing the silver-doped copper-zinc-tin-sulfur film according to claim 1, wherein the sputtering power of the copper-silver alloy target is 30-50W.
5. The method for preparing the silver-doped copper-zinc-tin-sulfur film according to claim 1, wherein the sputtering power of the elemental zinc target is 40-60W.
6. The method for preparing the silver-doped copper zinc tin sulfide thin film according to claim 1, wherein the sputtering power of the elemental tin target is 40-60W.
7. The method for preparing the silver-doped copper zinc tin sulfide thin film according to claim 1, wherein the working pressure of the vacuum sputtering is 0.1-1.0 Pa.
8. The method of claim 1, wherein the background vacuum degree of the vacuum sputtering is 5 x 10-4Pa。
9. The method of claim 1, wherein the substrate is soda-lime glass or molybdenum-plated soda-lime glass.
10. The method for preparing the silver-doped copper zinc tin sulfide thin film according to claim 1, wherein the temperature of the sulfurization is 500-580 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103165748A (en) * | 2013-02-28 | 2013-06-19 | 宁波大学 | Method of preparing copper-zinc tin-sulphur solar cell absorbed layer thin film |
| CN103985783A (en) * | 2014-04-15 | 2014-08-13 | 广东工业大学 | Method for preparing copper zinc tin sulfide thin film on flexible substrate through magnetron sputtering method |
| CN106298995A (en) * | 2016-11-03 | 2017-01-04 | 中国科学院兰州化学物理研究所 | A kind of Ag doping copper zinc tin sulfur selenium light absorbing zone thin-film material and application in solar cells thereof |
| CN107706252A (en) * | 2017-09-01 | 2018-02-16 | 苏州罗格特光电科技有限公司 | A kind of doped copper zinc-tin-sulfur film material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103165748A (en) * | 2013-02-28 | 2013-06-19 | 宁波大学 | Method of preparing copper-zinc tin-sulphur solar cell absorbed layer thin film |
| CN103985783A (en) * | 2014-04-15 | 2014-08-13 | 广东工业大学 | Method for preparing copper zinc tin sulfide thin film on flexible substrate through magnetron sputtering method |
| CN106298995A (en) * | 2016-11-03 | 2017-01-04 | 中国科学院兰州化学物理研究所 | A kind of Ag doping copper zinc tin sulfur selenium light absorbing zone thin-film material and application in solar cells thereof |
| CN107706252A (en) * | 2017-09-01 | 2018-02-16 | 苏州罗格特光电科技有限公司 | A kind of doped copper zinc-tin-sulfur film material |
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