CN113372117A - Preparation method of zinc telluride copper-doped target material - Google Patents
Preparation method of zinc telluride copper-doped target material Download PDFInfo
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Abstract
The invention discloses a preparation method of a zinc telluride copper-doped target material. The preparation method of the zinc telluride copper-doped target material comprises the following steps: putting a powder mixture in which zinc telluride and cuprous telluride are uniformly mixed into a mould in a vacuum hot pressing sintering machine for prepressing; and after the pre-pressing is finished, carrying out vacuum hot-pressing sintering to obtain the zinc telluride copper-doped target material. The invention carries out pre-pressing treatment before hot-pressing sintering, and ensures that the obtained zinc telluride copper-doped target material has higher density; meanwhile, the hot-pressing sintering is carried out under the vacuum condition, so that the oxygen content in the environment can be controlled, the introduction of impurities is reduced, and the high purity of the obtained target material is ensured.
Description
Technical Field
The invention belongs to the field of metal targets, and relates to a preparation method of a zinc telluride copper-doped target.
Background
CdTe (cadmium telluride) solar cells are fast-developing thin film solar cells, and since the CdTe light-absorbing layer is difficult to form a stable low-ohmic contact with the electrode material, a transition layer, i.e., a back contact layer, needs to be inserted between the electrode and the light-absorbing layer. The zinc telluride (ZnTe) copper-doped composite back contact layer is an ideal material of the CdTe solar cell back contact layer, can form good ohmic contact with a CdTe light absorption layer and an electrode, and can improve the performance of the CdTe thin film solar cell.
Research shows that zinc telluride is doped with cuprous telluride (Cu) by magnetron sputtering2Te) ZnTe/ZnTe can be prepared: ZnTe in Cu back contact layer: the Cu film layer (the ZnTe/ZnTe: Cu back contact layer refers to a composite back contact layer formed by the ZnTe film layer and the ZnTe copper-doped film layer, the ZnTe: Cu film layer refers to the ZnTe copper-doped film layer, and other similar descriptions are the same). At present, no patents for synthesizing zinc telluride doped cuprous telluride and preparing a zinc telluride doped cuprous telluride target are published, and the research article mostly adopts a codeposition method to prepare ZnTe/ZnTe: the Cu composite film layer, but compared with the magnetron sputtering coating using a target material, the purity, compactness and component uniformity of the coating formed by using a codeposition method are poor; there are also patents published for preparing zinc telluride single-component targets, which mainly adopt Hot Isostatic Pressing (HIP) method to prepare zinc telluride targets, although the prepared targets have good performance, the cost is relatively high.
Therefore, it is necessary to develop a method for preparing a zinc telluride copper-doped target material with low cost and excellent performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the zinc telluride copper-doped target material, which has the advantages of simple preparation process, low equipment requirement and low cost, and the obtained zinc telluride copper-doped target material has higher purity and density.
In order to achieve the purpose, the invention provides a preparation method of a zinc telluride copper-doped target material, which comprises the following steps:
(1) putting a powder mixture obtained by uniformly mixing zinc telluride and cuprous telluride into a mould in a vacuum hot-pressing sintering furnace for prepressing;
(2) and after the pre-pressing is finished, carrying out vacuum hot-pressing sintering to obtain the zinc telluride copper-doped target material.
The preparation method carries out pre-pressing treatment before hot-pressing sintering, and ensures that the obtained zinc telluride copper-doped target material has higher density; meanwhile, the hot-pressing sintering is carried out under the vacuum condition, so that the oxygen content in the environment can be controlled, the introduction of impurities is reduced, and the high purity of the obtained target material is ensured.
Preferably, the step of vacuum hot-pressing sintering comprises: and (3) vacuumizing, heating to 690-725 ℃, preserving heat for 20-30 min, pressurizing, and cooling after pressurizing is finished to obtain the zinc telluride copper-doped target material. Therefore, the hot-pressing sintering temperature is low, the raw materials are solid in the whole process, the segregation is avoided, and the obtained zinc telluride copper-doped target material is ensured to have good uniformity. Further preferably, the step of vacuum hot-pressing sintering comprises: and (3) vacuumizing, heating to 700 ℃, preserving heat for 20-30 min, pressurizing, and cooling after pressurizing to obtain the zinc telluride copper-doped target material.
Preferably, the step of raising the temperature to 690-725 ℃ for heat preservation comprises: heating to 390-410 ℃ at the speed of 9-10 ℃/min for first heat preservation, then heating to 690-725 ℃ at the speed of 9-10 ℃/min for second heat preservation, wherein the time of the first heat preservation and the second heat preservation is 20-30 min. The heating treatment of hot-pressing sintering is divided into two specific stages, the materials are more fully sintered, and the obtained zinc telluride copper-doped target material has higher density.
Preferably, in the step (2), the pressurizing step includes: pressurizing to 40-45 MPa, and keeping the pressure for 0.5-1.1 h. Under the pressurization procedure, the obtained zinc telluride copper-doped target material has higher density.
Preferably, in the step (2), the temperature reduction is natural temperature reduction; and in the temperature reduction process, after the temperature is lower than 450 ℃, vacuumizing is stopped, and protective gas is filled. And the vacuumizing is stopped and the protective gas is filled in the cooling process, so that the demolding is facilitated.
Preferably, in the step (2), demolding is performed after the temperature reduction is finished, and then CNC machining is performed to form the sheet, so that the zinc telluride copper-doped target material is obtained. Adopt CNC to process into the piece, can reach the purpose of getting rid of impurity.
Preferably, the powder mixture obtained by uniformly mixing the zinc telluride and the cuprous telluride contains 96-98% by mass of zinc telluride. The zinc telluride target is non-conductive, a certain amount of copper is doped in the zinc telluride, the conductivity of the zinc telluride can be improved, when the powder mixture formed by uniformly mixing the zinc telluride and the cuprous telluride contains 96-98% by mass of zinc telluride, the obtained target is the zinc telluride target doped with 1-2% of copper, and the obtained zinc telluride target has better conductivity. More preferably, the powder mixture in which the zinc telluride and the cuprous telluride are uniformly mixed contains 97% by mass of zinc telluride.
Preferably, the mould houses graphite paper to separate the powder mixture from the mould. The graphite paper is arranged in the die, so that the die is easy to demould, and the graphite paper on the surface of the blank is easy to remove.
Preferably, the mold is a graphite mold. The graphite mold has the advantages of high temperature and high pressure resistance, and is suitable for hot-pressing sintering.
Compared with the prior art, the invention has the beneficial effects that: the invention carries out pre-pressing treatment before hot-pressing sintering, and ensures that the obtained zinc telluride copper-doped target material has higher density; meanwhile, the hot-pressing sintering is carried out under the vacuum condition, so that the oxygen content in the environment can be controlled, the introduction of impurities is reduced, and the high purity of the obtained target material is ensured.
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. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
The embodiment provides a preparation method of a zinc telluride copper-doped target material, which comprises the following steps:
1. preparing materials: weighing zinc telluride powder and cuprous telluride powder, wherein the mass ratio of the zinc telluride powder to the cuprous telluride powder is as follows: cuprous telluride 97: 3;
2. mixing materials: loading the zirconium ball and the zinc telluride powder and cuprous telluride powder weighed in the step 1 into a three-dimensional homogenizer, homogenizing for 4 hours at a rotating speed of 56r/min under the protection of nitrogen, wherein the mass ratio of the total mass of the zirconium ball to the total mass of the zinc telluride powder and the cuprous telluride powder is 1:1, and the zirconium ball consists of a large part (with a diameter of 20mm), a medium part (with a diameter of 15mm) and a small part (with a diameter of 10mm), and the mass ratio of the large part to the medium part to the small part is 1:1: 1;
3. charging: loading the mixed material obtained by homogenizing in the step 2 into a graphite mould, wherein the size of the graphite mould is 208mmx116mm, the loading is 1.15kg, and graphite paper is arranged in the graphite mould to separate the material from the mould;
4. pre-pressing: placing the loaded graphite mold in a vacuum hot-pressing sintering furnace, pre-pressing the powder for 25t, sequentially opening a rough pumping valve, a mechanical pump and a roots pump to vacuumize the furnace body after the pre-pressing is finished, and starting heating when the vacuum degree of the furnace body is less than 10 pa;
5. first-stage temperature rise: heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min, and preserving heat at 400 ℃ for 30 min;
6. and (3) heating in the second stage: after the first stage is finished, continuously heating to 690 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 30min at 690 ℃;
7. pressurizing: after the heat preservation is finished at the second stage, pressurizing is started, the pressurizing pressure is 45MPa, the output power of the pressure is 0.5W, and the pressure is maintained for 1h after the pressurizing is finished;
8. cooling: after the pressure is maintained, the natural cooling is started, after the temperature is lower than 450 ℃, the rough pumping valve, the roots pump and the mechanical pump are closed in sequence, and finally N is introduced2Cooling to room temperature;
9. demolding and reprocessing: and (4) cooling to room temperature, discharging, demolding to obtain a blank target material of the zinc telluride copper-doped, and performing CNC (computerized numerical control) processing to obtain the qualified target material.
The purity of the target material of copper doped with zinc telluride obtained in this example was 4.8N, and the relative density was 93% (which is 97% of the theoretical density of copper doped with zinc telluride, and the theoretical density of copper doped with zinc telluride was 6.37g/cm3The same applies below).
Example 2
The embodiment provides a preparation method of a zinc telluride copper-doped target material, which comprises the following steps:
1. preparing materials: weighing zinc telluride powder and cuprous telluride powder, wherein the mass ratio of the zinc telluride powder to the cuprous telluride powder is as follows: cuprous telluride 97: 3;
2. mixing materials: loading the zirconium ball and the zinc telluride powder and cuprous telluride powder weighed in the step 1 into a three-dimensional homogenizer, homogenizing for 4 hours at a rotating speed of 56r/min under the protection of nitrogen, wherein the mass ratio of the total mass of the zirconium ball to the total mass of the zinc telluride powder and the cuprous telluride powder is 1:1, and the zirconium ball consists of a large part (with a diameter of 20mm), a medium part (with a diameter of 15mm) and a small part (with a diameter of 10mm), and the mass ratio of the large part to the medium part to the small part is 1:1: 1;
3. charging: loading the mixed material obtained by homogenizing in the step 2 into a graphite mould, wherein the size of the graphite mould is 208mmx116mm, the loading amount is 1.5kg, and graphite paper is arranged in the graphite mould to separate the material from the mould;
4. pre-pressing: placing the loaded graphite mold in a vacuum hot-pressing sintering furnace, pre-pressing the powder for 25T, opening a rough pumping valve, a mechanical pump and a roots pump in sequence after pre-pressing is completed to vacuumize the furnace body, and starting heating when the vacuum degree of the furnace body is less than 10 pa;
5. first-stage temperature rise: heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min, and preserving heat at 400 ℃ for 30 min;
6. and (3) heating in the second stage: after the first stage is finished, continuously heating to 700 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 30min at 700 ℃;
7. pressurizing: after the heat preservation is finished at the second stage, pressurizing is started, the pressurizing pressure is 45MPa, the output power of the pressure is 0.5W, and the pressure is maintained for 1h after the pressurizing is finished;
8. cooling: after the pressure is maintained, the natural cooling is started, after the temperature is lower than 450 ℃, the rough pumping valve, the roots pump and the mechanical pump are closed in sequence, and finally N is introduced2Cooling to room temperature;
9. demolding and reprocessing: and (4) cooling to room temperature, discharging, demolding to obtain a blank target material of the zinc telluride copper-doped, and performing CNC (computerized numerical control) processing to obtain the qualified target material.
The purity of the zinc telluride copper-doped target material obtained in the embodiment is 4.8N, and the relative density is 95%.
Example 3
The embodiment provides a preparation method of a zinc telluride copper-doped target material, which comprises the following steps:
1. preparing materials: weighing zinc telluride powder and cuprous telluride powder, wherein the mass ratio of the zinc telluride powder to the cuprous telluride powder is as follows: cuprous telluride 97: 3;
2. mixing materials: loading the zirconium ball and the zinc telluride powder and cuprous telluride powder weighed in the step 1 into a three-dimensional homogenizer, homogenizing for 4 hours at a rotating speed of 56r/min under the protection of nitrogen, wherein the mass ratio of the total mass of the zirconium ball to the total mass of the zinc telluride powder and the cuprous telluride powder is 1:1, and the zirconium ball consists of a large part (with a diameter of 20mm), a medium part (with a diameter of 15mm) and a small part (with a diameter of 10mm), and the mass ratio of the large part to the medium part to the small part is 1:1: 1;
3. charging: loading the mixed material obtained by homogenizing in the step 2 into a graphite mould, wherein the size of the graphite mould is 208mmx116mm, the loading amount is 1.5kg, and graphite paper is arranged in the graphite mould to separate the material from the mould;
4. pre-pressing: placing the loaded graphite mold in a vacuum hot-pressing sintering furnace, pre-pressing the powder for 25T, opening a rough pumping valve, a mechanical pump and a roots pump in sequence after pre-pressing is completed to vacuumize the furnace body, and starting heating when the vacuum degree of the furnace body is less than 10 pa;
5. first-stage temperature rise: heating from room temperature to 400 ℃ at a heating rate of 10 ℃/min, and preserving heat at 400 ℃ for 30 min;
6. and (3) heating in the second stage: after the heat preservation is finished in the first stage, continuously heating to 725 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 20-30 min at 725 ℃;
7. pressurizing: after the heat preservation is finished in the second stage, pressurizing is started, the pressurizing pressure is 40-45 MPa, the output power of the pressure is 0.5W, and the pressure is maintained for 1h after the pressurizing is finished;
8. cooling: after the pressure is maintained, the natural cooling is started, after the temperature is lower than 450 ℃, the rough pumping valve, the roots pump and the mechanical pump are closed in sequence, and finally N is introduced2Cooling to room temperature;
9. demolding and reprocessing: and (4) cooling to room temperature, discharging, demolding to obtain a blank target material of the zinc telluride copper-doped, and performing CNC (computerized numerical control) processing to obtain the qualified target material.
The purity of the zinc telluride copper-doped target material obtained in the embodiment is 4.8N, and the relative density is 95.7%.
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 (10)
1. A preparation method of a zinc telluride copper-doped target material is characterized by comprising the following steps:
(1) putting a powder mixture in which zinc telluride and cuprous telluride are uniformly mixed into a mould in a vacuum hot pressing sintering machine for prepressing;
(2) and after the pre-pressing is finished, carrying out vacuum hot-pressing sintering to obtain the zinc telluride copper-doped target material.
2. The method according to claim 1, wherein the pre-pressing pressure is 20 to 30T.
3. The method of claim 1, wherein the step of vacuum hot press sintering comprises: and (3) vacuumizing, heating to 690-725 ℃, preserving heat for 20-30 min, pressurizing, and cooling after pressurizing is finished to obtain the zinc telluride copper-doped target material.
4. The preparation method according to claim 3, wherein the step of raising the temperature to 690-725 ℃ for heat preservation comprises: heating to 390-410 ℃ at the speed of 9-10 ℃/min for first heat preservation, then heating to 690-725 ℃ at the speed of 9-10 ℃/min for second heat preservation, wherein the time of the first heat preservation and the second heat preservation is 20-30 min.
5. The production method according to claim 3, wherein in the step (2), the pressurizing step includes: pressurizing to 40-45 MPa, and keeping the pressure for 0.5-1.1 h.
6. The method according to claim 3, wherein in the step (2), the temperature reduction is natural temperature reduction; and in the temperature reduction process, after the temperature is lower than 450 ℃, vacuumizing is stopped, and protective gas is filled.
7. The preparation method according to claim 3, wherein in the step (2), after the temperature reduction is finished, demolding is carried out, and then CNC machining is adopted to form a sheet, so that the zinc telluride copper-doped target material is obtained.
8. The preparation method of claim 1, wherein the powder mixture in which the zinc telluride and the cuprous telluride are uniformly mixed contains 96-98% by mass of zinc telluride.
9. The method of claim 1, wherein graphite paper is placed inside the mold to separate the powder mixture from the mold.
10. The method of claim 1, wherein the mold is a graphite mold.
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| CN109704766A (en) * | 2019-01-21 | 2019-05-03 | 江西科泰新材料有限公司 | Zinc telluridse mixes the production technology of cuprous telluride target |
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