CN112501560A - Preparation method of high-heat-reflectivity black coating - Google Patents
Preparation method of high-heat-reflectivity black coating Download PDFInfo
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- CN112501560A CN112501560A CN202011272187.2A CN202011272187A CN112501560A CN 112501560 A CN112501560 A CN 112501560A CN 202011272187 A CN202011272187 A CN 202011272187A CN 112501560 A CN112501560 A CN 112501560A
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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
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- Physical Vapour Deposition (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a preparation method of a black coating with high heat reflectivity, which uses SnO2、Sb2O3And NH4And (2) Cl is used as a raw material, the raw materials with a certain molar ratio are put into a ball mill for ball milling and mixing to obtain raw material powder for evaporation, then the base material to be plated and the evaporation raw material powder are placed in a closed cavity for roasting, and a black tin antimony oxide heat-insulating coating with high reflectivity can be formed on the surface of the base material due to the decomposition of ammonium chloride and the sublimation characteristic of tin chloride. The invention can form compact black tin antimony oxide heat insulation coating on the surface of high temperature resistant base materials such as ceramics or corundum, etc., has convenient operation and simple process, and the prepared coating has dark and uniform color, strong reflection heat insulation performance and high acid and alkali resistance performance.
Description
Technical Field
The invention belongs to the field of preparation and application of heat-insulating coating materials, and particularly relates to a method for preparing a black heat-insulating coating with high heat reflectivity by high-temperature evaporation.
Technical Field
In recent years, antimony-doped tin oxide nano materials are widely researched and rapidly developed due to the integration of excellent performances such as electrical performance, optical performance, corrosion resistance, chemical stability and radiation resistance, and are widely applied to the fields of energy-saving glass, antistatic plastics, chemical fiber materials, heat-insulating coatings, photoelectric display devices, transparent electrode materials and the like. The antimony doped tin oxide nanometer is blue gray in the convention, the color of the powder can be changed between light blue and dark gray by changing the antimony doping amount, in addition, in the coating material, the white or bright colors (colors) are more generally used, the heat reflectivity of the colors is higher, the black generally has no reflectivity so as to absorb more, the pure black coating with high reflectivity is rare, and the reflectivity of the conventional black coating with reflectivity generally does not exceed 20%. On the other hand, black is a relatively common color in life, and people are seriously worried about the heat absorption property of black in summer, so that a black coating with high heat reflectivity has high application value.
SnO2Is an N-type semiconductor material, has the characteristics of high activity, easily controllable performance, flexible and various preparation methods and the like, and surrounds SnO2Research into new reflective insulation materials as matrix materials has also attracted interest to numerous scholars.
High-temperature evaporation refers to a process method in which a coating material (or called a coating material) is evaporated and gasified in a certain heating and evaporation manner under a high-temperature condition, and particles fly to the surface of a substrate to condense and form a film. The vapor deposition is a vapor deposition technology which is used earlier and has wider application, and has the advantages of simple film forming method, high film purity and compactness, unique film structure and performance and the like. The physical process of evaporation comprises the following steps: the deposition material is evaporated or sublimated into gaseous particles → the gaseous particles are rapidly transported from the evaporation source to the surface of the substrate → the gaseous particles are attached to the surface of the substrate to form nuclei, grow into a solid film → the atoms of the film are reconstructed or generate chemical bonding.
Disclosure of Invention
The invention aims to provide a preparation method of a high-heat-reflectivity black coating.
The preparation method of the black coating with high heat reflectivity comprises the following steps: in SnO2、Sb2O3And NH4And (2) taking Cl as a raw material, putting the raw material with a certain molar ratio into a ball mill for ball milling, drying and sieving a ball milling product to obtain raw material powder for evaporation, and roasting the base material to be plated and the evaporation raw material powder in a closed cavity to obtain the black heat-insulation coating with high reflectivity.
Specifically, NH in the vapor deposition raw material powder4Cl、SnO2And Sb2O3The molar ratio data of (A) to (B) are respectively 10, (9-10) and (1-3), wherein Sb is2O3Is NH4Cl and SnO26.5-10.1 wt% of the total mass. SnO2And Sb2O3The molar ratio of (A) is 9 to 10. NH (NH)4Cl and SnO2The molar ratio of (A) to (B) is 0.8 to 1.3.
Specifically, the ball milling and mixing time is 2-8 hours. The roasting evaporation temperature is 600-900 ℃, and the roasting time is 2-8 hours.
Specifically, the semi-closed cavity is a muffle furnace cavity or other resistance furnaces with similar structures.
Specifically, the ball mill is a planetary ball mill, a stirring ball mill or a vibration ball mill.
Specifically, the material of the ball milling tank is stainless steel, agate, corundum, polytetrafluoroethylene or nylon, and the material of the grinding ball is yttrium zirconium oxide, stainless steel, agate or corundum.
Specifically, the plating base material is ceramic, corundum, or a material with a smooth surface and high temperature resistance.
The invention realizes the preparation of the black coating with high heat reflectivity by forming the tin antimony oxide coating on the surface of the base material based on the thermal decomposition of ammonium chloride and the sublimation characteristic of tin chloride. The method has the advantages of convenient operation, simple process, environmental protection, and uniform and dark color of the prepared surface coating, acid and alkali resistance, and can form compactness on the surface of high-temperature resistant base materials such as ceramics or corundum. The invention selects NH4Cl is used as a sublimation medium of the coating material and can also be used as a diluent in the roasting process to form air holesAnd the structure reduces hard agglomeration in the roasting process. .
Drawings
FIG. 1 is a graph showing the light reflectance of a coating obtained in example 1 of the present invention, and the coating has a high reflectance in the near infrared band.
FIG. 2 is a schematic view of a coating obtained in example 1 of the present invention, wherein the coating is uniformly dark black as shown in the figure. The detection experiment shows that the hardness is high, the adhesiveness is good, and the acid resistance and the alkali resistance are good.
FIG. 3 is a scanning electron microscope image of the coating obtained in example 1 of the present invention, in which the particle size on the surface of the coating is uniform.
FIG. 4 is an XRD diffraction pattern of the coating obtained in example 1 of the present invention, wherein the XRD characteristic peak and JCPDS SnO with a number of 4114452And (5) performing anastomosis.
Detailed Description
The invention will be further illustrated by the following examples.
Example 1
Set Sb2O3The mol percentage of the powder in the coating is 5 percent, and the mol ratio of the raw materials of the powder in the coating is NH according to the proportion4Cl:SnO2:Sb2O3Sb in the coating powder is 10:10:12O3/(NH4Cl+SnO2) And the mass ratio of the ball materials is 8:1 in the ball milling and mixing process, the raw materials are mixed and put into a planetary ball mill for ball milling and mixing, the rotating speed of the ball mill is 720rpm, the ball milling time is 3 hours, the coating powder is prepared by ball milling and mixing, and the coating powder is dried at low temperature and then screened. Roasting the high-temperature resistant coating base material such as ceramic or corundum and the like and the coating powder in a muffle furnace at 600 ℃ for 3 hours to obtain NH4Decomposing and sublimating Cl and stannic chloride at high temperature to obtain SnO2/Sb2O3Evaporating to the surface of the base material, then cooling in a furnace, washing the cooled plating material, washing off surface impurities, and drying at normal temperature to obtain a finished product. The finished product is subjected to heat reflection and ratio analysis, the result is shown in figure 1, the structure of a coating scanning electron microscope is shown in figure 3, and the result of coating XRD diffraction analysis is shown in figure 4. The finished product has gray black color and relatively flat surface,has slight frosting feeling, high reflectivity in far infrared and good heat-insulating property.
Example 2
Set Sb2O3The mol percentage of the powder in the coating is 6 percent, and the mol ratio of the raw materials of the powder in the coating is NH according to the proportion4Cl:SnO2:Sb2O3Sb in the coating powder is 10:9:22O3/(NH4Cl+SnO2) And the mass ratio of the ball materials is 8:1 in the ball milling and mixing process, the raw materials are mixed and then put into a planetary ball mill for ball milling and mixing, the rotating speed of the ball mill is 720rpm, the ball milling and mixing time is 3 hours, the coating powder is prepared by ball milling and mixing, and the coating powder is dried at low temperature and then screened. Roasting the high-temperature resistant coating base material such as ceramic or corundum and the like and the coating powder in a muffle furnace at 700 ℃ for 3 hours to obtain NH4Decomposing and sublimating Cl and stannic chloride at high temperature to obtain SnO2/Sb2O3Evaporating the mixture on the surface of a base material, then cooling the mixture in a furnace, washing the cooled coating material, washing away surface impurities, and drying the coating material at normal temperature to obtain a finished product, wherein the finished product is black in color, flat in surface, free of frosted feeling, high in reflectivity of middle and far infrared rays, and excellent in heat insulation performance.
Example 3
Set Sb2O3The mol percentage of the powder in the coating is 7 percent, and the mol ratio of the raw materials of the powder in the coating is NH according to the proportion4Cl:SnO2:Sb2O3Sb in the coating powder (10: 9: 3)2O3/(NH4Cl+SnO2) And the mass ratio of the ball materials is 8:1 in the ball milling and mixing process, the raw materials are mixed and then put into a planetary ball mill for ball milling and mixing, the rotating speed of the ball mill is 720rpm, the ball milling and mixing time is 3 hours, the coating powder is prepared by ball milling and mixing, and the coating powder is dried at low temperature and then screened. Roasting the high-temperature resistant coating base material such as ceramic or corundum and the like and the coating powder in a muffle furnace at 800 ℃ for 3 hours to obtain NH4Decomposing and sublimating Cl and stannic chloride at high temperature to obtain SnO2/Sb2O3Evaporating the coating on the surface of the substrate, cooling in a furnace, and depositing the cooled coatingThe material is washed, surface impurities are washed, and the material is dried at normal temperature to obtain a finished product, wherein the finished product is dark black in color, very flat in surface, free of frosted feeling, high in reflectivity of middle and far infrared rays, excellent in heat insulation performance, and capable of keeping high adhesiveness and hardness under the action of external force.
Example 4
Set Sb2O3The mol percentage of the powder in the coating is 8 percent, and the mol ratio of the raw materials of the powder in the coating is NH according to the proportion4Cl:SnO2:Sb2O3Sb in the coating powder (10: 9: 3)2O3/(NH4Cl+SnO2) The coating powder is prepared by mixing the raw materials, putting the mixture into a planetary ball mill for ball milling and mixing at the rotating speed of 720rpm for 3 hours, carrying out ball milling and mixing to obtain the coating powder, drying the coating powder at low temperature, and sieving. Calcining high-temperature resistant coating base material such as ceramic or corundum and the like and coating powder in a muffle furnace at 900 ℃ for 3 hours to obtain NH4Decomposing and sublimating Cl and stannic chloride at high temperature to obtain SnO2/Sb2O3Evaporating to the surface of a substrate, then cooling in a furnace, washing the cooled coating material, washing off surface impurities, and drying at normal temperature to obtain a finished product, wherein the finished product has uniform surface color, strong adhesiveness, water resistance, acid and alkali resistance, and is a stable surface coating.
The semi-closed cavity in the implementation of the invention is a muffle furnace cavity, and other reaction containers meeting the requirements can also be adopted.
The ball mill in the implementation of the invention is one of a planetary ball mill, a stirring ball mill or a vibration ball mill.
The ball milling tank in the implementation of the invention can select a stainless steel, agate, corundum, polytetrafluoroethylene or nylon ball milling tank, and the grinding balls are yttrium zirconium oxide grinding balls, stainless steel, agate or corundum grinding balls.
The base material coated in the invention can be ceramic, corundum or material with smooth surface and high temperature resistance.
The above examples are only some embodiments of the present invention, and those skilled in the art can make routine changes based on the present invention, and also fall into the protection scope of the present invention.
Claims (10)
1. A preparation method of a black coating with high heat reflectivity is characterized by comprising the following steps: in SnO2、Sb2O3And NH4And (2) taking Cl as a raw material, putting the raw material with a certain molar ratio into a ball mill for ball milling, drying and sieving a ball milling product to obtain raw material powder for evaporation, and roasting the base material to be plated and the evaporation raw material powder in a closed cavity to obtain the black heat-insulation coating with high reflectivity.
2. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: NH in vapor deposition raw material powder4Cl、SnO2And Sb2O3The molar ratio data of (A) to (B) are respectively 10, (9-10) and (1-3), wherein Sb is2O3Is NH4Cl and SnO26.5-10.1 wt% of the total mass.
3. A method of producing a high heat reflectance black coating according to claim 1, wherein: SnO2And Sb2O3The molar ratio of (A) is 9 to 10.
4. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: NH (NH)4Cl and SnO2The molar ratio of (A) to (B) is 0.8 to 1.3.
5. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the ball milling and mixing time is 2-8 hours.
6. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the roasting evaporation temperature is 600-900 ℃, and the roasting time is 2-8 hours.
7. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the semi-closed cavity is a muffle furnace cavity or other resistance furnaces.
8. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the ball mill is a planetary ball mill, a stirring ball mill or a vibration ball mill.
9. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the material of the ball milling tank is stainless steel, agate, corundum, polytetrafluoroethylene or nylon, and the material of the grinding ball is yttrium zirconium grinding ball, stainless steel, agate or corundum.
10. The method of claim 1, wherein the black coating with high thermal reflectivity comprises: the plating base material is ceramic, corundum or a material with smooth surface and high temperature resistance.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06316439A (en) * | 1993-04-30 | 1994-11-15 | Sumitomo Cement Co Ltd | Heat ray shielding glass plate and production thereof |
| JP2008230954A (en) * | 2007-02-21 | 2008-10-02 | Sumitomo Metal Mining Co Ltd | Manufacturing method for antimony-containing tin oxide fine particles for forming solar radiation shielding body, dispersion for forming solar radiation shielding body, solar radiation shielding body, and solar radiation shielding base material |
| JP2010059040A (en) * | 2008-08-07 | 2010-03-18 | Idemitsu Kosan Co Ltd | Method for producing microparticle and heat-ray-shielding microparticle obtained thereby |
| CN104148050A (en) * | 2014-07-23 | 2014-11-19 | 陕西科技大学 | Preparation method for Sb2O3/SnO2 composite photocatalytic material |
| CN107880672A (en) * | 2017-11-20 | 2018-04-06 | 广东华兹卜新材料科技有限公司 | A kind of high IR shielding rate insulating moulding coating and preparation method thereof |
| CN110451816A (en) * | 2019-09-03 | 2019-11-15 | 天津工业大学 | A kind of preparation method of antimony-doped tin oxide infrared reflection films |
-
2020
- 2020-11-13 CN CN202011272187.2A patent/CN112501560B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06316439A (en) * | 1993-04-30 | 1994-11-15 | Sumitomo Cement Co Ltd | Heat ray shielding glass plate and production thereof |
| JP2008230954A (en) * | 2007-02-21 | 2008-10-02 | Sumitomo Metal Mining Co Ltd | Manufacturing method for antimony-containing tin oxide fine particles for forming solar radiation shielding body, dispersion for forming solar radiation shielding body, solar radiation shielding body, and solar radiation shielding base material |
| JP2010059040A (en) * | 2008-08-07 | 2010-03-18 | Idemitsu Kosan Co Ltd | Method for producing microparticle and heat-ray-shielding microparticle obtained thereby |
| CN104148050A (en) * | 2014-07-23 | 2014-11-19 | 陕西科技大学 | Preparation method for Sb2O3/SnO2 composite photocatalytic material |
| CN107880672A (en) * | 2017-11-20 | 2018-04-06 | 广东华兹卜新材料科技有限公司 | A kind of high IR shielding rate insulating moulding coating and preparation method thereof |
| CN110451816A (en) * | 2019-09-03 | 2019-11-15 | 天津工业大学 | A kind of preparation method of antimony-doped tin oxide infrared reflection films |
Non-Patent Citations (1)
| Title |
|---|
| P.BILLIK 等: "Synthesis of nanocrystalline SnO2 powder from SnCl4 by mechanochemical processing", 《POWDER TECHNOLOGY》 * |
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