Zinc telluride target material, method for preparing the same and use thereof
By combining zinc telluride, modified arsenic oxide, and antimony oxide, along with binders and thermal decomposition porosity technology, the problems of insufficient purity and density of zinc telluride target material were solved, and the preparation of highly conductive zinc telluride thin films was achieved, which are suitable for the battery field.
Patent Information
- Application Number
- CN202410249602.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-05
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2044-03-05
AI Technical Summary
Existing zinc telluride targets suffer from insufficient purity and density during preparation, which affects their application in highly conductive zinc telluride thin films.
By combining zinc telluride, modified arsenic oxide, and modified antimony oxide, the conductivity is improved by utilizing the high electron-hole and carrier concentration. Porosity is generated through the bonding effect of the binder and thermal decomposition. Combined with the combination of arsenic oxide, amino carbon nanotubes, and polyethylene glycol solution, a network pore structure is formed, which improves the conductivity and molding effect of the zinc telluride target material.
The prepared zinc telluride target material has high purity and high density, avoiding powder shedding and cracking. The zinc telluride thin film has low resistivity and high conductivity, making it suitable for the battery field.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of battery application target material, more particularly, it relates to a zinc telluride target material and a preparation method and application thereof. BACKGROUND
[0002] Zinc telluride thin film is an important semiconductor photoelectric material, which has important uses in photoluminescence and electroluminescence devices, solar cells, infrared detectors, thermal imaging technology and other fields.
[0003] At present, zinc telluride thin film is mainly prepared by electron beam vapor deposition and magnetron sputtering, and these preparation methods all use zinc telluride target material as raw material, so high-purity and high-density zinc telluride target material is extremely important for the application of the material.
[0004] Therefore, it is urgent to prepare a new zinc telluride target material which has the advantages of high purity and high density, and can be used to prepare high-conductivity zinc telluride thin film, and the zinc telluride thin film is applied in the field of batteries. SUMMARY
[0005] In order to prepare a new zinc telluride target material which has the advantages of high purity and high density, and can be used to prepare high-conductivity zinc telluride thin film, and the zinc telluride thin film is applied in the field of batteries, the present application provides a zinc telluride target material and a preparation method and application thereof.
[0006] In the first aspect, the present application provides a zinc telluride target material, which adopts the following technical scheme:
[0007] The zinc telluride target material comprises the following raw materials by weight: 95-99 parts of zinc telluride, 0.5-3 parts of dopant, and 0.5-2 parts of binder; the dopant is composed of modified arsenic oxide and modified antimony oxide in a mass ratio of 1:1-2; the modified arsenic oxide is prepared from arsenic oxide, amino carbon nanotube and polyethylene glycol solution in a mass ratio of 1:0.02-0.04:0.05-0.1; and the modified antimony oxide is prepared from antimony oxide, carboxyl modified porous boron carbide and polyethylene glycol solution in a mass ratio of 1:0.01-0.03:0.05-0.1.
[0008] By adopting the above technical scheme, zinc telluride, arsenic oxide and antimony oxide are matched, the multi-electron hole in arsenic and antimony is utilized, and the high carrier concentration is matched to improve the conductivity effect of the zinc telluride target material, and the purity is high. The binding effect of the binder can not only improve the binding density of zinc telluride, arsenic oxide and antimony oxide, ensure the forming effect of the zinc telluride target material, and prevent the problems of powder falling and cracking, but also improve the internal micropore porosity of the zinc telluride target material with the thermal decomposition of the binding liquid, promote the uniform film formation of the zinc telluride target material, and have more pore channels to improve the conductivity effect of the zinc telluride thin film, which can be applied in the field of batteries.
[0009] The arsenic oxide, the amino carbon nanotube and the polyethylene glycol solution are combined, the five electron holes of arsenic are combined with the pore structure in the amino carbon nanotube, the electron hole effect and the carrier concentration of the zinc telluride target material are further improved, and thus the conductivity of the zinc telluride target material is improved; the polyethylene glycol solution has a bonding effect, the hydroxyl in the polyethylene glycol solution is combined with the amino on the surface of the amino carbon nanotube, the amino carbon nanotube is bonded on the surface of the arsenic oxide, the electron hole effect of the arsenic oxide is combined with the porous hole effect of the amino carbon nanotube, the holes are connected, and thus the carrier concentration is further improved, and the conductivity of the zinc telluride target material is improved; with the preparation of the zinc telluride target material, the polyethylene glycol can be decomposed to produce gas by heating, the zinc telluride target material is not easy to be compacted, and thus the preparation of the zinc telluride film is not affected, and the purity of the zinc telluride target material and the conductivity of the zinc telluride film are not affected by the retention of impurities.
[0010] The antimony oxide, the carboxyl modified porous boron carbide and the polyethylene glycol solution are combined, the layered lapping structure of the antimony and the carboxyl modified porous boron carbide can further improve the porosity and the electron hole pair, the conductivity of the antimony and the boron carbide is combined, the conductivity is further improved, the porous structure of the boron carbide, the lapping network pores of the antimony oxide, the carboxyl modified porous boron carbide and the polyethylene glycol solution are combined, and thus the carrier concentration is further improved, and the conductivity of the zinc telluride target material is further improved.
[0011] The modified arsenic oxide and the modified antimony oxide are combined, the amino carbon nanotube on the surface of the arsenic oxide has a long columnar structure and is hollow, the layered lapping structure of the carboxyl modified porous boron carbide on the surface of the antimony oxide is combined, the lapping is facilitated, the amino on the surface of the amino carbon nanotube can be bonded with the carboxyl on the surface of the carboxyl modified boron carbide by mutual attraction, the binder on the surface of the zinc telluride is combined, the zinc telluride, the arsenic oxide and the antimony oxide are lapped and bonded, a bonding network is formed, the density of the zinc telluride target material is high, the uniformity is improved, the problems of powder falling and cracking are not easy to occur, the uniformity of film formation is not affected, the conductivity of the zinc telluride film is improved.
[0012] Preferably, the amino carbon nanotube is prepared by modifying a carbon nanotube with dopamine.
[0013] By adopting the above technical solution, the carbon nanotube and dopamine are combined, the surface of the carbon nanotube is modified with amino, the conductivity is improved, the carboxyl on the surface of the modified antimony oxide and the hydroxyl in the binder are combined, the structure density is ensured, and the conductivity and the uniformity of the zinc telluride film are ensured.
[0014] Preferably, the average length of the carbon nanotube is 8-12 μm.
[0015] By adopting the technical scheme, the strength of the zinc telluride target material is ensured while the conductive effect is ensured.
[0016] Preferably, the carboxyl-modified porous boron carbide is prepared by treating porous boron carbide with a sodium alginate solution.
[0017] By adopting the technical scheme, the carboxyl-modified porous boron carbide, the sodium alginate solution, the carboxyl group in the sodium alginate solution, the high porosity and good conductive effect of the porous boron carbide, the high porosity and network structure of the carboxyl-modified porous boron carbide and the amino carbon nanotube, and the conductive effect of the zinc telluride thin film are combined, so that the carrier concentration is improved, the conductive effect is improved, and the zinc telluride thin film has good conductivity.
[0018] Preferably, the average particle size of the porous boron carbide is 8-12 mu m, and the porosity is 20-25%.
[0019] By adopting the technical scheme, the adsorption of the porous structure is ensured, the carboxyl modification is facilitated, and the conductive effect of the zinc telluride target material is ensured.
[0020] Preferably, the polyethylene glycol solution is composed of a polyethylene glycol ethanol solution and ammonium bicarbonate particles, and the mass ratio of the polyethylene glycol ethanol solution to the ammonium bicarbonate particles is 1:0.1-0.2.
[0021] By adopting the technical scheme, the polyethylene glycol ethanol solution and the ammonium bicarbonate particles are combined, the ammonium bicarbonate particles are insoluble in ethanol, the ammonium bicarbonate particles can be dispersed in the polyethylene glycol ethanol solution, the adhesion of the polyethylene glycol ethanol solution is utilized, the ammonium bicarbonate particles are dispersed and adhered in the zinc telluride target material while the adhesion effect is exerted, the ammonium bicarbonate gradually pyrolyzes to produce gas as the zinc telluride target material is prepared and heated, a pore flow channel is provided, then the polyethylene glycol ethanol solution also gradually pyrolyzes to produce gas, the adhesion effect is ensured while the carrier concentration of the target material is improved, and thus the conductivity of the zinc telluride thin film prepared from the zinc telluride target material is improved.
[0022] Preferably, the polyethylene glycol is one or more of polyethylene glycol 4000, polyethylene glycol 8000, and polyethylene glycol 10000.
[0023] By adopting the above technical scheme, the polyethylene glycol 4000, the polyethylene glycol 8000 and the polyethylene glycol 10000 all have high viscosity, which ensures the bonding effect, so that the zinc telluride target is not prone to cracking and powder falling problems, and the thermal decomposition temperature of the polyethylene glycol 4000, the polyethylene glycol 8000 and the polyethylene glycol 10000 is higher than that of sodium bicarbonate, ethanol and water, thereby realizing a progressive thermal decomposition effect, the substances decomposed first generate pores, and the substances decomposed later realize a pore connection effect, through the pore connection, the carrier concentration is improved, and the conductivity is improved; and in the preparation process of the zinc telluride target, the temperature can be uniformly dispersed, the internal and external stability is kept balanced, thereby the sintering activity of the powder is uniformly controlled, the uniformity of the thin film is improved, and the conductivity is ensured.
[0024] Preferably, the binder is a polyvinyl alcohol aqueous solution.
[0025] By adopting the above technical scheme, the polyethylene glycol 4000, the polyethylene glycol 8000 and the polyethylene glycol 10000 all have high viscosity, which ensures the bonding effect, so that the zinc telluride target is not prone to cracking and powder falling problems, and the thermal decomposition temperature of the polyethylene glycol 4000, the polyethylene glycol 8000 and the polyethylene glycol 10000 is higher than that of sodium bicarbonate, ethanol and water, thereby realizing a progressive thermal decomposition effect, the substances decomposed first generate pores, and the substances decomposed later realize a pore connection effect, through the pore connection, the carrier concentration is improved, and the conductivity is improved; and in the preparation process of the zinc telluride target, the temperature can be uniformly dispersed, the internal and external stability is kept balanced, thereby the sintering activity of the powder is uniformly controlled, the uniformity of the thin film is improved, and the conductivity is ensured.
[0026] In a second aspect, the application provides a preparation method of a zinc telluride target, which adopts the following technical scheme:
[0027] A preparation method of a zinc telluride target, comprising the following steps:
[0028] S1, after the zinc telluride, the dopant and the binder are uniformly mixed, pre-pressing treatment is performed to obtain initial mixture;
[0029] S2, the initial mixture is heated to 600-750℃ at a heating rate of 2-5℃ / min, vacuum heat preservation is performed for 6-10h, then pressure heat preservation is performed for 1-2h, and the temperature is reduced to room temperature at a cooling rate of 1-3℃ / min, to obtain a finished target.
[0030] By adopting the above technical scheme, the heating rate and the temperature reached by heating are limited, so that the thermal decomposition substances in the initial mixture realize step-by-step thermal decomposition and gas generation, the pores are connected, the sintering activity of the powder on the inner and outer surfaces of the initial mixture is uniformly ensured while the zinc telluride and the dopant are uniformly contacted with high temperature, thereby in the preparation process of the thin film, good uniformity can be achieved; the temperature and the time are limited, so that the polyethylene glycol and other substances are uniformly removed, and are not prone to residual effects on the purity of the zinc telluride target, the sintering mode of vacuum sintering is adopted, the volatilization of the zinc telluride and the dopant under high temperature is effectively avoided, and when the zinc telluride thin film is prepared, the thin film has high conductivity.
[0031] In a third aspect, the application provides the application of the zinc telluride target in a zinc telluride thin film, which adopts the following technical scheme: the application of the zinc telluride target or the zinc telluride target prepared by the preparation method of the zinc telluride target in a zinc telluride thin film.
[0032] By adopting the technical scheme, the zinc telluride thin film prepared by using the zinc telluride target material has lower resistivity and higher conductivity.
[0033] To sum up, the application has the following beneficial effects:
[0034] 1. The zinc telluride, arsenic oxide and antimony oxide are combined, the multi-electron holes in arsenic and antimony are utilized, the higher carrier concentration is combined, the conductive effect of the zinc telluride target material is improved, the purity is higher, the bonding effect of the bonding agent is combined, the bonding density of the zinc telluride, arsenic oxide and antimony oxide is improved, the forming effect of the zinc telluride target material is ensured, the problems of powder falling and cracking are not prone to occur, with the thermal decomposition of the bonding liquid, the internal micropore porosity of the zinc telluride target material is improved, the film forming of the zinc telluride target material is promoted to be uniform, there are more pore channels, the conductive effect of the zinc telluride thin film is improved, and the zinc telluride thin film can be applied in the field of batteries.
[0035] 2. The arsenic oxide, amino carbon nanotube and polyethylene glycol solution are combined, the pore structure in the amino carbon nanotube is utilized by using the five electron holes of arsenic, the electron hole effect and the carrier concentration of the zinc telluride target material are further improved, thereby the conductivity of the zinc telluride target material is improved; the multi-pore hole effect of the amino carbon nanotube is combined with the electron hole effect of the arsenic oxide, the holes are docked and connected, thereby the carrier concentration is further improved, the conductive effect of the zinc telluride target material is improved; with the preparation of the zinc telluride target material, the polyethylene glycol can be decomposed to produce gas under heat, the zinc telluride target material is not prone to be compact in structure and affect the preparation of the zinc telluride thin film, and the zinc telluride target material and the zinc telluride thin film are not prone to be affected in the conductive effect due to the retention of impurities.
[0036] 3. The antimony oxide, carboxyl modified porous boron carbide and polyethylene glycol solution are combined, the layered lapping structure of the antimony and the carboxyl modified porous boron carbide can further improve the porosity and the electron hole pair, the conductive effect of the antimony and the boron carbide is combined, the conductivity is further improved, the multi-pore structure of the boron carbide and the lapping network pores of the antimony oxide, the carboxyl modified porous boron carbide and the polyethylene glycol solution are combined, the carrier concentration is further improved, thereby the conductivity of the zinc telluride target material is further improved. DETAILED DESCRIPTION
[0037] The application will be further described in detail below in combination with embodiments.
[0038] Preparation example of modified arsenic oxide
[0039] The modified arsenic oxide is prepared by the following method.
[0040] Take polyethylene glycol in ethanol stirring mixed until all dissolved, prepared mass fraction 10% polyethylene glycol ethanol solution, polyethylene glycol is polyethylene glycol 8000, the mass fraction of ethanol is 75%; Take 1kg polyethylene glycol ethanol solution and 0.15kg ammonium bicarbonate particles mixed stirring uniform, prepared polyethylene glycol solution; Ammonium bicarbonate particles average particle size is 5μm;
[0041] Take 1kg carbon nanotube is placed in 10kg dopamine solution soaking, the average length of carbon nanotube is 10μm, dopamine solution is mass fraction 10% dopamine aqueous solution, under the condition of 1000r / min rotation speed mixing stirring 20min, then filter separation of carbon nanotube, drying, get amino carbon nanotube;
[0042] On the surface of 1kg arsenic oxide uniform spraying 0.08kg polyethylene glycol solution, then add 0.03kg amino carbon nanotube, the addition rate of amino carbon nanotube is 30g / min, in the process of adding, arsenic oxide is constantly stirring under the speed of 120r / min, after mixing uniform, drying, dispersion, prepared finished product modified arsenic oxide.
[0043] Preparation example 2: the difference between this preparation example and preparation example 1 is:
[0044] Take polyethylene glycol in ethanol stirring mixed until all dissolved, prepared mass fraction 10% polyethylene glycol ethanol solution, polyethylene glycol is polyethylene glycol 4000, the mass fraction of ethanol is 75%; Take 1kg polyethylene glycol ethanol solution and 0.1kg ammonium bicarbonate particles mixed stirring uniform, prepared polyethylene glycol solution; Ammonium bicarbonate particles average particle size is 5μm;
[0045] Take 1kg carbon nanotube is placed in 10kg dopamine solution soaking, the average length of carbon nanotube is 8μm, dopamine solution is mass fraction 10% dopamine aqueous solution, under the condition of 1000r / min rotation speed mixing stirring 20min, then filter separation of carbon nanotube, drying, get amino carbon nanotube;
[0046] On the surface of 1kg arsenic oxide uniform spraying 0.05kg polyethylene glycol solution, then add 0.02kg amino carbon nanotube, the addition rate of amino carbon nanotube is 30g / min, in the process of adding, arsenic oxide is constantly stirring under the speed of 120r / min, after mixing uniform, drying, dispersion, prepared finished product modified arsenic oxide.
[0047] Preparation example 3: the difference between this preparation example and preparation example 1 is:
[0048] Take polyethylene glycol in ethanol stirring mixed until all dissolved, prepared mass fraction 10% polyethylene glycol ethanol solution, polyethylene glycol is polyethylene glycol 10000, the mass fraction of ethanol is 75%; Take 1kg polyethylene glycol ethanol solution and 0.2kg ammonium bicarbonate particles mixed stirring uniform, prepared polyethylene glycol solution; Ammonium bicarbonate particles average particle size is 5μm;
[0049] Take 1kg carbon nanotube is placed in 10kg dopamine solution soaking, the average length of carbon nanotube is 12μm, dopamine solution is mass fraction 10% dopamine aqueous solution, under the condition of 1000r / min rotation speed mixing stirring 20min, then filter separation out carbon nanotube, drying, get amino carbon nanotube;
[0050] In 1kg arsenic oxide surface evenly sprayed 0.1kg polyethylene glycol solution, then add 0.04kg amino carbon nanotube, the addition rate of amino carbon nanotube is 30g / min, in the process of adding, arsenic oxide is constantly stirring under the speed of 120r / min, after mixing uniform, drying, dispersion, prepared finished product modified arsenic oxide.
[0051] Preparation example of modified antimony oxide
[0052] Preparation example 4: modified antimony oxide is prepared by the following method:
[0053] Take polyethylene glycol in ethanol stirring mixed until all dissolved, prepared mass fraction 10% polyethylene glycol ethanol solution, polyethylene glycol is polyethylene glycol 8000, the mass fraction of ethanol is 75%; Take 1kg polyethylene glycol ethanol solution and 0.15kg ammonium bicarbonate particles mixed stirring uniform, prepared polyethylene glycol solution; Ammonium bicarbonate particles average particle size is 5μm;
[0054] Take 1kg porous boron carbide is placed in 9kg mass fraction 0.5% sodium alginate solution soaking, the porosity of porous boron carbide is 20-25%, the average particle size of porous boron carbide is 10μm, sodium alginate solution is mass fraction 1% sodium alginate aqueous solution, under the condition of 1000r / min stirring mixing 10min, then filter separation out porous boron carbide, drying, scattering, prepared carboxyl modified porous boron carbide;
[0055] In 1kg antimony oxide surface evenly sprayed 0.08kg polyethylene glycol solution, then evenly sprayed 0.02kg carboxyl modified porous boron carbide, the addition rate of carboxyl modified porous boron carbide is 30g / min, in the process of adding, antimony oxide is stirring under the speed of 120r / min, after mixing uniform, drying, dispersion, prepared finished product.
[0056] Preparation example 5: the difference between this preparation example and preparation example 4 is:
[0057] The polyethylene glycol is weighed and stirred in ethanol until completely dissolved to prepare a 10% polyethylene glycol ethanol solution, the polyethylene glycol is polyethylene glycol 4000, and the mass fraction of ethanol is 75%; 1 kg of the polyethylene glycol ethanol solution is mixed with 0.1 kg of ammonium bicarbonate particles to prepare a polyethylene glycol solution; the average particle size of the ammonium bicarbonate particles is 5 μm;
[0058] 1 kg of porous boron carbide is soaked in 9 kg of a 0.5% sodium alginate solution, the porosity of the porous boron carbide is 20-25%, the average particle size of the porous boron carbide is 8 μm, and the sodium alginate solution is a 1% sodium alginate aqueous solution; the mixture is stirred at 1000 r / min for 10 min, and then the porous boron carbide is separated by filtration, dried, and dispersed to prepare carboxyl-modified porous boron carbide;
[0059] 0.05 kg of the polyethylene glycol solution is uniformly sprayed on the surface of 1 kg of antimony oxide, and then 0.01 kg of the carboxyl-modified porous boron carbide is uniformly sprayed, the addition speed of the carboxyl-modified porous boron carbide is 30 g / min, the antimony oxide is stirred at a speed of 120 r / min during the addition process, and after uniform mixing, the product is prepared by drying and dispersing.
[0060] Preparation Example 6: The difference between this preparation example and Preparation Example 4 is that:
[0061] The polyethylene glycol is weighed and stirred in ethanol until completely dissolved to prepare a 10% polyethylene glycol ethanol solution, the polyethylene glycol is polyethylene glycol 10000, and the mass fraction of ethanol is 75%; 1 kg of the polyethylene glycol ethanol solution is mixed with 0.2 kg of ammonium bicarbonate particles to prepare a polyethylene glycol solution; the average particle size of the ammonium bicarbonate particles is 5 μm;
[0062] 1 kg of porous boron carbide is soaked in 9 kg of a 0.5% sodium alginate solution, the porosity of the porous boron carbide is 20-25%, the average particle size of the porous boron carbide is 12 μm, and the sodium alginate solution is a 1% sodium alginate aqueous solution; the mixture is stirred at 1000 r / min for 10 min, and then the porous boron carbide is separated by filtration, dried, and dispersed to prepare carboxyl-modified porous boron carbide;
[0063] 0.05 kg of the polyethylene glycol solution is uniformly sprayed on the surface of 1 kg of antimony oxide, and then 0.01 kg of the carboxyl-modified porous boron carbide is uniformly sprayed, the addition speed of the carboxyl-modified porous boron carbide is 30 g / min, the antimony oxide is stirred at a speed of 120 r / min during the addition process, and after uniform mixing, the product is prepared by drying and dispersing.
[0064] Example
[0065] Example 1: A zinc telluride target material:
[0066] Zinc telluride 98 kg, dopant 1.5 kg, binder 0.5 kg; the dopant is composed of arsenic oxide and antimony oxide with a mass ratio of 1:1.5, the arsenic oxide is the modified arsenic oxide prepared in Preparation Example 1; the antimony oxide is the modified antimony oxide prepared in Preparation Example 4; the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the polyvinyl alcohol aqueous solution is 1%;
[0067] The preparation method is as follows:
[0068] S1, after the dopant and the binder are mixed, zinc telluride is added, and then mixed uniformly, and pre-pressing treatment is performed under a pressure of 25T to obtain a preliminary mixture;
[0069] S2, the preliminary mixture is heated to 690℃ at a heating rate of 3℃ / min, vacuum heat preservation is performed for 8h, then pressure heat preservation is performed for 2h, and then the temperature is reduced to room temperature at a cooling rate of 2℃ / min to obtain a finished target material.
[0070] Example 2: The difference between this example and Example 1 is that:
[0071] Zinc telluride 95 kg, dopant 3 kg, binder 2 kg; the dopant is composed of arsenic oxide and antimony oxide with a mass ratio of 1:1, the arsenic oxide is the modified arsenic oxide prepared in Preparation Example 2; the antimony oxide is the modified antimony oxide prepared in Preparation Example 5; the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the polyvinyl alcohol aqueous solution is 1%;
[0072] The preparation method is as follows:
[0073] S1, after the dopant and the binder are mixed, zinc telluride is added, and then mixed uniformly, and pre-pressing treatment is performed under a pressure of 25T to obtain a preliminary mixture;
[0074] S2, the preliminary mixture is heated to 600℃ at a heating rate of 2℃ / min, vacuum heat preservation is performed for 10h, then pressure heat preservation is performed for 2h, and then the temperature is reduced to room temperature at a cooling rate of 1℃ / min to obtain a finished target material.
[0075] Example 3: The difference between this example and Example 1 is that:
[0076] Zinc telluride 99 kg, dopant 0.5 kg, binder 0.5 kg; the dopant is composed of arsenic oxide and antimony oxide with a mass ratio of 1:2, the arsenic oxide is the modified arsenic oxide prepared in Preparation Example 3; the antimony oxide is the modified antimony oxide prepared in Preparation Example 6; the binder is a polyvinyl alcohol aqueous solution, and the mass fraction of the polyvinyl alcohol aqueous solution is 1%;
[0077] The preparation method is as follows:
[0078] S1, the dopant and the binder are weighed and mixed, then zinc telluride is added and mixed uniformly, and pre-pressing is performed under a pressure of 25T to obtain a preliminary mixture;
[0079] S2, the preliminary mixture is heated to 750°C at a heating rate of 5°C / min, vacuumized for 6h, then pressurized for 1h, and cooled to room temperature at a cooling rate of 3°C / min to obtain a finished target material.
[0080] Comparative Example
[0081] Comparative Example 1: The difference between this comparative example and Example 1 is that:
[0082] No binder and dopant are added to the raw materials.
[0083] Comparative Example 2: The difference between this comparative example and Example 1 is that:
[0084] The dopant in the raw materials is elemental antimony.
[0085] Comparative Example 3: The difference between this comparative example and Example 1 is that:
[0086] The heating rate in S2 is 10°C / min.
[0087] Comparative Example 4: The difference between this comparative example and Example 1 is that:
[0088] No amino carbon nanotubes are added during the preparation of the modified arsenic oxide.
[0089] Comparative Example 5: The difference between this comparative example and Example 1 is that:
[0090] During the preparation of the modified arsenic oxide, the same mass of carbon nanotubes is used to replace the amino carbon nanotubes, and no polyethylene glycol solution is added.
[0091] Comparative Example 6: The difference between this comparative example and Example 1 is that:
[0092] During the preparation of the modified arsenic oxide, no ammonium bicarbonate particles are added to the polyethylene glycol solution.
[0093] Comparative Example 7: The difference between this comparative example and Example 1 is that:
[0094] During the preparation of the modified antimony oxide, no carboxyl-modified porous boron carbide is added.
[0095] Comparative Example 8: The difference between this comparative example and Example 1 is that:
[0096] During the preparation of the modified antimony oxide, the same mass of silicon carbide is used to replace the carboxyl-modified porous boron carbide, and the porosity of the silicon carbide is less than 1%.
[0097] Applications
[0098] Zinc telluride targets were prepared by the preparation methods of Examples 1-3 and Comparative Examples 1-8, respectively, for preparing zinc telluride thin films.
[0099] Performance detection test
[0100] 1. Relative density detection
[0101] The finished zinc telluride targets were prepared by the preparation methods of Examples 1-3 and Comparative Examples 1-8, respectively, and the calculation method of relative density was: relative density = actual density / theoretical density, wherein the actual density was measured by Archimedes drainage method.
[0102] 2. Stability detection
[0103] The finished zinc telluride targets were prepared by the preparation methods of Examples 1-3 and Comparative Examples 1-3, respectively, and the powder dropping and cracking conditions were recorded and scored, with no powder dropping and cracking being 10 points, and severe powder dropping and cracking being 1 point.
[0104] In the table, " / " represents that the corresponding example is not detected for the item, so there is no data.
[0105] Table 1 Performance test table
[0106]
[0107]
[0108] 3. Conductivity detection
[0109] The finished zinc telluride thin films were prepared by the preparation methods of Examples 1-3 and Comparative Examples 1-8, respectively, and the resistivity, mobility and carrier concentration of the thin films were detected by using a Hall effect tester to record the data.
[0110] In the table, " / " represents that the corresponding example is not detected for the item, so there is no data.
[0111] Table 2 Thin film performance test table
[0112]
[0113] It can be seen from the combination of examples 1-3 and tables 1 and 2 that the target material prepared in the application has a high relative density, and is not prone to cracking and powdering. The film made of the target material has a low resistivity, a high mobility and a high carrier concentration, which indicates that the modified arsenic oxide and the modified antimony oxide are matched to appropriately reduce the relative density, so that the target material is not cracked and does not fall off, and the relative density is low, which indicates that the porosity is high. The modified arsenic oxide and the modified antimony oxide generate thermal decomposition gas during the preparation of the target material, which further increases the connected porosity, reduces the sintering activity of the powder, and ensures the conductivity effect after film formation.
[0114] It can be seen from the combination of examples 1 and comparative examples 1-8 and tables 1 and 2 that the target material prepared in comparative example 1 has a higher relative density and a lower fraction than example 1. The resistivity of the film prepared in comparative example 1 is higher than that of example 1, and the carrier concentration is lower than that of example 1. This indicates that the addition of the binder and the dopant can control the relative density while preventing the target material from cracking, and the film prepared has good conductivity.
[0115] The dopant of comparative example 2 is elemental antimony. The target material prepared in comparative example 2 has a higher relative density than example 1, and the resistivity of the film prepared in comparative example 2 is higher than that of example 1, and the carrier concentration is lower than that of example 1. This indicates that the combination of arsenic oxide and antimony oxide can improve the conductivity of the film.
[0116] The heating rate of comparative example 3 is 10℃ / min. The target material prepared in comparative example 3 has a higher relative density than example 1, and the resistivity of the film prepared in comparative example 3 is higher than that of example 1, and the carrier concentration is lower than that of example 1. This indicates that a faster heating rate can affect the uniformity and conductivity of the target material.
[0117] Comparative example 4 does not add amino carbon nanotubes during the preparation of the modified arsenic oxide. The target material of comparative example 4 has a higher relative density than example 1, and the resistivity of the film prepared in comparative example 4 is higher than that of example 1, and the carrier concentration is lower than that of example 1. This indicates that the carbon nanotubes themselves have a certain porosity, which can reduce the relative density, and the addition of amino carbon nanotubes can increase the carrier concentration and improve the conductivity effect of the zinc telluride target material.
[0118] In the preparation of the modified arsenic oxide of Comparative Example 5, the amino carbon nanotubes are replaced with the same mass of carbon nanotubes, and no polyethylene glycol solution is added. Compared with Example 1, the relative density of the target of Comparative Example 5 is greater than that of Example 1, the resistivity of the film is higher than that of Example 1, and the carrier concentration is lower than that of Example 1. It is shown that after the amino treatment, the bonding effect of arsenic oxide and polyethylene glycol can be improved, and with the thermal decomposition of polyethylene glycol and the electron hole effect of arsenic oxide, the relative density can be properly adjusted. At the same time, the carboxyl group on the surface of the modified antimony oxide and the hydroxyl group in the bonding agent cooperate with each other to bond, ensuring the structural density while ensuring the conductive effect of the zinc telluride film.
[0119] In the preparation of the modified arsenic oxide of Comparative Example 6, no ammonium bicarbonate particles are added to the polyethylene glycol solution. Compared with Example 1, the relative density of the target of Comparative Example 6 is greater than that of Example 1, the resistivity of the film is higher than that of Example 1, and the carrier concentration is lower than that of Example 1. It is shown that with the preparation of the zinc telluride target heated, ammonium bicarbonate gradually decomposes to produce gas, providing a pore flow channel. Then, the polyethylene glycol ethanol solution also gradually decomposes to produce gas, ensuring the bonding effect while improving the carrier concentration of the target, thereby improving the conductivity of the zinc telluride film prepared from the zinc telluride target.
[0120] In the preparation of the modified antimony oxide of Comparative Example 7, no carboxyl-modified porous boron carbide is added. Compared with Example 1, the relative density of the target of Comparative Example 7 is greater than that of Example 1, the resistivity of the film is higher than that of Example 1, and the carrier concentration is lower than that of Example 1. It is shown that the layered lapping structure of antimony, carboxyl-modified porous boron carbide, and polyethylene glycol solution cooperates to further improve the porosity and carrier concentration, and cooperates with the conductive effect of antimony and boron carbide to further improve the conductivity. In addition, the porous structure of boron carbide and the lapping network pores of antimony, carboxyl-modified porous boron carbide, and polyethylene glycol solution further improve the carrier concentration, thereby further improving the conductivity of the zinc telluride target.
[0121] In the preparation of the modified antimony oxide of Comparative Example 8, the same mass of silicon carbide is used to replace the carboxyl-modified porous boron carbide. The porosity of silicon carbide is less than 1%. Compared with Example 1, the relative density of the target of Comparative Example 8 is greater than that of Example 1, the resistivity of the film is higher than that of Example 1, and the carrier concentration is lower than that of Example 1. It is shown that the low porosity of silicon carbide affects the electronic capacity, thereby affecting the conductivity of the film.
[0122] The specific embodiments are merely illustrative of the present application, and are not intended to limit the present application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the present specification, and the modifications are protected by the patent law as long as they are within the scope of the claims of the present application.
Claims
1. A zinc telluride target material, characterized in that, The raw materials comprise the following parts by weight: 95-99 parts zinc telluride, 0.5-3 parts dopant, and 0.5-2 parts binder; the dopant is composed of modified arsenic oxide and modified antimony oxide in a mass ratio of 1:1-2; the modified arsenic oxide is prepared by a mass ratio of arsenic oxide, amino carbon nanotubes, and polyethylene glycol solution in a mass ratio of 1:0.02-0.04:0.05-0.1; the modified antimony oxide is prepared by a mass ratio of antimony oxide, carboxyl-modified porous boron carbide, and polyethylene glycol solution in a mass ratio of 1:0.01-0.03:0.05-0.
1.
2. The zinc telluride target material according to claim 1, characterized in that: The amino-carbon nanotubes are prepared by modifying carbon nanotubes with dopamine.
3. The zinc telluride target material according to claim 2, characterized in that, The average length of the carbon nanotubes is 8-12 μm.
4. The zinc telluride target material according to claim 1, characterized in that, The carboxyl-modified porous boron carbide was prepared by treating porous boron carbide with sodium alginate solution.
5. A zinc telluride target material according to claim 4, characterized in that, The porous boron carbide has an average particle size of 8-12 μm and a porosity of 20-25%.
6. The zinc telluride target material according to claim 1, characterized in that, The polyethylene glycol solution is composed of a polyethylene glycol ethanol solution and ammonium bicarbonate microparticles in a mass ratio of 1:0.1-0.
2.
7. A zinc telluride target material according to claim 6, characterized in that, The polyethylene glycol is one or more of polyethylene glycol 4000, polyethylene glycol 8000, and polyethylene glycol 10000.
8. A zinc telluride target material according to claim 1, characterized in that, The adhesive is an aqueous solution of polyvinyl alcohol.
9. A method for preparing a zinc telluride target according to any one of claims 1-8, characterized in that, Includes the following steps: S1. Weigh zinc telluride, dopant, and binder, mix them evenly, and then pre-press them to obtain the initial mixture. S2. The initial mixture is heated to 600-750℃ at a heating rate of 2-5℃ / min and vacuum-held for 6-10 hours. Then it is pressurized and held for 1-2 hours, and cooled to room temperature at a cooling rate of 1-3℃ / min to obtain the finished target material.
10. The application of the zinc telluride target material prepared by any one of claims 1-8 or the zinc telluride target material prepared by the preparation method of claim 9 in zinc telluride thin films.
Citation Information
Patent Citations
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