CN111204806B - Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof - Google Patents

Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof Download PDF

Info

Publication number
CN111204806B
CN111204806B CN202010031043.1A CN202010031043A CN111204806B CN 111204806 B CN111204806 B CN 111204806B CN 202010031043 A CN202010031043 A CN 202010031043A CN 111204806 B CN111204806 B CN 111204806B
Authority
CN
China
Prior art keywords
aluminum
doped
infrared reflection
solution
stirring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010031043.1A
Other languages
Chinese (zh)
Other versions
CN111204806A (en
Inventor
王玉成
李星星
傅正义
王为民
王皓
张金咏
张帆
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan University of Technology WUT
Original Assignee
Wuhan University of Technology WUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan University of Technology WUT filed Critical Wuhan University of Technology WUT
Priority to CN202010031043.1A priority Critical patent/CN111204806B/en
Publication of CN111204806A publication Critical patent/CN111204806A/en
Application granted granted Critical
Publication of CN111204806B publication Critical patent/CN111204806B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G37/00—Compounds of chromium
    • C01G37/02—Oxides or hydrates thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses aluminum-doped Cr2O3High infrared reflection material and preparation method thereof, the aluminum is doped with Cr2O3The preparation method of the high infrared reflection material comprises the following steps: sequentially dispersing chromium salt and aluminum saltStirring in water to obtain solution A; sequentially dispersing citric acid and ethylene glycol into water, and stirring for reaction to obtain a solution B; dropwise adding the solution B into the solution A, and carrying out heat preservation stirring, heating stirring and heat preservation standing to obtain wet gel; drying, grinding and calcining the wet gel to obtain the aluminum-doped Cr2O3A high infrared reflection material. The mixture obtained by the sol-gel method does not influence the mixing uniformity due to material layering caused by different material precipitation rates in the subsequent standing process; meanwhile, the temperature required in the calcining process is lower; the aluminum doped Cr obtained by the invention2O3The high infrared reflection material is green and has high infrared reflectivity.

Description

Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of inorganic materials, in particular to aluminum-doped Cr2O3High infrared reflection material and its preparation method.
Background
Nowadays, with the development of large-scale urbanization worldwide, more and more plants around buildings are removed and replaced by a high-rise building, and the heat island effect generated by the removal of plants gradually attracts public attention. The heat island effect is a phenomenon that the urban building group is dense due to the fact that the urbanization speed is high, the asphalt road and the cement road absorb heat faster than soil and vegetation in suburbs, and the heat capacity is small, so that the temperature of the urban area is generally higher than the temperature of the suburbs around the urban area at the same time, and the high-temperature urban area is surrounded by the suburbs at low temperature, like an island in the waning sea. The heat island effect enables the temperature around the building to be higher than that of the suburb by more than 10 ℃, so that citizens feel stuffy, and the energy consumption of refrigeration equipment such as an air conditioner and the like can be aggravated.
Generally, the traditional infrared reflective materials are mainly white, such as titanium dioxide, and the like, and the traditional infrared reflective materials have the defect of single color and cannot meet the requirement of people on the diversity of colors of the infrared reflective materials. In the prior art, Cr is added2O3The infrared reflecting materials with different colors can be obtained by doping other metals. The method is characterized in that a solid phase reaction method is generally adopted for doping, and the specific steps of the method are to mix required oxides into a ball milling tank according to different proportions for mixing, but the mixing mode is rough, the materials are not easy to be uniformly mixed, even if the materials are uniformly mixed by a planetary ball mill, in the subsequent standing process of the ball milling tank, various materials in the tank can be layered due to inconsistent precipitation rates, the calcining process of the subsequent mixture is influenced, and the temperature required by calcining is high. Therefore, a new doping method is sought, and the method has important practical significance for improving the mixing uniformity of materials and reducing the calcining temperature.
Disclosure of Invention
The invention aims to overcome the technical defects and provides an aluminum-doped Cr2O3The high infrared reflection material and the preparation method thereof solve the technical problems that the materials are not easy to be uniformly mixed and the calcination temperature is high in the existing doping method in the prior art.
To achieve the above technical object, a first solution of the present invention provides an aluminum-doped Cr2O3The preparation method of the high infrared reflection material comprises the following steps:
sequentially dispersing chromium salt and aluminum salt into water, and stirring to obtain a solution A;
sequentially dispersing citric acid and ethylene glycol into water, and stirring for reaction to obtain a solution B;
dropwise adding the solution B into the solution A, and carrying out heat preservation stirring, heating stirring and heat preservation standing to obtain wet gel;
drying, grinding and calcining the wet gel to obtain the aluminum-doped Cr2O3A high infrared reflection material.
A second solution of the invention provides an aluminum-doped Cr2O3High infrared reflection material, the aluminum being doped with Cr2O3High infrared reflective material is obtained by doping Cr with aluminum as provided in the first solution of the invention2O3The high infrared reflection material is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
the mixture obtained by the sol-gel method does not influence the mixing uniformity due to material layering caused by different material precipitation rates in the subsequent standing process; meanwhile, the temperature required in the calcining process is lower; the aluminum doped Cr obtained by the invention2O3The high infrared reflection material is green and has high infrared reflectivity.
Drawings
FIG. 1 shows the present invention with Cr doped with aluminum2O3A process flow diagram of one embodiment of a method of making a high infrared reflectance material.
FIG. 2 is an XRD pattern of the product obtained in examples 1-2 with the same amount at different temperatures;
FIG. 3 is an XRD pattern of the products obtained in examples 3 to 6 with different doping amounts at the same temperature;
FIG. 4 is a graph of the infrared reflectance of the product obtained in example 1 at a spectral band of 800 to 2500 nm;
FIG. 5 is a graph of the infrared reflectance of the product obtained in example 2 at a spectral band of 800 to 2500 nm;
FIG. 6 is a graph of the infrared reflectance of the product obtained in example 3 at a spectral band of 800 to 2500 nm;
FIG. 7 is a graph of the infrared reflectance of the product obtained in example 4 at a spectral band of 800 to 2500 nm;
FIG. 8 is a graph of the infrared reflectance of the product obtained in example 5 at a spectral band of 800 to 2500 nm;
FIG. 9 is a graph of the infrared reflectance of the product obtained in example 6 at a spectral band of 800 to 2500 nm;
FIG. 10 is an XRD pattern of the products obtained in comparative examples 1 to 3;
FIG. 11 is a graph showing the infrared reflectance of the products obtained in comparative examples 1 to 3 at a spectral band of 800 to 2500 nm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to FIG. 1, FIG. 1 shows the Al-doped Cr provided by the present invention2O3A process flow diagram of one embodiment of a method of making a high infrared reflectance material. For the first solution of the present invention, the present invention provides an aluminum-doped Cr2O3The preparation method of the high infrared reflection material comprises the following steps:
sequentially dispersing chromium salt and aluminum salt into water, and stirring to obtain a solution A;
sequentially dispersing citric acid and ethylene glycol into water, and stirring for reaction to obtain a solution B;
dropwise adding the solution B into the solution A, and carrying out heat preservation stirring, heating stirring and heat preservation standing to obtain wet gel;
drying, grinding and calcining the wet gel to obtain the aluminum-doped Cr2O3A high infrared reflection material.
In the invention, various raw materials are dispersed in water, so that the mixing uniformity of the materials is improved conveniently.
In the invention, the sol-gel method is adopted, compared with the solid phase reaction, the diffusion of each component in the system is in a nanometer range, the chemical reaction is easier to carry out, and only lower synthesis temperature is needed.
In the invention, the uniformly mixed materials are wrapped by using the complex formed by hydrolysis reaction of citric acid and glycol, so that the materials are prevented from being unevenly distributed due to layering in the standing process, and in the subsequent calcining process, the temperature of a reaction system is favorably reduced, solid solution is favorably formed, and the product with high infrared reflectivity is finally obtained.
In the invention, the chromium salt is one or more of chromium nitrate, chromium sulfate and chromium chloride.
In the invention, the aluminum salt is one or more of aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum formate, aluminum acetate and aluminum citrate.
In the present invention, the molar ratio of the aluminum salt to the chromium salt is (3-9): 10, preferably (6-8): 10, and more preferably 7: 10.
In the process of obtaining the solution A, the stirring temperature is 60-70 ℃, and the stirring time is 1.5-2.5 h. In the temperature and time range, the aluminum salt and the chromium salt are more favorably and uniformly dispersed in the system.
In the invention, the molar ratio of citric acid to the total addition of aluminum salt and chromium salt in the solution A is 1 (1-1.2), preferably 1:1.
In the invention, the molar ratio of the citric acid to the ethylene glycol is 1 (1-2), preferably 1: 1.5.
In the process of obtaining the solution B, the stirring reaction temperature is 20-30 ℃, the stirring reaction time is 1.5-2.5 h, and the citric acid and the ethylene glycol are conveniently and fully hydrolyzed.
In the invention, in the process of dropwise adding the solution B into the solution A, the temperature of the solution A is controlled to be 60-70 ℃, and the dropwise adding time is 1-2 min.
In the process of obtaining the wet gel, the temperature for heat preservation and stirring is 60-70 ℃, the time for heat preservation and stirring is 6-7 hours, wherein the process of heat preservation and sol formation is carried out under the stirring condition, so that the raw materials in the solution A and the solution B are fully mixed, and the water is slowly evaporated to form the sol.
In the process of obtaining the wet gel, after the heat preservation and stirring process is finished, the temperature is raised to 75-85 ℃ under the stirring condition, and the wet gel is kept standing for 1.5-2.5 hours, so that the moisture in the sol is continuously evaporated until the gel is formed. Here, in the process of forming a gel by heating, it is sufficient to stand without stirring.
In the invention, the drying temperature is 70-75 ℃, and the drying time is 3-4 days. In the process, if the drying temperature is too low, the drying time is longer, and if the drying temperature is too high, the colloid overflows due to expansion caused by too high temperature. It should be noted that, after the gel is taken out, the drying in the process is determined, whether the gel is still adhered to the bottom of the container is observed, if not, the drying is complete, and if so, the drying is continued.
In the invention, the calcining temperature is 800-900 ℃, the calcining time is 2-6 h, and preferably, the calcining time is 4 h.
Further, the temperature rise rate in the calcining process is 5-10 ℃/min, and preferably 8 ℃/min. Wherein the temperature rise in the calcining process is from room temperature to a target temperature.
In the traditional synthesis process, the aluminum-doped Cr is prepared2O3The calcining temperature of the high infrared reflection material is more than 1000 ℃, and the invention can effectively reduce the reaction temperature in the subsequent calcining process by adopting the sol-gel method to fully mix the raw materials, thereby being beneficial to energy conservation and conforming to the current environmental protection and high efficiency concept.
For the second solution of the present invention, the present invention provides an aluminum-doped Cr2O3High infrared reflection material, the aluminum being doped with Cr2O3High infrared reflective material is obtained by doping Cr with aluminum as provided in the first solution of the invention2O3The high infrared reflection material is prepared by the preparation method.
Example 1
Mixing Cr (NO)3)3·9H2O(23.69g，0.0592mol)、Al(NO3)3·9H2O (6.66g, 0.0177mol) is added into 35ml of deionized water and stirred for 1.5h at the temperature of 60 ℃ to obtain a solution A;
c is to be6H8O7·H2O (16.1963g, 0.0769mol) and ethylene glycol (7.17ml, 0.1155mol) are added into 10ml of deionized water and stirred for 1.5h at normal temperature to obtain solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 7 hours at 60 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, preserving the temperature and standing for 1.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 70 ℃ oven, taking out the wet gel after 4 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to be 800 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 3: 10.
Example 2
Mixing Cr (NO)3)3·9H2O(23.69g，0.0592mol)、Al(NO3)3·9H2O (6.66g, 0.0177mol) is added into 35ml of deionized water and stirred for 1.5h at the temperature of 60 ℃ to obtain a solution A;
c is to be6H8O7·H2O (16.1963g, 0.0769mol) and ethylene glycol (7.17ml, 0.1155mol) are added into 10ml of deionized water and stirred for 1.5h at normal temperature to obtain solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 7 hours at 60 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, preserving the temperature and standing for 1.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 70 ℃ oven, taking out the wet gel after 4 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to 900 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 3: 10.
Example 3
Mixing Cr (NO)3)3·9H2O(21.06g，0.05263mol)、(Al(NO3)3·9H2O) (11.85g, 0.03159mol) was added to 35ml of deionized water and stirred at 60 ℃ for 2.5h to give solution A;
c is to be6H8O7·H2O (17.72g, 0.08422mol), ethylene glycol (7.84ml, 0.1263mol) were added to 10ml of deionized water,stirring for 2.5h at normal temperature to obtain a solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 6 hours at 70 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, and keeping the temperature and standing for 2.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 75 ℃ oven, taking out the wet gel after 3 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to 900 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 6: 10.
Example 4
Mixing Cr (NO)3)3·9H2O(18.43g，0.04605mol)、Al(NO3)3·9H2O (12.09g, 0.03223mol) was added to 35ml of deionized water and stirred at 60 ℃ for 2.5h to give solution A;
c is to be6H8O7·H2O (16.47g, 0.07828mol) and ethylene glycol (7.29mlg, 0.11745mol) are added into 10ml of deionized water and stirred for 2.5 hours at normal temperature to obtain solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 6 hours at 70 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, and keeping the temperature and standing for 2.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 75 ℃ oven, taking out the wet gel after 3 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to 900 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 7: 10.
Example 5
Mixing Cr (NO)3)3·9H2O(18.43g，0.04605mol)、Al(NO3)3·9H2O (13.83g, 0.03686mol) was added to 35ml of deionized water and stirred at 60 ℃ for 2.5h to give solution A;
c is to be6H8O7·H2O (17.444g, 0.08291mol) and ethylene glycol (7.72ml, 0.1244mol) are added into 10ml of deionized water and stirred for 2.5 hours at normal temperature to obtain solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 6 hours at 70 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, and keeping the temperature and standing for 2.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 75 ℃ oven, taking out the wet gel after 3 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to 900 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 8: 10.
Example 6
Mixing Cr (NO)3)3·9H2O(18.43g，0.04605mol)、Al(NO3)3·9H2O (15.55g, 0.04145mol) was added to 35ml of deionized water and stirred at 60 ℃ for 2.5h to give solution A;
18.41gC6H8O7·H2O (18.41g, 0.0875mol) and ethylene glycol (8.15ml, 0.1313mol) are added into 10ml of deionized water and stirred for 2.5h at normal temperature to obtain solution B;
dropwise adding the solution B into the solution A by using a dropper, continuously stirring for 6 hours at 70 ℃ to form sol, then increasing the temperature to 80 ℃ under the stirring condition, and keeping the temperature and standing for 2.5 hours to obtain wet gel;
taking out the wet gel, putting the wet gel into a 75 ℃ oven, taking out the wet gel after 3 days, grinding the wet gel into precursor powder, putting the precursor powder into a muffle furnace with the temperature set to 900 ℃ for calcination, wherein the heating rate is 8 ℃/min, and the heat preservation time is 4h to obtain the aluminum-doped Cr2O3A high infrared reflection material. In this example, the molar ratio of aluminum salt to chromium salt was 9: 10.
Comparative examples 1 to 3
Mixing Cr2O3(25.33g, 0.167mol) and Al2O3(11.89g, 0.117mol) is added into a ball milling tank, and ethanol is used as the solventDispersing medium, and performing wet ball milling; the proportion of the grinding material, the grinding balls and the absolute ethyl alcohol is 1:4:1, the rotation speed of the ball mill is 200r/min, the ball milling time is 6 hours, after the ball milling is finished, the materials are placed into a 70 ℃ constant-temperature drying box to be dried, then the dried powder is uniformly divided into 3 parts which are respectively placed into muffle furnaces with the temperature of 900 ℃, 1000 ℃ and 1100 ℃ to be calcined, the heating rate is 8 ℃/min, the temperature is kept for 4 hours, and the materials are cooled to the room temperature, so that the sample of the comparative examples 1-3 is obtained. In comparative examples 1 to 3, Al2O3And Cr2O3Is 7: 10.
Performance testing
The samples obtained in examples 1 to 6 and comparative examples 1 to 3 were subjected to a performance test. Wherein, XRD is adopted to carry out phase analysis on the sample, and an ultraviolet visible near-infrared spectrophotometer is adopted to carry out infrared reflection performance test on the sample.
As can be seen from FIG. 2, under the same doping amount and at the calcining temperature of 800 ℃ and 900 ℃, respectively, the obtained aluminum is doped with Cr2O3The high infrared reflection material has a different crystalline phase structure. Under the condition that the molar ratio of the aluminum salt to the chromium salt is 3:10 and the calcining temperature is 900 ℃, 1.73Cr is obtained2O3·0.35Al2O3The calcination temperature is 800 ℃ to obtain 1.70Cr2O3·0.30Al2O3. Meanwhile, as can be seen from the combination of fig. 4 and 5, when the calcination temperature is 900 ℃, the obtained aluminum is doped with Cr2O3The infrared reflectivity of the high infrared reflection material is higher than that of the high infrared reflection material when the calcining temperature is 800 ℃.
As can be seen from FIG. 3, the molar ratio of aluminum salt to chromium salt is not uniform at the same calcination temperature, which also results in different crystal phase structures. When the molar ratio of the aluminum salt to the chromium salt is (6-8): 10 under the condition that the calcination temperature is 900 ℃, 3.8Cr is obtained2O3·1.3Al2O3The molar ratio of aluminum salt to chromium salt is 9:10, 2.3Cr is obtained2O3·1.1Al2O3. Meanwhile, as can be seen from fig. 6 to 9, the obtained aluminum-doped Cr is increased with the increase of the molar ratio of the aluminum salt to the chromium salt2O3Infrared reflection of high infrared reflection materialThe refractive index shows the tendency of rising first and then falling, when the molar ratio of the aluminum salt to the chromium salt is increased to 7:10, the obtained aluminum is doped with Cr2O3The infrared reflectivity of the high infrared reflection material is the highest, the reflectivity in each wavelength range of the near infrared band is the lowest 64 percent and the highest 81 percent, and the reflectivity is more than 70 percent in the range exceeding 3/4.
As can be seen from FIG. 10, when the calcination temperature is 900-1100 ℃, the prepared products are all 1Cr2O3·0.7Al2O3(ii) a As can be seen from fig. 11, the ir reflectance of the product obtained by the solid-phase reaction method increases with the increase of the calcination temperature, and when the calcination temperature is increased to 1100 ℃, the ir reflectance of the product is the highest, but the performance of the product provided by the present invention is not yet achieved.
In conclusion, the method of the invention can obtain the aluminum-doped Cr with high infrared reflectivity at lower calcination temperature2O3A high infrared reflection material.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the solution A and the solution B are prepared separately, and the solution B is dripped into the solution A, so that the uniformity of material mixing is improved; the complex formed by the sol-gel method wraps the materials after the materials are uniformly mixed, so that the materials are not layered to influence the mixing uniformity due to different material precipitation rates in the subsequent standing process; meanwhile, compared with a solid phase method, the temperature required in the calcining process of the mixed material obtained by the sol-gel method is lower;
the aluminum doped Cr obtained by the invention2O3The high infrared reflection material can keep green, and simultaneously has higher infrared reflectivity which can reach 81 percent, and the reflectivity of the high infrared reflection material can reach 70 percent within the range of exceeding 3/4.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (8)

1. Aluminum-doped Cr2O3The preparation method of the high infrared reflection material is characterized by comprising the following steps:
sequentially dispersing chromium salt and aluminum salt into water, and stirring to obtain a solution A; the molar ratio of the aluminum salt to the chromium salt is (3-9) to 10;
sequentially dispersing citric acid and ethylene glycol into water, and stirring for reaction to obtain a solution B;
dropwise adding the solution B into the solution A, and carrying out heat preservation stirring, heating stirring and heat preservation standing to obtain wet gel;
drying, grinding and calcining the wet gel to obtain the aluminum-doped Cr2O3A high infrared reflection material; the calcining temperature is 800-900 ℃, and the calcining time is 2-6 h.
2. Aluminum doped Cr according to claim 12O3The preparation method of the high infrared reflection material is characterized in that the chromium salt is one or more of chromium nitrate, chromium sulfate and chromium chloride; the aluminum salt is one or more of aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum formate, aluminum acetate and aluminum citrate.
3. Aluminum doped Cr according to claim 12O3The preparation method of the high infrared reflection material is characterized in that in the process of obtaining the solution A, the stirring temperature is 60-70 ℃, and the stirring time is 1.5-2.5 hours.
4. Aluminum doped Cr according to claim 12O3The preparation method of the high infrared reflection material is characterized in that the molar ratio of the citric acid to the total adding amount of the aluminum salt and the chromium salt in the solution A is 1 (1-1.2), and the molar ratio of the citric acid to the glycol is 1 (1-2).
5. Aluminum doped Cr according to claim 12O3Preparation of high infrared reflection materialThe method is characterized in that in the process of obtaining the solution B, the temperature of the stirring reaction is 20-30 ℃, and the time of the stirring reaction is 1.5-2.5 h.
6. Aluminum doped Cr according to claim 12O3The preparation method of the high infrared reflection material is characterized in that in the process of obtaining the wet gel, the temperature of heat preservation stirring is 60-70 ℃, and the time of heat preservation stirring is 6-7 hours.
7. Aluminum doped Cr according to claim 12O3The preparation method of the high infrared reflection material is characterized in that in the process of obtaining the wet gel, after the heat preservation and stirring process is finished, the temperature is raised to 75-85 ℃ under the stirring condition, and the wet gel is kept standing for 1.5-2.5 hours.
8. Aluminum-doped Cr2O3The high infrared reflection material is characterized in that the aluminum is doped with Cr2O3The high infrared reflection material is prepared by the aluminum-doped Cr of any one of claims 1 to 72O3The high infrared reflection material is prepared by the preparation method.
CN202010031043.1A 2020-01-13 2020-01-13 Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof Active CN111204806B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010031043.1A CN111204806B (en) 2020-01-13 2020-01-13 Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010031043.1A CN111204806B (en) 2020-01-13 2020-01-13 Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111204806A CN111204806A (en) 2020-05-29
CN111204806B true CN111204806B (en) 2021-03-23

Family

ID=70780624

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010031043.1A Active CN111204806B (en) 2020-01-13 2020-01-13 Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111204806B (en)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6174360B1 (en) * 1998-10-26 2001-01-16 Ferro Corporation Infrared reflective color pigment
CN104445409B (en) * 2013-09-12 2018-02-02 中国科学院过程工程研究所 A kind of method that the chromic oxide-based pigment of near-infrared high reflection is prepared by hydrated chromium oxide
CN108101531B (en) * 2017-12-15 2020-09-22 华南理工大学 Composite spinel material with high infrared emissivity and preparation method thereof

Also Published As

Publication number Publication date
CN111204806A (en) 2020-05-29

Similar Documents

Publication Publication Date Title
Thongkanluang et al. Preparation of NIR reflective brown pigment
CN105175012A (en) Spinel type composite ultrafine blue ceramic pigment and preparation method thereof
CN105755800B (en) A kind of heat-reflective coating cloth
Li et al. Synthesis and characterization of yellow pigments (Li0. 4RE0. 6Al0. 6) 1/2MoO4–BiVO4 with high NIR reflectance
CN110066529B (en) Double-doped calcium aluminate type near-infrared reflection pigment and preparation method thereof
CN105086560A (en) Thermal reflectivity, imitation stone effect coating system
CN103332869A (en) Method for preparing multifunctional composite ZnO/In coating glass
CN111204806B (en) Aluminum-doped Cr2O3High infrared reflection material and preparation method thereof
Zhang et al. Nanoporous Mg-doped SiO2 nanoparticles with tunable infrared emissivity toward effective radiative cooling coatings
CN102329533A (en) Composite tin antimony oxide thermal insulation material and preparation method thereof
CN111394069B (en) Silicon dioxide coated magnesium phosphite radiation refrigeration material and preparation method thereof
CN105668625B (en) A kind of vanadium dioxide nano particle coated by nano aluminium oxide and preparation method thereof
CN110878179A (en) Black heat-reflective pigment and preparation method and application thereof
CN102976626A (en) Method of using sol-gel to prepare MgF2 antireflection film
CN105000911B (en) Preparation method of purple ceramic pigment with cobalt-silicon olivine structure
CN109133170B (en) Amorphous zinc oxide coated vanadium dioxide nano powder and preparation method thereof
CN112266649B (en) Cyan material and preparation method thereof, near-infrared high-reflection blue coating and preparation method thereof
CN115340331A (en) Preparation method of heat reflection cement-based material
CN112441623B (en) Preparation of high near-infrared reflection color pigment by using modified cobalt blue pigment
CN112048193B (en) Green pigment with low lightness and high near-infrared reflectivity and preparation method thereof
CN114644837B (en) High near infrared reflection rare earth colorful pigment and preparation method and application thereof
CN107286776B (en) Infrared-reflection heat-insulation coating and preparation method thereof based on cerium dopping compound
CN105482506A (en) Vanadium-doped calcium zirconate inorganic pigment and preparing method thereof
CN115594227B (en) Inorganic yellow high-entropy pigment with high near infrared reflection performance and preparation method thereof
Rus et al. Near-infrared reflective coatings based on Ca1-xNdxAl12-xNixO19 blue pigments, prepared by solution combustion synthesis

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant