CN114262874B - Target material for building glass and preparation method thereof - Google Patents
Target material for building glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a target material for building glass, which comprises the following raw materials in parts by weight: 1-5 parts of Sn, 1-2 parts of In, 1-3 parts of Sb, 1-3 parts of Ga, 5-10 parts of Ni powder and 30-40 parts of silicon powder; the target material also comprises 0.5-1.5 parts of refining agent and 0.1-0.5 part of strengthening agent; smelting: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted; step two, adding a refining agent into the smelted raw materials, stirring for 10-30min at a rotating speed of 100-500r/min, and then adding a reinforcing agent. The invention relates to a target material for building glass, which is prepared by main metal elements such as Sn, in, sb, ga and the like; the building glass obtained by the target coating has excellent performances of corrosion resistance, mechanical scratch resistance, high-temperature oxidation resistance and the like.
Description
Technical Field
The invention relates to the technical field of building glass, in particular to a target material for building glass and a preparation method thereof.
Background
The building glass is mainly flat glass, and has the advantages of crystal and clear surface, light transmission, sound insulation, heat preservation, wear resistance, weather resistance, stable material quality and the like. The high-temperature heat-resistant ceramic material is prepared from quartz sand, sandstone or quartz rock, limestone, feldspar, dolomite, sodium carbonate and the like serving as main raw materials through the procedures of crushing, screening, proportioning, high-temperature melting, forming, annealing, cooling, processing and the like. The magnetron sputtering film plating is a new physical vapor film plating mode, that is, electron gun system is used to emit and focus electrons onto the material to be plated, so that sputtered atoms are separated from the material with high kinetic energy to fly toward the substrate to deposit film by following the momentum conversion principle. This plated material is called a sputter target. The sputtering target material is metal, alloy, ceramic compound, etc.
The existing glass target material is simple in raw materials, common in preparation process, and poor in corrosion resistance, scratch resistance, high-temperature oxidation resistance and the like, and needs further improvement treatment based on the prepared target material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a target material for building glass and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a target material for building glass, which comprises the following raw materials in parts by weight:
1-5 parts of Sn, 1-2 parts of In, 1-3 parts of Sb, 1-3 parts of Ga, 5-10 parts of Ni powder and 30-40 parts of silicon powder; the target material also comprises 0.5-1.5 parts of refining agent and 0.1-0.5 part of reinforcing agent.
Preferably, the target material for the building glass comprises the following raw materials in parts by weight:
3 parts of Sn, 1.5 parts of In, 2 parts of Sb, 2 parts of Ga, 7.5 parts of Ni powder and 35 parts of silicon powder; the target material also comprises 1.0 part of refining agent and 0.3 part of reinforcing agent.
Preferably, the preparation method of the refining agent comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1000-1500r/min, and the ball milling time is 20-30min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 10-20min, the hot pressing temperature is 800-1000 ℃, after hot pressing, the mixture is crushed to 10-20 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 1-5 meshes;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 15-25min at 200-300 ℃, and then heating is carried out at 1-3 ℃/min to 400 ℃ and heat preservation is carried out for 10-20min;
then annealing to 150-190 ℃, continuing to keep the temperature for 20-30min, and finally cooling to room temperature at a speed of 1 ℃/min.
Preferably, the preparation method of the enhancer comprises the following steps:
mixing rare earth yttrium and bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 10-30% for low-speed stirring, wherein the stirring speed is 100-500r/min, the stirring time is 20-30min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 1-9 meshes, and the reinforcing agent is obtained after the granulation is finished.
Preferably, the specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 1-3 times, heating to 70-90deg.C, and calcining at 300-500deg.C for 35-45min;
s2: cooling calcined bentonite to 80-90 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 100-300r/min, and the stirring time is 10-20min;
s3: then washing with water, drying, cooling at 1-5deg.C for 15-25min, cold rolling at 0-10deg.C for 15-25min with cold rolling deformation rate of 10-20% to obtain bentonite improver.
Preferably, the modifier is hydrochloric acid, and the mass fraction is 5-15%.
Preferably, the mass fraction of the hydrochloric acid is 10%.
The invention also provides a preparation method of the target material for the building glass, which comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 10-30min at a rotating speed of 100-500r/min, then adding a reinforcing agent, continuously stirring for 20-30min at a rotating speed of 1000-1500r/min, and pouring into a mould for cooling and forming;
thirdly, preheating at 100-200 ℃ for 10-20min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 420-500 ℃, preserving heat for 10-20min, then continuously heating to 550 ℃, continuously preserving heat for 5-10min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 150-160 ℃, then sending into a tempering furnace for tempering to 560 ℃, preserving heat for 15-25min, and finally annealing to room temperature at a speed of 1-4 ℃/min;
step five, homogenizing, and maintaining at 65-75 ℃ for 25-35min to obtain the target material; in the preparation of the target material, the performance of the product is further improved through preheating treatment, heat improvement treatment and homogenization treatment, the alloy product is preheated to a certain temperature by the purpose of preheating treatment, unstable grains caused by overlarge temperature change in the heat improvement treatment are avoided, meanwhile, the grains of the product are modified through heat improvement, the grain refinement of the product and the connectivity among the products are improved, and finally, the performance of the product is improved through homogenization treatment, and the performance integrity of the prepared product is improved in a coordinated manner.
Preferably, the water cooling in the quenching treatment is from 300 ℃ to 220-240 ℃ and then combined with air cooling to 150-160 ℃.
Preferably, the specific operation steps of the homogenization treatment are as follows:
heat treating the product at 160-180deg.C for 15-25min, heating to 260-270 deg.C at a rate of 1deg.C/min, maintaining for 15-25min, heating to 350deg.C at a rate of 2deg.C/min, and maintaining for 5-10min;
then cooling to 120-150 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 15-25min, and finally cooling to room temperature at a speed of 3 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the invention relates to a target material for building glass, which is prepared by main metal elements such as Sn, in, sb, ga and the like; the building glass obtained by the target coating has excellent performances of corrosion resistance, mechanical scratch resistance, high-temperature oxidation resistance and the like;
in the preparation of the product, the refining agent is added, so that the crystal grains of the product can be refined, the density of the product structure is improved, meanwhile, the added strengthening agent adopts the rare earth agent and the modified bentonite, the activity of the rare earth agent is high, the interlayer spacing of the modified bentonite is small, the activity is strong, and the rare earth agent and the modified bentonite are matched, so that the corrosion resistance and other performances of the product can be enhanced;
in the preparation of the target material, the performance of the product is further improved through preheating treatment, heat improvement treatment and homogenization treatment, the alloy product is preheated to a certain temperature by the purpose of preheating treatment, unstable grains caused by overlarge temperature change in the heat improvement treatment are avoided, meanwhile, the grains of the product are modified by the heat improvement, the grain refinement of the product and the connectivity among the products are improved, and finally, the performance of the product is improved by the homogenization treatment, and the performance comprehensive performance of the prepared product is improved in a coordinated manner.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The target for the building glass comprises the following raw materials in parts by weight:
1-5 parts of Sn, 1-2 parts of In, 1-3 parts of Sb, 1-3 parts of Ga, 5-10 parts of Ni powder and 30-40 parts of silicon powder; the target material also comprises 0.5-1.5 parts of refining agent and 0.1-0.5 part of reinforcing agent.
The target material for the building glass comprises the following raw materials in parts by weight:
3 parts of Sn, 1.5 parts of In, 2 parts of Sb, 2 parts of Ga, 7.5 parts of Ni powder and 35 parts of silicon powder; the target material also comprises 1.0 part of refining agent and 0.3 part of reinforcing agent.
The preparation method of the refining agent of the embodiment comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1000-1500r/min, and the ball milling time is 20-30min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 10-20min, the hot pressing temperature is 800-1000 ℃, after hot pressing, the mixture is crushed to 10-20 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 1-5 meshes;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 15-25min at 200-300 ℃, and then heating is carried out at 1-3 ℃/min to 400 ℃ and heat preservation is carried out for 10-20min;
then annealing to 150-190 ℃, continuing to keep the temperature for 20-30min, and finally cooling to room temperature at a speed of 1 ℃/min.
The preparation method of the reinforcing agent of the embodiment comprises the following steps:
mixing rare earth yttrium and bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 10-30% for low-speed stirring, wherein the stirring speed is 100-500r/min, the stirring time is 20-30min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 1-9 meshes, and the reinforcing agent is obtained after the granulation is finished.
The specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 1-3 times, heating to 70-90deg.C, and calcining at 300-500deg.C for 35-45min;
s2: cooling calcined bentonite to 80-90 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 100-300r/min, and the stirring time is 10-20min;
s3: then washing with water, drying, cooling at 1-5deg.C for 15-25min, cold rolling at 0-10deg.C for 15-25min with cold rolling deformation rate of 10-20% to obtain bentonite improver.
The refining agent is added, so that the product crystal grain can be refined, the density of the product structure is improved, meanwhile, the added strengthening agent adopts rare earth agent and modified bentonite, the activity of the rare earth agent is high, the interlayer spacing of the modified bentonite is small, the activity is strong, and the rare earth agent and the modified bentonite are matched, so that the corrosion resistance and other performances of the product can be enhanced;
the modifier of the embodiment is hydrochloric acid, and the mass fraction is 5-15%.
The mass fraction of hydrochloric acid in this example was 10%.
The preparation method of the target material for the building glass comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 10-30min at a rotating speed of 100-500r/min, then adding a reinforcing agent, continuously stirring for 20-30min at a rotating speed of 1000-1500r/min, and pouring into a mould for cooling and forming;
thirdly, preheating at 100-200 ℃ for 10-20min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 420-500 ℃, preserving heat for 10-20min, then continuously heating to 550 ℃, continuously preserving heat for 5-10min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 150-160 ℃, then sending into a tempering furnace for tempering to 560 ℃, preserving heat for 15-25min, and finally annealing to room temperature at a speed of 1-4 ℃/min;
and fifthly, homogenizing, and maintaining at 65-75 ℃ for 25-35min to obtain the target material.
In the quenching treatment of this embodiment, water cooling is performed from 300 ℃ to 220-240 ℃ and then air cooling is combined to 150-160 ℃.
The specific operation steps of the homogenization treatment in this embodiment are:
heat treating the product at 160-180deg.C for 15-25min, heating to 260-270 deg.C at a rate of 1deg.C/min, maintaining for 15-25min, heating to 350deg.C at a rate of 2deg.C/min, and maintaining for 5-10min;
then cooling to 120-150 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 15-25min, and finally cooling to room temperature at a speed of 3 ℃/min.
Example 1.
The target for the building glass comprises the following raw materials in parts by weight:
1 part of Sn, 1 part of In, 1 part of Sb, 1 part of Ga, 5 parts of Ni powder and 30 parts of silicon powder; the target material also comprises 0.5 part of refining agent and 0.1 part of reinforcing agent.
The preparation method of the refining agent of the embodiment comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1000r/min, and the ball milling time is 20min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 10min, the hot pressing temperature is 800 ℃, the mixture is crushed and passes through 10 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 1 mesh;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 15min at 200 ℃, and then heating is carried out at 1 ℃/min to 400 ℃ and heat preservation is carried out for 10min;
and then annealing to 150 ℃, continuing to keep the temperature for 20min, and finally cooling to room temperature at a speed of 1 ℃/min.
The preparation method of the reinforcing agent of the embodiment comprises the following steps:
mixing rare earth yttrium with bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 10% for low-speed stirring, wherein the stirring speed is 100r/min, the stirring time is 20min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 1 mesh, and the reinforcement is obtained after the granulation is finished.
The specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 1 time, heating to 70deg.C, and calcining at 300deg.C for 35min;
s2: cooling calcined bentonite to 80 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 100r/min, and the stirring time is 10min;
s3: then washing with water, drying, cooling at 1 ℃ for 15min, and then cold-rolling at 0 ℃ for 15min, wherein the cold-rolling deformation rate is 10%, thus obtaining the bentonite improver.
The modifier of the embodiment is hydrochloric acid, and the mass fraction is 5%.
The preparation method of the target material for the building glass comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 10min at a rotating speed of 100r/min, then adding a reinforcing agent, continuously stirring for 20min at a rotating speed of 1000r/min, and pouring into a mould for cooling and molding after the stirring is finished;
thirdly, preheating at 100 ℃ for 10min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 420 ℃, preserving heat for 10min, then continuously heating to 550 ℃, continuously preserving heat for 5min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 150 ℃, then sending into a tempering furnace to temper to 560 ℃, preserving heat for 15min, and finally annealing to room temperature at a rate of 1 ℃/min;
and fifthly, homogenizing, and maintaining at 65 ℃ for 25min to obtain the target material.
The water cooling in the quenching treatment of this example was from 300 ℃ to 220 ℃ and then combined with air cooling to 150 ℃.
The specific operation steps of the homogenization treatment in this embodiment are:
heat-treating the product at 160deg.C for 15min, heating to 260deg.C at rate of 1deg.C/min, maintaining for 15min, heating to 350deg.C at rate of 2deg.C/min, and maintaining for 5-10min;
then cooling to 120 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 15min, and finally cooling to room temperature at a speed of 3 ℃/min.
Example 2.
The target for the building glass comprises the following raw materials in parts by weight:
5 parts of Sn, 2 parts of In, 3 parts of Sb, 3 parts of Ga, 10 parts of Ni powder and 40 parts of silicon powder; the target material also comprises 1.5 parts of refining agent and 0.5 part of reinforcing agent.
The preparation method of the refining agent of the embodiment comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1500r/min, and the ball milling time is 30min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 20min, the hot pressing temperature is 1000 ℃, the mixture is crushed and passes through 20 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 5 meshes;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 25min at 300 ℃, and then heating is carried out for 20min at 3 ℃/min to 400 ℃;
and then annealing to 190 ℃, continuing to keep the temperature for 30min, and finally cooling to room temperature at a speed of 1 ℃/min.
The preparation method of the reinforcing agent of the embodiment comprises the following steps:
mixing rare earth yttrium with bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 30% for low-speed stirring, wherein the stirring speed is 500r/min, the stirring time is 30min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 9 meshes, and the reinforcing agent is obtained after the granulation is finished.
The specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 3 times, heating to 90deg.C, and calcining at 500deg.C for 45min;
s2: cooling calcined bentonite to 90 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 300r/min, and the stirring time is 20min;
s3: then washing with water, drying, cooling at 5 ℃ for 25min, and then cold-rolling at 10 ℃ for 25min, wherein the cold-rolling deformation rate is 20%, thus obtaining the bentonite improver.
The modifier of the embodiment is hydrochloric acid, and the mass fraction is 15%.
The preparation method of the target material for the building glass comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 30min at a rotation speed of 500r/min, then adding a reinforcing agent, continuously stirring for 30min at a rotation speed of 1500r/min, and pouring into a mould for cooling and molding after the stirring is finished;
thirdly, preheating at 200 ℃ for 20min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 500 ℃, preserving heat for 20min, then continuously heating to 550 ℃, continuously preserving heat for 10min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 160 ℃, then sending into a tempering furnace to temper to 560 ℃, preserving heat for 25min, and finally annealing to room temperature at a rate of 4 ℃/min;
step five, homogenizing, and maintaining at 75 ℃ for 35min, wherein the maintenance is finished to obtain the target material; in the preparation of the target material, the performance of the product is further improved through preheating treatment, heat improvement treatment and homogenization treatment, the alloy product is preheated to a certain temperature by the purpose of preheating treatment, unstable grains caused by overlarge temperature change in the heat improvement treatment are avoided, meanwhile, the grains of the product are modified through heat improvement, the grain refinement of the product and the connectivity among the products are improved, and finally, the performance of the product is improved through homogenization treatment, and the performance integrity of the prepared product is improved in a coordinated manner.
The water cooling in the quenching treatment of this example was from 300 ℃ to 240 ℃ and then combined with air cooling to 160 ℃.
The specific operation steps of the homogenization treatment in this embodiment are:
heat-treating the product at 180deg.C for 25min, heating to 280deg.C at a rate of 1deg.C/min, maintaining the temperature for 25min, heating to 350deg.C at a rate of 2deg.C/min, and maintaining the temperature for 10min;
then cooling to 150 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 25min, and finally cooling to room temperature at a speed of 3 ℃/min.
Example 3.
The target for the building glass comprises the following raw materials in parts by weight:
3 parts of Sn, 1.5 parts of In, 2 parts of Sb, 2 parts of Ga, 7.5 parts of Ni powder and 35 parts of silicon powder; the target material also comprises 1.0 part of refining agent and 0.3 part of reinforcing agent.
The preparation method of the refining agent of the embodiment comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1250r/min, and the ball milling time is 25min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 15min, the hot pressing temperature is 900 ℃, the mixture is crushed and passes through 15 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 1-5 meshes;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 20min at 250 ℃, and then heating is carried out at 2 ℃/min to 400 ℃ and heat preservation is carried out for 15min;
and then annealing to 170 ℃, continuing to keep the temperature for 25min, and finally cooling to room temperature at a speed of 1 ℃/min.
The preparation method of the reinforcing agent of the embodiment comprises the following steps:
mixing rare earth yttrium with bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 20% for low-speed stirring, wherein the stirring speed is 300r/min, the stirring time is 25min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 5 meshes, and the reinforcing agent is obtained after the granulation is finished.
The specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 2 times, heating to 80deg.C, and calcining at 400deg.C for 40min;
s2: cooling calcined bentonite to 85 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 200r/min, and the stirring time is 15min;
s3: then washing with water, drying, cooling at 3 ℃ for 20min, and then cold-rolling at 5 ℃ for 20min, wherein the cold-rolling deformation rate is 15%, thus obtaining the bentonite improver.
The modifier of this embodiment is hydrochloric acid, and the mass fraction of hydrochloric acid is 10%.
The preparation method of the target material for the building glass comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 20min at a rotating speed of 300r/min, then adding a reinforcing agent, continuously stirring for 25min at a rotating speed of 1250r/min, and pouring into a mould for cooling and molding after the stirring is finished;
thirdly, preheating at 150 ℃ for 15min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 55 ℃, preserving heat for 15min, then continuously heating to 550 ℃, continuously preserving heat for 7.5min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 155 ℃, then sending into a tempering furnace to temper to 560 ℃, preserving heat for 20min, and finally annealing to room temperature at a rate of 2.5 ℃/min;
and fifthly, homogenizing, and maintaining at 70 ℃ for 30min to obtain the target material.
The water cooling in the quenching treatment of this example was from 300 ℃ to 230 ℃ and then combined with air cooling to 155 ℃.
The specific operation steps of the homogenization treatment in this embodiment are:
heat-treating the product at 170deg.C for 20min, heating to 265deg.C at a rate of 1deg.C/min, maintaining the temperature for 20min, heating to 350deg.C at a rate of 2deg.C/min, and maintaining the temperature for 7.5min;
then cooling to 135 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 20min, and finally cooling to room temperature at a speed of 3 ℃/min.
Comparative example 1.
The difference from example 3 is that no bentonite modifier is added to the strengthening agent.
Comparative example 2.
Unlike example 3, no refining agent was added to prepare the alloy sputtering target.
Comparative example 3.
The difference from example 3 is that the quenching treatment was not performed by combining water cooling and air cooling in the heat improvement treatment.
Comparative example 4.
The difference from example 3 is that the homogenization treatment is carried out by a conventional constant temperature heat treatment at 170℃for 20min.
Comparative example 5.
The difference from example 3 is that no preheating treatment was performed.
Experimental example 1, corrosion resistance test:
the test uses a Prlington 273A electrochemical workstation to perform corrosion resistance tests on the performances of examples 1-3 and comparative examples 1-3, a conventional three-electrode system is adopted in the test, a tested sample, platinum and calomel are respectively used as a working electrode, an auxiliary electrode and a reference electrode, a corrosion solution used in the corrosion test is a 3.5% NaCl solution, the test area is 0.785cm, the scanning rate is 0.5mV/s, and the self-corrosion potential and the self-corrosion current density are obtained.
From examples 1-3 and comparative examples 1-5, it can be seen that the bentonite modifier and the refining agent have a certain influence on the corrosion resistance of the product in the preparation of the product, and the treatment conditions in the preparation method of the target material have an influence on the product performance.
Experimental example 2 scratch resistance test:
carrying out scratch resistance test on the product, adopting a workpiece to scratch back and forth on the surface of the product, and observing whether scratches exist and metallic luster leaks;
experimental example 3, high temperature oxidation experiment:
carrying out a high-temperature oxidation experiment on the product at 1000 ℃, weighing the product in 0h, 5h, 10h, 24h and 175h by adopting a resistance furnace in the experiment, and then calculating the oxidation weight gain rate;
as can be seen from comparative examples 1 to 5 of example 3, the product of example 3 of the present invention has excellent high-temperature oxidation resistance.
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 characteristics 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 disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (4)
1. The target for the building glass is characterized by comprising the following raw materials in parts by weight:
1-5 parts of Sn, 1-2 parts of In, 1-3 parts of Sb, 1-3 parts of Ga, 5-10 parts of Ni powder and 30-40 parts of silicon powder; the target material also comprises 0.5-1.5 parts of refining agent and 0.1-0.5 part of strengthening agent;
the preparation method of the refining agent comprises the following steps:
s1: mixing SiN, liCl and light calcium carbonate according to a weight ratio of 3:2:1, and then adding the mixture into a ball mill for ball milling, wherein the ball milling speed is 1000-1500r/min, and the ball milling time is 20-30min;
s2: then the mixture is sent into a hot press for hot pressing treatment, the hot pressing pressure is 10-20min, the hot pressing temperature is 800-1000 ℃, after hot pressing, the mixture is crushed to 10-20 meshes, and then the mixture is sent into a granulator for granulation, and the particle size is 1-5 meshes;
s3: carrying out heat treatment on the granulated product;
the specific heat treatment method comprises the following steps:
heat treatment is carried out for 15-25min at 200-300 ℃, and then heating is carried out at 1-3 ℃/min to 400 ℃ and heat preservation is carried out for 10-20min;
then annealing to 150-190 ℃, continuing to keep the temperature for 20-30min, and finally cooling to room temperature at a speed of 1 ℃/min; the preparation method of the reinforcing agent comprises the following steps:
mixing rare earth yttrium and bentonite modifier according to a weight ratio of 3:1, then sending into a sodium dodecyl sulfate solution with a mass fraction of 10-30% for low-speed stirring, wherein the stirring speed is 100-500r/min, the stirring time is 20-30min, and then washing and drying;
then the mixture is sent into a granulator for granulation, the particle size of the granulation is 1-9 meshes, and the reinforcement agent is obtained after the granulation is finished; the specific preparation method of the bentonite improver comprises the following steps:
s1: repeatedly washing bentonite with hot water for 1-3 times, heating to 70-90deg.C, and calcining at 300-500deg.C for 35-45min;
s2: cooling calcined bentonite to 80-90 ℃, and sending the calcined bentonite into a modifier for stirring treatment, wherein the stirring speed is 100-300r/min, and the stirring time is 10-20min;
s3: then washing with water, drying, cooling at 1-5deg.C for 15-25min, cold rolling at 0-10deg.C for 15-25min with cold rolling deformation rate of 10-20% to obtain bentonite improver; the modifier is hydrochloric acid, and the mass fraction is 5-15%;
the preparation method of the target material for the building glass comprises the following steps:
step one, smelting treatment: sn, in, sb, ga, ni powder and silicon powder are fed into a smelting furnace for smelting treatment until the raw materials are completely melted;
adding a refining agent into the smelted raw materials, stirring for 10-30min at a rotating speed of 100-500r/min, then adding a reinforcing agent, continuously stirring for 20-30min at a rotating speed of 1000-1500r/min, and pouring into a mould for cooling and forming;
thirdly, preheating at 100-200 ℃ for 10-20min, heating to 280 ℃ at a speed of 1 ℃/min, and preserving heat;
step four, heat improvement treatment: heating the product obtained in the third step to 420-500 ℃, preserving heat for 10-20min, then continuously heating to 550 ℃, continuously preserving heat for 5-10min, and then air-cooling to 300 ℃;
then carrying out quenching treatment by combining water cooling and air cooling, quenching to 150-160 ℃, then sending into a tempering furnace for tempering to 560 ℃, preserving heat for 15-25min, and finally annealing to room temperature at a speed of 1-4 ℃/min;
step five, homogenizing, and maintaining at 65-75 ℃ for 25-35min to obtain a target; the specific operation steps of the homogenization treatment are as follows:
heat treating the product at 160-180deg.C for 15-25min, heating to 260-270 deg.C at a rate of 1deg.C/min, maintaining for 15-25min, heating to 350deg.C at a rate of 2deg.C/min, and maintaining for 5-10min;
then cooling to 120-150 ℃ at a speed of 1 ℃/min, continuing to keep the temperature for 15-25min, and finally cooling to room temperature at a speed of 3 ℃/min.
2. The target for the architectural glass according to claim 1, wherein the target for the architectural glass comprises the following raw materials in parts by weight:
3 parts of Sn, 1.5 parts of In, 2 parts of Sb, 2 parts of Ga, 7.5 parts of Ni powder and 35 parts of silicon powder; the target material also comprises 1.0 part of refining agent and 0.3 part of reinforcing agent.
3. The target material for building glass according to claim 1, wherein the mass fraction of the hydrochloric acid is 10%.
4. The target for architectural glass according to claim 1, wherein the quenching process is water-cooled from 300 ℃ to 220-240 ℃ and then combined with air-cooled quenching to 150-160 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2009074127A (en) * | 2007-09-20 | 2009-04-09 | Kojundo Chem Lab Co Ltd | Sintered sputtering target material and manufacturing method therefor |
| CN110129759A (en) * | 2019-06-27 | 2019-08-16 | 江阴恩特莱特镀膜科技有限公司 | A kind of sial zirconium target and preparation method thereof for Low-E glass |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009074127A (en) * | 2007-09-20 | 2009-04-09 | Kojundo Chem Lab Co Ltd | Sintered sputtering target material and manufacturing method therefor |
| CN110129759A (en) * | 2019-06-27 | 2019-08-16 | 江阴恩特莱特镀膜科技有限公司 | A kind of sial zirconium target and preparation method thereof for Low-E glass |
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