CN115418616B - Tungsten alloy target material for electrically-controlled color-changing glass and preparation method thereof - Google Patents
Tungsten alloy target material for electrically-controlled color-changing glass and preparation method thereof Download PDFInfo
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- CN115418616B CN115418616B CN202211374033.3A CN202211374033A CN115418616B CN 115418616 B CN115418616 B CN 115418616B CN 202211374033 A CN202211374033 A CN 202211374033A CN 115418616 B CN115418616 B CN 115418616B
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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
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- C22C27/04—Alloys based on tungsten or molybdenum
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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
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Abstract
The invention discloses a tungsten alloy target material for electrically-controlled color-changing glass and a preparation method thereof, wherein the tungsten alloy target material comprises the following raw materials in percentage by weight: 1.2 to 1.5 percent of silicon powder, 0.3 to 0.6 percent of chromium powder, 0.2 to 0.4 percent of manganese powder, 0.1 to 0.4 percent of thermal modifier, 0.2 to 0.6 percent of smelting modifier and the balance of 0.1 to 0.4 percent of tungsten; the preparation method of the smelting modifier comprises the following steps: the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 1-5% of the total weight of the titanium dioxide, and stirring and mixing fully; step two: then the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 500-600 ℃, the calcining time is 15-25min, and the calcining is finished. The tungsten alloy target prepared by taking tungsten powder as a main raw material has good density, and the color-changing film prepared by the tungsten alloy target has more stable color-changing effect.
Description
Technical Field
The invention relates to the technical field of metal targets, in particular to a tungsten alloy target for electrically-controlled color-changing glass and a preparation method thereof.
Background
The color-changing glass is glass which changes color under certain conditions such as illumination, temperature, electric field or current, surface pressure and the like, changes correspondingly along with the change of the conditions, and can be reversibly and automatically restored to an initial state after the applied conditions disappear, and is also called as light-adjusting glass. The transmission characteristic of the color-changing glass is changed along with the change of the external environment, so that the effective control of solar radiation energy can be realized, and the aim of saving energy is fulfilled. The target material is the target material bombarded by high-speed charged energy particles. There are metals, alloys, oxides, and the like. For example: the evaporation magnetron sputtering coating is heating evaporation coating, aluminum film and the like. Different target materials (such as aluminum, copper, stainless steel, titanium, nickel targets and the like) are replaced, and different film systems (such as superhard, wear-resistant and corrosion-resistant alloy films and the like) can be obtained.
The existing tungsten alloy target material has poor compactness, unstable performance and poor discoloration stability, and therefore the invention provides the tungsten alloy target material for the electrically-controlled discoloration glass and the preparation method thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a tungsten alloy target material for electrically-controlled color-changing glass and a preparation method thereof, so as to solve the problems in the background art.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the invention provides a tungsten alloy target material for electrically-controlled color-changing glass, which comprises the following raw materials in percentage by weight:
1.2 to 1.5 percent of silicon powder, 0.3 to 0.6 percent of chromium powder, 0.2 to 0.4 percent of manganese powder, 0.1 to 0.4 percent of thermal modifier, 0.2 to 0.6 percent of smelting modifier and the balance of 0.1 to 0.4 percent of tungsten;
the preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 1-5% of the total weight of the titanium dioxide, and stirring and mixing fully;
step two: then the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 500-600 ℃, the calcining time is 15-25min, and the calcining is finished;
step three: and (3) feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 10-20min, the ball milling rotation speed is 1000-1500r/min, and the smelting modifier is obtained after the ball milling is finished.
Preferably, the tungsten alloy target for the electrically-controlled color-changing glass comprises the following raw materials in parts by weight:
1.35 percent of silicon powder, 0.45 percent of chromium powder, 0.3 percent of manganese powder, 0.3 percent of thermal modifier, 0.4 percent of smelting modifier and the balance of 0.25 percent of tungsten.
Preferably, the preparation method of the modified additive comprises the following steps:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: pouring and molding, adopting extrusion treatment, wherein the extrusion speed is 0.01-0.03m/s, the pressure is 20-30Mpa, the extrusion is 10-20s, and the extrusion is finished;
s3: and finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling on the mixture by a sieve of 10-20 meshes to obtain the modified additive.
Preferably, the preparation method of the thermal modifier comprises the following steps:
s1: mixing cerium oxide and strontium oxide according to a weight ratio of 1:2, and then carrying out smelting treatment to obtain a smelting material;
s2: adding yttrium oxide which accounts for 1-6% of the total weight of the smelting material into the smelting material, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally cooling and forming, performing thermal homogenization treatment at the temperature of 100-300 ℃ for 10-20min, and cooling to room temperature at the speed of 1-3 ℃/min after the treatment is finished to obtain the thermal modifier.
Preferably, the frequency of the microwave treatment is 300-500KHz, and the treatment time is 5-10min.
The invention provides a preparation method of a tungsten alloy target material for electrically-controlled color-changing glass, which comprises the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then carrying out cold plasma treatment, wherein the treatment power is 100W, and the treatment time is 10-20min;
step three: then carrying out proton irradiation treatment for 5-10min, wherein the irradiation power is 150-200W;
step four: sending into surface treatment liquid for microwave treatment with treatment power of 100-300W and treatment time of 10-20min, washing with water, and drying;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target material of the invention after the treatment is finished.
Preferably, the preparation method of the surface treatment liquid comprises the following steps:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder 10-20% of the total weight of the wollastonite agent, stirring at the rotation speed of 100-300r/min for 20-30min, and stirring to obtain surface treatment liquid.
Preferably, the wollastonite agent is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to a weight ratio of 3.
Preferably, the specific operation steps of the thermal modification homogenization treatment are as follows:
s1: heating to 210-220 ℃ at the speed of 1-3 ℃/min, and carrying out heat preservation reaction for 10-20min;
s2: then air-cooling to room temperature, heating to 310-350 ℃ at the speed of 3-5 ℃/min, and keeping the temperature for 25-35min;
s3: and finally, carrying out oil cooling to room temperature by using oil at the temperature of 1-3 ℃, and then washing and drying.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the tungsten alloy target prepared by taking the tungsten powder as the main raw material, the prepared target has good density, and the color-changing film prepared by the target has more stable color-changing effect;
2. the smelting modifier added into the raw materials of the product adopts the proportion of titanium dioxide and a-alumina powder and the needle structure of the a-alumina powder, and can be filled in the target structure in the preparation of the target so as to improve the density of the product; the modified additive adopts Sn powder and lanthanum oxide, and can improve the ductility and the fluidity of the raw materials in the preparation of the target after treatment, thereby promoting the full reaction of the raw materials and improving the preparation efficiency of the target;
3. in the preparation of the metal target, cerium oxide and strontium oxide are adopted as thermal modifiers to be matched with yttrium oxide, so that the thermal modifiers have the effects of refining grains, preventing the grains from growing and improving the color change stability of the target in the thermal modification homogenization treatment;
4. before the product is treated by the surface treatment liquid, after plasma and proton irradiation treatment, the microstructure is sparse and activated, and calcium carbonate is provided by oyster shell powder in the surface treatment liquid, so that the adsorption force is exerted, the wollastonite in the wollastonite agent can be conveniently further filled in a structure, the needle-shaped wollastonite has a reinforcing effect, and the performance of the product target is further improved by matching thermal modification homogenization treatment.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1.
The tungsten alloy target for the electrically-controlled color-changing glass comprises the following raw materials in percentage by weight:
1.2% of silicon powder, 0.3% of chromium powder, 0.2% of manganese powder, 0.1% of thermal modifier, 0.2% of smelting modifier and the balance of 0.1% of tungsten;
the preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 1% of the total weight of the titanium dioxide, and stirring and mixing the mixture fully;
step two: then, the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 500 ℃, the calcining time is 15min, and the calcining is finished;
step three: and (3) feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 10min, the ball milling rotation speed is 1000r/min, and the smelting modifier is obtained after the ball milling is finished.
The preparation method of the modified additive of this example is:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: then pouring and forming are carried out, extrusion processing is adopted, the extrusion speed is 0.01m/s, the pressure is 20Mpa, the extrusion is carried out for 10s, and the extrusion is finished;
s3: and finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling on the mixture by a sieve of 10 meshes to obtain the modified additive.
The preparation method of the thermal modifier in the embodiment comprises the following steps:
s1: cerium oxide and strontium oxide are mixed according to the weight ratio of 1:2, and then smelting treatment is carried out to obtain a smelting material;
s2: adding yttrium oxide accounting for 1 percent of the total weight of the smelting materials into the smelting materials, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally cooling and forming, carrying out thermal homogenization treatment at the temperature of 100 ℃ for 10min, and cooling to room temperature at the speed of 1 ℃/min after the treatment is finished to obtain the thermal modifier.
The frequency of the microwave treatment in this embodiment is 300KHz, and the treatment time is 5min.
The preparation method of the tungsten alloy target material for the electrically-controlled color-changing glass comprises the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then carrying out cold plasma treatment, wherein the treatment power is 100W, and the treatment time is 10min;
step three: then carrying out proton irradiation treatment for 5min, wherein the irradiation power is 150W;
step four: sending the mixture into surface treatment liquid for microwave treatment, wherein the treatment power is 100W, the treatment time is 10min, and after the treatment is finished, washing and drying the mixture;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target material of the invention after the treatment is finished.
The preparation method of the surface treatment liquid in this example was:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder with 10% of wollastonite agent total weight, stirring at 100r/min for 20min, and stirring to obtain surface treatment liquid.
The wollastonite agent of the present embodiment is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to a weight ratio of 3.
The specific operation steps of the thermal modification homogenization treatment in this example are as follows:
s1: heating to 210 ℃ at the speed of 1 ℃/min, and carrying out heat preservation reaction for 10min;
s2: then air-cooling to room temperature, heating to 310 ℃ at the speed of 3 ℃/min, and keeping the temperature for 25min;
s3: and finally, cooling the mixture to room temperature by using oil at the temperature of 1 ℃, and then washing and drying the mixture.
Example 2.
The tungsten alloy target for the electrically-controlled color-changing glass comprises the following raw materials in percentage by weight:
1.5% of silicon powder, 0.6% of chromium powder, 0.4% of manganese powder, 0.4% of thermal modifier, 0.6% of smelting modifier and the balance of tungsten, wherein the balance is 0.4%;
the preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 1-5% of the total weight of the titanium dioxide, and stirring and mixing fully;
step two: then, the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 600 ℃, the calcining time is 25min, and the calcining is finished;
step three: and (3) feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 20min, the ball milling rotation speed is 1500r/min, and the smelting modifier is obtained after the ball milling is finished.
The preparation method of the modified additive of this example is:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: then pouring and forming are carried out, extrusion processing is adopted, the extrusion speed is 0.03m/s, the pressure is 30Mpa, the extrusion is carried out for 20s, and the extrusion is finished;
s3: and finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling for 20 meshes to obtain the modified additive.
The preparation method of the thermal modifier in the embodiment comprises the following steps:
s1: cerium oxide and strontium oxide are mixed according to the weight ratio of 1:2, and then smelting treatment is carried out to obtain a smelting material;
s2: adding yttrium oxide accounting for 6 percent of the total weight of the smelting materials into the smelting materials, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally cooling and forming, carrying out thermal homogenization treatment at the temperature of 300 ℃ for 20min, and cooling to room temperature at the speed of 3 ℃/min after the treatment is finished to obtain the thermal modifier.
The frequency of the microwave treatment in this embodiment is 500KHz, and the treatment time is 10min.
The preparation method of the tungsten alloy target material for the electrically-controlled color-changing glass comprises the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then carrying out cold plasma treatment with the treatment power of 100W and the treatment time of 20min;
step three: then carrying out proton irradiation treatment for 10min, wherein the irradiation power is 200W;
step four: sending the mixture into surface treatment liquid for microwave treatment, wherein the treatment power is 300W, the treatment time is 20min, and after the treatment is finished, washing and drying the mixture;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target material of the invention after the treatment is finished.
The preparation method of the surface treatment liquid in this example was:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder accounting for 20% of the total weight of the wollastonite agent, stirring at the rotating speed of 300r/min for 30min, and obtaining the surface treatment liquid after stirring.
The wollastonite agent of the embodiment is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to the weight ratio of 3.
The specific operation steps of the thermal modification homogenization treatment in this example are as follows:
s1: heating to 220 ℃ at the speed of 3 ℃/min, and reacting for 20min under the condition of heat preservation;
s2: then air-cooling to room temperature, heating to 350 ℃ at the speed of 5 ℃/min, and keeping the temperature for 35min;
s3: and finally, carrying out oil cooling to room temperature by using oil at the temperature of 3 ℃, and then washing and drying.
Example 3.
The tungsten alloy target for the electrically-controlled color-changing glass comprises the following raw materials in percentage by weight:
1.35 percent of silicon powder, 0.45 percent of chromium powder, 0.3 percent of manganese powder, 0.3 percent of thermal modifier, 0.4 percent of smelting modifier and the balance of 0.25 percent of tungsten.
The preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 3 percent of the total weight of the titanium dioxide, and stirring and mixing the mixture fully;
step two: then, the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 550 ℃, the calcining time is 20min, and the calcining is finished;
step three: and (3) feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 15min, the ball milling rotation speed is 1250r/min, and the smelting modifier is obtained after the ball milling is finished.
The preparation method of the modified additive of this example is:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: then pouring and forming are carried out, extrusion processing is adopted, the extrusion speed is 0.02m/s, the pressure is 25Mpa, the extrusion is carried out for 15s, and the extrusion is finished;
s3: and finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling for 15 meshes to obtain the modified additive.
The preparation method of the thermal modifier in the embodiment comprises the following steps:
s1: cerium oxide and strontium oxide are mixed according to the weight ratio of 1:2, and then smelting treatment is carried out to obtain a smelting material;
s2: adding yttrium oxide accounting for 3.5 percent of the total weight of the smelting materials into the smelting materials, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally cooling and forming, carrying out thermal homogenization treatment at the temperature of 200 ℃ for 15min, and cooling to room temperature at the speed of 2 ℃/min after the treatment is finished to obtain the thermal modifier.
The frequency of the microwave treatment in this example is 400KHz, and the treatment time is 7.5min.
The preparation method of the tungsten alloy target material for the electrically-controlled color-changing glass comprises the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then carrying out cold plasma treatment, wherein the treatment power is 100W, and the treatment time is 15min;
step three: then carrying out proton irradiation treatment for 7.5min, wherein the irradiation power is 175W;
step four: sending into surface treatment liquid for microwave treatment with treatment power of 200W for 10-20min, washing with water, and drying;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target material of the invention after the treatment is finished.
The preparation method of the surface treatment liquid in this example was:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder 15% of the total weight of the wollastonite agent, stirring at the rotation speed of 200r/min for 25min, and obtaining the surface treatment liquid after stirring.
The wollastonite agent of the embodiment is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to the weight ratio of 3.
The specific operation steps of the thermal modification homogenization treatment in this example are as follows:
s1: heating to 215 ℃ at the speed of 2 ℃/min, and carrying out heat preservation reaction for 15min;
s2: then air cooling to room temperature, heating to 330 ℃ at the speed of 4 ℃/min, and keeping the temperature for 30min;
s3: and finally, carrying out oil cooling to room temperature by using oil at the temperature of 3 ℃, and then washing and drying.
Example 4.
The tungsten alloy target for the electrically-controlled color-changing glass comprises the following raw materials in percentage by weight:
1.3% of silicon powder, 0.4% of chromium powder, 0.25% of manganese powder, 0.2% of thermal modifier, 0.25% of smelting modifier and the balance of 0.2% of tungsten;
the preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing titanium dioxide with alpha-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 2% of the total weight of the titanium dioxide, and stirring and mixing fully;
step two: then, the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 520 ℃, the calcining time is 16min, and the calcining is finished;
step three: and (3) feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 14min, the ball milling rotation speed is 1200r/min, and the smelting modifier is obtained after the ball milling is finished.
The preparation method of the modified additive of this example is:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: then pouring and forming are carried out, extrusion processing is adopted, the extrusion speed is 0.015m/s, the pressure is 23Mpa, the extrusion is carried out for 12s, and the extrusion is finished;
s3: and finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling on the mixture by a sieve of 10-20 meshes to obtain the modified additive.
The preparation method of the thermal modifier in the embodiment comprises the following steps:
s1: cerium oxide and strontium oxide are mixed according to the weight ratio of 1:2, and then smelting treatment is carried out to obtain a smelting material;
s2: adding yttrium oxide accounting for 2 percent of the total weight of the smelting materials into the smelting materials, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally, cooling and forming, carrying out thermal homogenization treatment at the temperature of 150 ℃ for 12min, and cooling to room temperature at the speed of 1.2 ℃/min after the treatment is finished to obtain the thermal modifier.
The frequency of the microwave treatment of the embodiment is 300-500KHz, and the treatment time is 5-10min.
The preparation method of the tungsten alloy target material for the electrically-controlled color-changing glass comprises the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then carrying out cold plasma treatment, wherein the treatment power is 100W, and the treatment time is 12min;
step three: then carrying out proton irradiation treatment for 6min, wherein the irradiation power is 150-200W;
step four: sending the mixture into surface treatment liquid for microwave treatment, wherein the treatment power is 120W, the treatment time is 13min, and after the treatment is finished, washing and drying the mixture;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target material after the treatment is finished.
The preparation method of the surface treatment liquid in this example includes:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder accounting for 12% of the total weight of the wollastonite agent, stirring at the rotating speed of 120r/min for 23min, and obtaining the surface treatment liquid after stirring.
The wollastonite agent of the present embodiment is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to a weight ratio of 3.
The specific operation steps of the thermal modification homogenization treatment in this example are as follows:
s1: heating to 212 ℃ at the speed of 1.2 ℃/min, and carrying out heat preservation reaction for 13min;
s2: then air-cooling to room temperature, heating to 320 ℃ at the speed of 3.5 ℃/min, and keeping the temperature for 28min;
s3: and finally, carrying out oil cooling to room temperature by using oil at the temperature of 1.2 ℃, and then washing and drying.
Comparative example 1.
Unlike example 3, no smelting modifier was added.
Comparative example 2.
The difference from the example 3 is that no modifying additive is added to the smelting modifier.
Comparative example 3.
In contrast to example 3, no thermal modifier was added.
Comparative example 4.
Unlike example 3, the surface treatment liquid was not used.
Comparative example 5.
In contrast to example 3, no thermal modification homogenization treatment was used.
The raw materials of examples 1 to 4 and comparative examples 1 to 5 of the present invention were sputtered onto a glass substrate by a sputtering machine to form a metal target.
As can be seen from examples 1-4 and comparative examples 1-5, the target material of the product of the invention, example 3, has a density as high as 10.98g/cm, an average crystal grain size as low as 1.9um, and the product has excellent performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The tungsten alloy target material for the electrically-controlled color-changing glass is characterized by comprising the following raw materials in percentage by weight:
1.2-1.5% of silicon powder, 0.3-0.6% of chromium powder, 0.2-0.4% of manganese powder, 0.1-0.4% of thermal modifier, 0.2-0.6% of smelting modifier and the balance of tungsten;
the preparation method of the smelting modifier comprises the following steps:
the method comprises the following steps: mixing the titanium dioxide with the a-alumina powder according to the weight ratio of 1:2, then adding a modified additive accounting for 1-5% of the total weight of the titanium dioxide, and stirring and mixing fully;
step two: then the mixture is sent into a calcining furnace for calcining treatment, the calcining temperature is 500-600 ℃, the calcining time is 15-25min, and the calcining is finished;
step three: feeding the calcined product material into a ball mill for ball milling, wherein the ball milling time is 10-20min, the ball milling rotation speed is 1000-1500r/min, and obtaining a smelting modifier after the ball milling is finished; the preparation method of the modified additive comprises the following steps:
s1: mixing Sn powder and lanthanum oxide according to a weight ratio of 3:1, and then smelting to molten liquid;
s2: pouring and molding, adopting extrusion treatment, wherein the extrusion speed is 0.01-0.03m/s, the pressure is 20-30Mpa, the extrusion is 10-20s, and the extrusion is finished;
s3: finally, carrying out ball milling treatment, finishing ball milling, and carrying out ball milling on the mixture by a sieve of 10-20 meshes to obtain a modified additive; the preparation method of the thermal modifier comprises the following steps:
s1: cerium oxide and strontium oxide are mixed according to the weight ratio of 1:2, and then smelting treatment is carried out to obtain a smelting material;
s2: adding yttrium oxide which accounts for 1-6% of the total weight of the smelting material into the smelting material, continuously and fully smelting, and adopting microwave treatment in the smelting process;
s3: and finally cooling and forming, carrying out thermal homogenization treatment at the temperature of 100-300 ℃ for 10-20min, and cooling to room temperature at the speed of 1-3 ℃/min after the treatment is finished to obtain the thermal modifier.
2. The tungsten alloy target material for electrically controlled color-changing glass according to claim 1, wherein the tungsten alloy target material for electrically controlled color-changing glass comprises the following raw materials in parts by weight:
1.35% of silicon powder, 0.45% of chromium powder, 0.3% of manganese powder, 0.3% of thermal modifier, 0.4% of smelting modifier and the balance of tungsten.
3. The tungsten alloy target for electrically controlled color-changing glass according to claim 1, wherein the frequency of the microwave treatment is 300-500KHz, and the treatment time is 5-10min.
4. The preparation method of the tungsten alloy target material for the electrically controlled color-changing glass according to any one of claims 1 to 3, characterized by comprising the following steps:
the method comprises the following steps: completely smelting raw materials of silicon powder, chromium powder, manganese powder, a thermal modifier, a smelting modifier and the balance of tungsten to obtain a smelting material;
step two: cooling and shaping the smelting material, and then performing cold plasma treatment, wherein the treatment power is 100W, and the treatment time is 10-20min;
step three: then carrying out proton irradiation treatment for 5-10min, wherein the irradiation power is 150-200W;
step four: sending into surface treatment liquid for microwave treatment with treatment power of 100-300W and treatment time of 10-20min, washing with water, and drying;
step five: and then carrying out thermal modification homogenization treatment, and obtaining the tungsten alloy target after the treatment is finished.
5. The method for preparing the tungsten alloy target material for the electrically-controlled color-changing glass according to claim 4, wherein the method for preparing the surface treatment liquid comprises the following steps:
adding hydrochloric acid into wollastonite agent, adjusting pH to 5.0, adding oyster shell powder 10-20% of the total weight of the wollastonite agent, stirring at the rotation speed of 100-300r/min for 20-30min, and obtaining the surface treatment liquid after the stirring is finished.
6. The preparation method of the tungsten alloy target material for the electrically-controlled color-changing glass according to claim 5, wherein the wollastonite agent is prepared from wollastonite, ethanol and sodium dodecyl sulfate according to a weight ratio of 3.
7. The method for preparing the tungsten alloy target material for the electrically-controlled color-changing glass according to claim 6, wherein the thermal modification homogenization treatment comprises the following specific operation steps:
s1: heating to 210-220 ℃ at the speed of 1-3 ℃/min, and carrying out heat preservation reaction for 10-20min;
s2: then air-cooling to room temperature, heating to 310-350 ℃ at the speed of 3-5 ℃/min, and keeping the temperature for 25-35min;
s3: and finally, carrying out oil cooling to room temperature by using oil at the temperature of 1-3 ℃, and then washing and drying.
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