CN111647857A - Method for recycling residual target of cadmium telluride thin film battery - Google Patents
Method for recycling residual target of cadmium telluride thin film battery Download PDFInfo
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- CN111647857A CN111647857A CN202010466045.3A CN202010466045A CN111647857A CN 111647857 A CN111647857 A CN 111647857A CN 202010466045 A CN202010466045 A CN 202010466045A CN 111647857 A CN111647857 A CN 111647857A
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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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
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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
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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Abstract
The invention discloses a method for recycling residual targets of a cadmium telluride thin film battery. The cadmium telluride thin film battery target material with high density, good mechanical property and high purity is prepared by pretreating, crushing and sieving the residual target of the cadmium telluride thin film battery to obtain residual target powder, doping the residual target powder into the new cadmium telluride thin film battery target material powder and performing a vacuum hot-pressing sintering process. The invention realizes the full recycling of the residual target of the cadmium telluride thin film battery and reduces the generation of waste materials on the premise of not influencing the performance of the target material of the cadmium telluride thin film battery.
Description
Technical Field
The invention relates to the technical field of recycling of sputtering targets, in particular to a method for recycling residual targets of a cadmium telluride thin film battery.
Background
The sputtering method is one of the main techniques for preparing the film material at present, the raw material of the sputtering deposition film is the target material, and the film prepared by the sputtering deposition of the target material has high density and good adhesiveness. Since the 90 s in the 20 th century, new devices and new materials in the microelectronic industry have been developed rapidly, and electronic, magnetic, optical, photoelectric and superconducting films and the like have been widely applied to high and new technologies and industrial fields, so that the market scale of sputtering targets is promoted to be enlarged day by day. Nowadays, the target material has been developed vigorously into a specialized industry.
Cadmium telluride (CdTe), which is an extremely important semiconductor material with a theoretical conversion efficiency of 30%, is a highly desirable photovoltaic material and, therefore, is commonly fabricated as a target material for the preparation of thin film solar cells. The cadmium telluride thin film cell adopts CdTe as an absorption layer, and also needs other materials as a window layer, a TCO layer and the like to form a complete thin film solar cell, generally the materials and the CdTe are collectively called cadmium telluride thin film cell materials, a target material prepared by the materials is called a cadmium telluride thin film cell target material, and the cadmium telluride thin film cell target material comprises a CdTe target material, a cadmium zinc telluride target material, a cadmium oxide target material, a cadmium stannate target material and the like.
The utilization rate of the plane target material of the cadmium telluride thin film battery is 15-30 percent, the utilization rate of the rotary target is 60-80 percent, the residual target after sputtering at present is generally only used for recovering some useful or harmful substances in the residual target, and the processing and recovery utilization rate of the residual target is lower, thereby not only causing the waste of resources, but also increasing the pollution to the environment in the recovery process.
Based on the recycling current situation of the cadmium telluride thin film battery residual target, the invention aims to invent a method for recycling the cadmium telluride thin film battery residual target, improve the processing recycling rate of the residual target and reduce the generation of residual target waste.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling residual targets of cadmium telluride thin film batteries.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for recycling residual targets of a cadmium telluride thin film battery comprises the following steps:
(1) pretreating a residual target of the cadmium telluride thin film battery, crushing and sieving to obtain residual target powder;
(2) adding the residual target powder obtained in the step (1) into the new cadmium telluride thin film battery target material powder, and performing ball milling to obtain mixed powder;
(3) and (3) carrying out vacuum hot-pressing sintering on the mixed powder obtained in the step (2) to obtain the cadmium telluride thin film battery target.
The method has the advantages that the residual target of the cadmium telluride thin film battery is pretreated, crushed and sieved to obtain residual target powder, the residual target powder is doped into the new target powder of the cadmium telluride thin film battery, the new target of the cadmium telluride thin film battery is prepared and reused by the vacuum hot-pressing sintering process, the working procedures of acid dissolution and the like with great environmental pollution are reduced, the process flow is simple, the recovery utilization rate of the residual target is greatly improved, the production efficiency is high, and the method is suitable for large-scale production. The cadmium telluride thin film cell target prepared by the method has high density, good mechanical property and high purity, and can be used for preparing cadmium telluride thin film cells.
Preferably, in the step (2), the adding amount of the residual target powder is 10-25% of the mass of the cadmium telluride thin film battery target new powder.
Compared with the new cadmium telluride thin film battery target material powder, the activity of the residual target powder is slightly low, the addition amount of the residual target powder is too high, and the density and the strength of the cadmium telluride thin film battery target material can be reduced under the same vacuum hot-pressing sintering condition.
Preferably, in the step (2), the ball milling time is 5-8 hours, so that residual target powder and new cadmium telluride thin film battery target powder are fully and uniformly mixed, and the consistency of the target is ensured.
Preferably, in the step (1), the pretreatment comprises grinding, acid washing, ultrasonic water washing and drying of the cadmium telluride thin film battery residual target.
Preferably, the polishing depth of the sputtering surface of the residual target of the cadmium telluride thin film battery is 1-2 mm, and the polishing depth of the non-sputtering surface is 2-3 mm.
Preferably, the specific method for pickling comprises the following steps: the nitric acid with the mass concentration of 5% -10% is used for soaking for 20-30 min, and pollutants on the surface of the residual target can be effectively removed.
Preferably, the ultrasonic water washing time is 5-10 min, and the residual target surface is cleaned.
Preferably, the particle size of the residual target powder is smaller than 100 meshes, which is beneficial to improving the compactness of the target material.
Preferably, the vacuum hot-pressing sintering is specifically as follows: heating under the vacuum condition, keeping the temperature when the temperature is raised to 500-900 ℃, keeping the temperature for 10-50 min, then starting to keep the temperature and pressurize, keeping the temperature and pressurizing pressure at 10-40 MPa, keeping the temperature and pressurizing for 20-40 min, and then keeping the temperature and depressurizing. The invention is beneficial to improving the relative density and the mechanical property of the target material by controlling the sintering temperature, the heat preservation time, the heat preservation pressurization pressure and the heat preservation pressurization time of the vacuum hot-pressing sintering.
Preferably, the cadmium telluride thin film battery target comprises a cadmium telluride target, a cadmium zinc telluride target, a cadmium oxide target or a cadmium stannate target.
Compared with the prior art, the invention has the beneficial effects that:
the cadmium telluride thin film battery target material with high density, good mechanical property and high purity is prepared by pretreating, crushing and sieving the residual target of the cadmium telluride thin film battery to obtain residual target powder, doping the residual target powder into the new cadmium telluride thin film battery target material powder and performing a vacuum hot-pressing sintering process. The invention realizes the full recycling of the residual target of the cadmium telluride thin film battery and reduces the generation of waste materials on the premise of not influencing the performance of the target material of the cadmium telluride thin film battery.
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.
A method for recycling residual targets of a cadmium telluride thin film battery comprises the following steps:
(1) pretreating a residual target of the cadmium telluride thin film battery, crushing and sieving to obtain residual target powder;
(2) adding the residual target powder obtained in the step (1) into the new cadmium telluride thin film battery target material powder, and performing ball milling to obtain mixed powder;
(3) and (3) carrying out vacuum hot-pressing sintering on the mixed powder obtained in the step (2) to obtain the cadmium telluride thin film battery target.
The cadmium telluride thin film battery target is prepared by pretreating, crushing and sieving the residual target of the cadmium telluride thin film battery to obtain residual target powder, doping the residual target powder into the new cadmium telluride thin film battery target powder and performing a vacuum hot-pressing sintering process. The cadmium telluride thin film cell target prepared by the method has high density, good mechanical property and high purity, and can be used for preparing cadmium telluride thin film cells.
In the invention, in the step (2), the adding amount of the residual target powder is 10-25% of the mass of the new cadmium telluride thin film battery target material powder. Compared with new powder, the residual target powder has slightly low activity, and the relative density and strength of the finally obtained cadmium telluride thin film battery target are reduced due to overhigh addition amount of the residual target powder, the addition amount of the residual target powder is preferably 10-25% of the mass of the cadmium telluride thin film battery target new powder, the utilization rate of the residual target of the cadmium telluride thin film battery is improved on the premise of not obviously reducing the mechanical property and the density of the cadmium telluride thin film battery target, and the generation of waste materials is reduced.
In the invention, in the step (2), the ball milling time is 5-8 h, so that residual target powder and new cadmium telluride thin film battery target powder are fully and uniformly mixed, the consistency of the target is ensured, and the compactness of the target is favorably improved.
In the invention, in the step (1), the pretreatment comprises grinding, acid washing, ultrasonic water washing and drying of the residual target of the cadmium telluride thin film battery.
In the invention, when the cadmium telluride thin film battery residual target is polished, the polishing depth of the sputtering surface of the cadmium telluride thin film battery residual target is 1-2 mm, and the polishing depth of the non-sputtering surface is 2-3 mm, and impurities on the surface of the residual target are polished and removed.
In the invention, the specific method for pickling comprises the following steps: and (3) soaking the residual target in nitric acid with the mass concentration of 5-10% for 20-30 min to effectively remove pollutants on the surface of the residual target.
In the invention, the ultrasonic water washing time is 5-10 min, and the residual target surface is cleaned.
The excessive granularity of the residual target powder can influence the compactness and the mechanical property of the final target material, and in the invention, the granularity of the residual target powder is smaller than 100 meshes, which is beneficial to improving the relative density of the target material.
The invention can adopt the vacuum hot-pressing sintering process of the existing conventional cadmium telluride thin film battery target, the specific parameters of the vacuum hot-pressing sintering process can be properly adjusted according to the type of the target, and the vacuum hot-pressing sintering process specifically comprises the following steps: heating under the vacuum condition, keeping the temperature when the temperature is raised to 500-900 ℃, keeping the temperature for 10-50 min, then starting to keep the temperature and pressurize, keeping the temperature and pressurizing pressure at 10-40 MPa, keeping the temperature and pressurizing for 20-40 min, and then keeping the temperature and depressurizing. The invention is beneficial to improving the relative density and the mechanical property of the target material by controlling the sintering temperature, the heat preservation time, the heat preservation pressurization pressure and the heat preservation pressurization time of the vacuum hot-pressing sintering.
In the invention, the cadmium telluride thin film battery target comprises a cadmium telluride target, a cadmium zinc telluride target, a cadmium oxide target or a cadmium stannate target.
Example 1
A method for recycling cadmium telluride targets, comprising the following steps:
(1) polishing the sputtered cadmium telluride residual target by using a polishing machine, wherein the polishing depth along the sputtering track is 1.5mm, and the polishing depth of the non-sputtering surface is 2 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 25min, then putting the residual target in pure water, and ultrasonically cleaning for 10 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 2.5h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the cadmium telluride target new powder, wherein the doping amount of the residual target powder is 25% of the mass of the cadmium telluride target new powder, and performing ball milling for 6 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 600 ℃, preserving heat for 30min, preserving heat and pressurizing the graphite mold at the pressure of 30MPa, preserving heat and pressurizing the graphite mold for 30min, preserving heat and depressurizing the graphite mold, reducing the pressure to 12MPa, naturally cooling the graphite mold to 25 ℃, opening a furnace door, and demolding to obtain the cadmium telluride target.
Example 2
A method for recycling cadmium telluride targets, comprising the following steps:
(1) polishing the sputtered cadmium telluride residual target by using a polishing machine, wherein the polishing depth along the sputtering track is 1.5mm, and the polishing depth of the non-sputtering surface is 2 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 25min, then putting the residual target in pure water, and ultrasonically cleaning for 10 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 2.5h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the cadmium telluride target new powder, wherein the doping amount of the residual target powder is 20% of the mass of the cadmium telluride target new powder, and performing ball milling for 6 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 600 ℃, preserving heat for 30min, preserving heat and pressurizing the graphite mold at the pressure of 30MPa, preserving heat and pressurizing the graphite mold for 30min, preserving heat and depressurizing the graphite mold, reducing the pressure to 12MPa, naturally cooling the graphite mold to 25 ℃, opening a furnace door, and demolding to obtain the cadmium telluride target.
Example 3
A method for recycling cadmium telluride targets, comprising the following steps:
(1) polishing the sputtered cadmium telluride residual target by using a polishing machine, wherein the polishing depth along the sputtering track is 1.5mm, and the polishing depth of the non-sputtering surface is 2 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 25min, then putting the residual target in pure water, and ultrasonically cleaning for 10 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 2.5h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the cadmium telluride target new powder, wherein the doping amount of the residual target powder is 25% of the mass of the cadmium telluride target new powder, and performing ball milling for 8 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 600 ℃, preserving heat for 30min, preserving heat and pressurizing the graphite mold at the pressure of 30MPa, preserving heat and pressurizing the graphite mold for 30min, preserving heat and depressurizing the graphite mold, reducing the pressure to 12MPa, naturally cooling the graphite mold to 25 ℃, opening a furnace door, and demolding to obtain the cadmium telluride target.
Example 4
A method for recycling zinc telluride targets comprises the following steps:
(1) polishing the sputtered zinc telluride residual target by using a polishing machine, wherein the polishing depth along a sputtering track is 1mm, and the polishing depth of a non-sputtering surface is 2.5 mm;
(2) soaking the polished residual target in 10% dilute nitric acid for 30min, then placing the residual target in pure water, and ultrasonically cleaning for 8 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 2h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the new zinc telluride target powder, wherein the doping amount of the residual target powder is 15% of the mass of the new zinc telluride target powder, and performing ball milling for 5 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 500 ℃, preserving heat for 50min, then preserving heat and pressurizing, preserving heat and pressurizing at the pressure of 40MPa, preserving heat and pressurizing for 20min, preserving heat and depressurizing, reducing the pressure to 12MPa, naturally cooling to 35 ℃, opening a furnace door, and demolding to obtain the zinc telluride target.
Example 5
A method for recycling cadmium zinc telluride residual targets comprises the following steps:
(1) polishing the sputtered tellurium-zinc-cadmium residual target by using a polishing machine, wherein the polishing depth along a sputtering track is 2mm, and the polishing depth of a non-sputtering surface is 3 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 20min, then placing the residual target in pure water, and ultrasonically cleaning for 50 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 3h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the new tellurium-zinc-cadmium target powder, wherein the doping amount of the residual target powder is 10% of the mass of the new tellurium-zinc-cadmium target powder, and performing ball milling for 8 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 900 ℃, preserving heat for 10min, preserving heat and pressurizing at the pressure of 10MPa for 40min, preserving heat and depressurizing, reducing the pressure to 12MPa, naturally cooling to 25 ℃, opening a furnace door, and demolding to obtain the tellurium-zinc-cadmium target material.
Comparative example 1
A method for recycling cadmium zinc telluride residual targets comprises the following steps:
(1) polishing the sputtered tellurium-zinc-cadmium residual target by using a polishing machine, wherein the polishing depth along a sputtering track is 2mm, and the polishing depth of a non-sputtering surface is 3 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 20min, then placing the residual target in pure water, and ultrasonically cleaning for 50 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 3h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the new tellurium-zinc-cadmium target powder, wherein the doping amount of the residual target powder is 30% of the mass of the new tellurium-zinc-cadmium target powder, and performing ball milling for 8 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 900 ℃, preserving heat for 10min, preserving heat and pressurizing at the pressure of 10MPa for 40min, preserving heat and depressurizing, reducing the pressure to 12MPa, naturally cooling to 25 ℃, opening a furnace door, and demolding to obtain the tellurium-zinc-cadmium target material.
Comparative example 2
A method for recycling cadmium telluride targets, comprising the following steps:
(1) polishing the sputtered cadmium telluride residual target by using a polishing machine, wherein the polishing depth along the sputtering track is 1.5mm, and the polishing depth of the non-sputtering surface is 2 mm;
(2) soaking the polished residual target in dilute nitric acid with the mass concentration of 8% for 25min, then putting the residual target in pure water, and ultrasonically cleaning for 10 min;
(3) putting the cleaned residual target into a vacuum oven, drying for 2.5h at 50 ℃, then crushing into powder, and sieving by a 100-mesh sieve to obtain residual target powder;
(4) doping residual target powder into the cadmium telluride target new powder, wherein the doping amount of the residual target powder is 25% of the mass of the cadmium telluride target new powder, and performing ball milling for 4 hours to obtain mixed powder, wherein the ball-to-material ratio is 1: 1;
(5) and (2) putting the mixed powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, heating the graphite mold under a vacuum condition, preserving heat when the temperature is increased to 600 ℃, preserving heat for 30min, preserving heat and pressurizing the graphite mold at the pressure of 30MPa, preserving heat and pressurizing the graphite mold for 30min, preserving heat and depressurizing the graphite mold, reducing the pressure to 12MPa, naturally cooling the graphite mold to 25 ℃, opening a furnace door, and demolding to obtain the cadmium telluride target.
The densities of the targets prepared in examples 1 to 5 and comparative examples 1 to 2 were measured according to the drainage method, and the results are shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | |
| Relative density of target material | 97.80％ | 98.3％ | 97％ | 97.6％ | 98.10％ | 95.6％ | 96.1％ |
The results in table 1 show that the target material prepared by the invention has high density, and the relative density is more than 97%. In addition, as can be seen from example 1 and comparative example 2, the ball milling time in step (2) is too short to ensure that the residual target powder and the new powder are uniformly mixed, and the density of the target material is reduced. From the results of example 5 and comparative example 1, it can be seen that under the same vacuum hot-pressing sintering conditions, the compactness of the target material of the cadmium telluride thin film battery is reduced due to the excessive addition of the residual target powder.
The bending strength of the targets prepared in example 5 and comparative example 1 was measured according to GB/T14452-93 "test method for bending mechanical Properties of metals", and the results are shown in Table 2.
TABLE 2
| Example 5 | Comparative example 1 | |
| Bending strength (MPa) | 12.3 | 10.9 |
From the results in table 2, it can be seen that the residual target powder has slightly lower activity compared with the new target powder, and under the same vacuum hot-pressing sintering condition, the bending strength of the cadmium telluride thin film battery target is reduced due to the excessively high addition amount of the residual target powder, and comprehensively, the addition amount of the residual target powder in the invention is preferably 10-25% of the mass of the new target powder of the cadmium telluride thin film battery.
The target materials prepared in example 1 and examples 4 to 5 were tested for impurities by ICP-MS, and the results are shown in table 3.
TABLE 3
The results in table 3 show that the target material prepared by the invention has high purity and low impurity content, and the target material prepared by doping the recovered residual target powder into the new target material powder can be used for preparing a thin-film solar cell.
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 method for recycling residual targets of a cadmium telluride thin film battery is characterized by comprising the following steps:
(1) pretreating a residual target of the cadmium telluride thin film battery, crushing and sieving to obtain residual target powder;
(2) adding the residual target powder obtained in the step (1) into the new cadmium telluride thin film battery target material powder, and performing ball milling to obtain mixed powder;
(3) and (3) carrying out vacuum hot-pressing sintering on the mixed powder obtained in the step (2) to obtain the cadmium telluride thin film battery target.
2. The method for recycling residual target of the cadmium telluride thin film battery as claimed in claim 1, wherein in the step (2), the addition amount of residual target powder is 10% -25% of the mass of the new target powder of the cadmium telluride thin film battery.
3. The method for recycling the residual target of the cadmium telluride thin film battery as claimed in claim 1, wherein in the step (2), the time of ball milling is 5-8 h.
4. The method of claim 1, wherein the pretreating in step (1) comprises grinding, pickling, ultrasonic water washing, and drying the cadmium telluride thin film battery stub target.
5. The recycling method of the cadmium telluride thin film battery residual target as claimed in claim 4, wherein the polishing depth of the sputtering surface of the cadmium telluride thin film battery residual target is 1-2 mm, and the polishing depth of the non-sputtering surface is 2-3 mm.
6. The method for recycling the residual target of the cadmium telluride thin film battery as claimed in claim 4, wherein the specific method of acid washing is as follows: soaking the raw materials in nitric acid with the mass concentration of 5-10% for 20-30 min.
7. The method for recycling the residual target of the cadmium telluride thin film battery as claimed in claim 4, wherein the time of ultrasonic water washing is 5-10 min.
8. The method of claim 1, wherein the stub target powder has a particle size of less than 100 mesh.
9. The method for recycling the residual target of the cadmium telluride thin film battery as claimed in claim 1, wherein the vacuum hot-pressing sintering is specifically as follows: heating under the vacuum condition, keeping the temperature when the temperature is raised to 500-900 ℃, keeping the temperature for 10-50 min, then starting to keep the temperature and pressurize, keeping the temperature and pressurizing pressure at 10-40 MPa, keeping the temperature and pressurizing for 20-40 min, and then keeping the temperature and depressurizing.
10. A method for recycling residual targets of a cadmium telluride thin film battery as claimed in any one of claims 1 to 9, wherein the target material of the cadmium telluride thin film battery comprises a target material of cadmium telluride, a target material of cadmium zinc telluride, a target material of cadmium oxide or a target material of cadmium stannate.
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| CN113526955A (en) * | 2021-07-30 | 2021-10-22 | 广东先导稀材股份有限公司 | Preparation method of cadmium zinc telluride target |
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