CN110980813B - High near-infrared reflectivity yttrium ferrite powder and preparation method thereof - Google Patents

High near-infrared reflectivity yttrium ferrite powder and preparation method thereof Download PDF

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CN110980813B
CN110980813B CN201911400124.8A CN201911400124A CN110980813B CN 110980813 B CN110980813 B CN 110980813B CN 201911400124 A CN201911400124 A CN 201911400124A CN 110980813 B CN110980813 B CN 110980813B
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yttrium
ferrite powder
grinding
citric acid
high near
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CN110980813A (en
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马妍
李悦影
王周福
刘浩
王玺堂
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/0018Mixed oxides or hydroxides
    • C01G49/0054Mixed oxides or hydroxides containing one rare earth metal, yttrium or scandium

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Abstract

The invention relates to yttrium ferrite powder with high near-infrared reflectivity and a preparation method thereof. The technical scheme is as follows: mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate to glycol of 1: 1 to (2-8) to obtain a mixture. And grinding the mixture at room temperature for 30-120 min, and drying at 100-110 ℃ to obtain the yttrium ferrite precursor. Grinding the yttrium ferrite precursor for 10-15 min to obtain a grinding material, putting the grinding material into a corundum crucible, then putting the corundum crucible into a muffle furnace, heating to 800-1000 ℃ at the speed of 3-5 ℃/min, preserving heat for 3-5 h, and cooling with the furnace to obtain the high near-infrared reflectivity yttrium ferrite powder. The method has the characteristics of simple process, low equipment requirement, short production period and suitability for industrial production, and the prepared product has high near-infrared reflectivity.

Description

High near-infrared reflectivity yttrium ferrite powder and preparation method thereof
Technical Field
The invention belongs to the technical field of yttrium ferrite powder. In particular to yttrium ferrite powder with high near-infrared reflectivity and a preparation method thereof.
Background
Under the high temperature condition of over 900 ℃, the heat transfer mechanism mainly takes radiation heat transfer as the main mechanism. The heat radiation under high temperature conditions is mainly concentrated in the infrared short wave region. Therefore, the powder with good near-infrared reflection performance can be applied to heat-insulating and heat-preserving paint and used as functional filler, and the heat-insulating and heat-preserving paint is applied to the surface of the lining of the high-temperature hearth, and has considerable prospect.
The yttrium ferrite has ferroelectricity and weak ferromagnetism at the same time, and can be used in a multi-state memory as a multiferroic material. The weak ferromagnetism and the special magneto-optical effect enable the material to have wide application prospect in the fields of magneto-optical switches, magneto-optical sensors and the like. In addition, the yttrium ferrite has higher melting point and better high temperature resistance, and can also be used in the technical fields of photocatalysis, fuel cells, gas sensors and the like.
At present, the method for preparing yttrium ferrite powder comprises the following steps: the patent technology of the microwave preparation method of the yttrium ferrite nano powder (CN102173459A) is characterized in that although the yttrium ferrite nano powder is prepared under the microwave condition, the requirement on equipment is higher; the patent of "a preparation method of yttrium ferrite powder" (CN105540677A) is a technology, the technology uses urea, citric acid monohydrate, ethylene diamine tetraacetic acid or hydrazine as reducing agent, the combustion synthesis reaction is carried out at the controlled temperature of 200-800 ℃ to prepare yttrium ferrite powder, the technology needs to dissolve the raw materials in deionized water to prepare solution, and then carry out subsequent reaction, the technology is comparatively complicated, the production cycle is long.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing high-near-infrared-reflectance yttrium ferrite powder, which has the advantages of simple process, low requirement on equipment, short production period and suitability for industrial production.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate to ferric nitrate nonahydrate to citric acid monohydrate to glycol of 1: 1 to (2-8) to obtain a mixture.
And secondly, grinding the mixture for 30-120 min at room temperature, and drying for 2-12 h at 100-110 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 10-15 min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 800-1000 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 3-5 h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
The purity of the yttrium nitrate hexahydrate is more than or equal to 99 percent; the grain size of the yttrium nitrate hexahydrate is less than or equal to 74 mu m.
The purity of the ferric nitrate nonahydrate is more than or equal to 99 percent; the particle size of the ferric nitrate nonahydrate is less than or equal to 74 mu m.
The purity of the citric acid monohydrate is more than or equal to 99 percent; the particle size of the citric acid monohydrate is less than or equal to 74 mu m.
The purity of the ethylene glycol is more than or equal to 99 percent.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
the invention adopts a low-temperature solid phase method, and the sintering is carried out by keeping the temperature at 800-1000 ℃ for 3-5 h, so that the sintering temperature required by the reaction can be obviously reduced, the sintering time is shortened, and the production period is short.
The yttrium ferrite powder with high near-infrared reflectivity is prepared by mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol, grinding, drying and calcining, and the process is simple; and has no special requirements for equipment, and is suitable for industrial production.
The phase composition of the high near infrared reflectivity yttrium ferrite powder prepared by the invention is basically a single orthogonal phase, the near infrared reflectivity can reach 80%, and the prepared high near infrared reflectivity yttrium ferrite powder has high near infrared reflectivity.
Therefore, the method has the characteristics of simple process, low equipment requirement, short production period and suitability for industrial production, and the prepared yttrium ferrite powder with high near-infrared reflectivity has high near-infrared reflectivity.
Drawings
FIG. 1 is an X-ray diffraction diagram of a high near-infrared reflectance yttrium ferrite powder prepared by the invention;
FIG. 2 is a diagram showing the near-infrared reflectance of the high-near-infrared-reflectance yttrium ferrite powder shown in FIG. 1.
Detailed Description
The invention will be further described with reference to the following drawings and detailed description, without limiting its scope:
a high near-infrared reflectivity yttrium ferrite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate to ferric nitrate nonahydrate to citric acid monohydrate to glycol of 1: 1 to (2-8) to obtain a mixture.
And secondly, grinding the mixture for 30-120 min at room temperature, and drying for 2-12 h at 100-110 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 10-15 min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 800-1000 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 3-5 h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
In this embodiment: the purity of the yttrium nitrate hexahydrate is more than or equal to 99 percent, and the particle size of the yttrium nitrate hexahydrate is less than or equal to 74 microns; the purity of the ferric nitrate nonahydrate is more than or equal to 99 percent, and the grain size of the ferric nitrate nonahydrate is less than or equal to 74 mu m; the purity of the citric acid monohydrate is more than or equal to 99 percent, and the particle size of the citric acid monohydrate is less than or equal to 74 mu m; the purity of the ethylene glycol is more than or equal to 99 percent. The details in the embodiments are not repeated.
Example 1
A high near-infrared reflectivity yttrium ferrite powder and a preparation method thereof. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol of 1: 2 to obtain a mixture.
And secondly, grinding the mixture for 30min at room temperature, and drying for 12h at 100 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 11min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 900 ℃ at the speed of 4 ℃/min, preserving the temperature for 4h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
Example 2
A high near-infrared reflectivity yttrium ferrite powder and a preparation method thereof. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol of 1: 4: 3 to obtain a mixture.
And secondly, grinding the mixture for 60min at room temperature, and drying for 2h at 110 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 13min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 850 ℃ at the speed of 3 ℃/min, preserving heat for 3h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
Example 3
A high near-infrared reflectivity yttrium ferrite powder and a preparation method thereof. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol of 1: 6: 5 to obtain a mixture.
And secondly, grinding the mixture for 90min at room temperature, and drying for 8h at 100 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 10min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 1000 ℃ at the speed of 5 ℃/min, preserving the temperature for 5h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
Example 4
A high near-infrared reflectivity yttrium ferrite powder and a preparation method thereof. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol of 1: 8 to obtain a mixture.
And secondly, grinding the mixture for 120min at room temperature, and drying for 4h at 110 ℃ to obtain the yttrium ferrite precursor.
And thirdly, grinding the yttrium ferrite precursor for 15min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 800 ℃ at the speed of 3 ℃/min, preserving the temperature for 3h, cooling along with the furnace, and discharging to obtain the high near-infrared reflectivity yttrium ferrite powder.
Compared with the prior art, the specific implementation mode has the following positive effects:
the method adopts a low-temperature solid phase method, and the sintering is carried out by keeping the temperature at 800-1000 ℃ for 3-5 h, so that the calcining temperature required by the reaction can be obviously reduced, the energy consumption is low, the calcining time is shortened, and the production period is short.
The yttrium ferrite powder with high near-infrared reflectivity is prepared by mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol, grinding, drying and calcining, and the process is simple; and no special requirements are required for equipment, the production process is green and environment-friendly, and the method is suitable for industrial production.
The high near-infrared reflectance yttrium ferrite powder prepared by the embodiment is shown in the attached drawing, and fig. 1 is an X-ray diffraction diagram of the high near-infrared reflectance yttrium ferrite powder prepared in example 1; FIG. 2 is a graph showing the near infrared reflectance of the high near infrared reflectance yttrium ferrite powder shown in FIG. 1. As can be seen from fig. 1, the crystal forms are all orthogonal phases. As can be seen from FIG. 2, the maximum value of the near infrared reflectivity of the prepared high near infrared reflectivity yttrium ferrite powder can reach 82%. The prepared yttrium ferrite powder with high near-infrared reflectivity has high near-infrared reflectivity and high purity.
Therefore, the specific implementation mode has the characteristics of simple process, low equipment requirement, short production period and suitability for large-scale production, and the prepared high-near-infrared-reflectance yttrium ferrite powder has high near-infrared reflectance and high purity.

Claims (3)

1. A preparation method of yttrium ferrite powder with high near-infrared reflectivity is characterized by comprising the following steps:
firstly, mixing yttrium nitrate hexahydrate, ferric nitrate nonahydrate, citric acid monohydrate and glycol according to the mass ratio of yttrium nitrate hexahydrate to ferric nitrate nonahydrate to citric acid monohydrate to glycol of 1: 1 to (2-8) to obtain a mixture;
secondly, grinding the mixture at room temperature for 30-120 min, and drying at 100-110 ℃ for 2-12 h to obtain a yttrium ferrite precursor;
thirdly, grinding the yttrium ferrite precursor for 10-15 min to obtain a grinding material, putting the grinding material into a corundum crucible, putting the corundum crucible into a muffle furnace, heating to 800-1000 ℃ at the speed of 3-5 ℃/min, preserving the temperature for 3-5 h, and cooling along with the furnace to obtain high near-infrared reflectivity yttrium ferrite powder;
the purity of the yttrium nitrate hexahydrate is more than or equal to 99 percent, and the particle size of the yttrium nitrate hexahydrate is less than or equal to 74 microns;
the purity of the ferric nitrate nonahydrate is more than or equal to 99 percent, and the grain size of the ferric nitrate nonahydrate is less than or equal to 74 mu m;
the purity of the citric acid monohydrate is more than or equal to 99 percent, and the grain diameter of the citric acid monohydrate is less than or equal to 74 mu m.
2. The method for preparing yttrium ferrite powder with high near-infrared reflectivity according to claim 1, wherein the purity of the ethylene glycol is not less than 99%.
3. The high-near-infrared-reflectivity yttrium ferrite powder is characterized by being prepared according to the preparation method of the high-near-infrared-reflectivity yttrium ferrite powder in any one of claims 1-2.
CN201911400124.8A 2019-12-30 2019-12-30 High near-infrared reflectivity yttrium ferrite powder and preparation method thereof Active CN110980813B (en)

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US4265980A (en) * 1977-12-30 1981-05-05 Bell Telephone Laboratories, Incorporated Technique for the growth of magnetic garnet compositions
CN104804737A (en) * 2015-04-27 2015-07-29 重庆文理学院 Synthetic method of Gd2O3:Dy<3+> nanoparticles
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CN105294095A (en) * 2015-10-22 2016-02-03 上海应用技术学院 Preparation method for yttrium ferrite tape casting biscuit film
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