CN113353987B - Spinel type ferrite material doped with rare earth element lanthanum or cerium - Google Patents

Spinel type ferrite material doped with rare earth element lanthanum or cerium Download PDF

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CN113353987B
CN113353987B CN202110807143.3A CN202110807143A CN113353987B CN 113353987 B CN113353987 B CN 113353987B CN 202110807143 A CN202110807143 A CN 202110807143A CN 113353987 B CN113353987 B CN 113353987B
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infrared radiation
nitrate
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rare earth
cerium
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CN113353987A (en
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高祥虎
金鹏霞
刘维民
刘刚
何成玉
赵士杰
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C01G49/00—Compounds of iron
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Abstract

The invention relates to a spinel type ferrite material doped with rare earth element lanthanum or cerium, the chemical general formula of the material is ALa x Fe 2‑x O 4 Or ACe x Fe 2‑x O 4 Wherein A is one of Ni, cu, and a mixture of Ni and Cu in any proportion, and x is more than or equal to 0 and less than or equal to 0.50. The invention adopts a one-step hydrothermal method and combines crystallization treatment technology to dope rare earth element lanthanum or cerium into spinel type nickel/copper ferrite structure to form ALa x Fe 2‑x O 4 Or ACe x Fe 2‑x O 4 The spinel type ferrite material has high normal infrared emissivity in a wave band of 3-12 mu m, and can be suitable for the technical field of infrared heating.

Description

Spinel type ferrite material doped with rare earth element lanthanum or cerium
Technical Field
The invention relates to the technical field of new materials, in particular to a spinel type ferrite material doped with rare earth element lanthanum or cerium.
Background
In recent years, with the acceleration of the progress of industrialization, the problem of global energy shortage is becoming more serious. Therefore, it is obviously urgent to explore alternative energy supplies. Infrared radiation is a clean novel energy source, is friendly to natural environment and human health, covers power generation and application, and is the most promising candidate of clean energy sources for promoting sustainable industrial development of the environment. Undoubtedly, the exploration of high infrared radiation materials will provide an efficient and convenient method for energy conservation.
Ferrite materials have great attention in the field of materials, particularly spinel-structured ferrite nanomaterials, because of their characteristics of large coercivity, high saturation magnetization, stable chemical properties, high infrared radiation performance, and the like. Along with the aggravation of energy crisis caused by the combustion of fossil fuel, the infrared radiation material with the photo-thermal conversion function has wide application prospect in the fields of industrial heating, energy conservation, medical treatment, environmental protection and the like.
Infrared radiation has a strong thermal effect, also called thermal radiation, and the wavelength range is 0.75-1000 μm. The application of infrared radiation has the problem of matching absorption, and the wave band of 8-14 μm belongs to the far infrared range, and has wide application in the fields of industrial heating, military, medical treatment and the like, so that the research on the radiation performance of the material in the wave band of 8-14 μm is particularly important. The application of the infrared radiation heating technology has the advantages of saving energy, improving productivity and the like, and the wave band matched with the infrared radiation heating field is just 8-14 mu m, so that the requirement of general industrial heating can be met, and therefore, the material with high infrared emissivity in the wave band is the focus of attention in the current infrared radiation material field. Zhang et al successfully prepared Co by high temperature solid phase synthesis 0.6 Zn 0.4 (RE/Mn) 0.8 Fe 1.2 O 4 (re=la, ce, pr, nd, sm, eu, gd, tb, dy) ferrite, the method inevitably has uneven raw material mixing by mechanical ball milling, and it is difficult to achieve designed molar ratio; meanwhile, the reaction takes a long time. Wu et al prepared a lanthanum doped cobalt ferrite material at a high temperature of 6 using a sol-gel self-propagating combustion methodThe spinel ferrite with good crystallinity can be obtained only by calcining at 00 ℃, and the preparation method also has the defect of long reaction time consumption.
The one-step hydrothermal method is combined with crystallization treatment technology, is a simple means for synthesizing and modifying materials, and has the advantages of short reaction period, no pollution, rapidness, high efficiency and the like. At present, a one-step hydrothermal method and crystallization treatment technology are combined to prepare rare earth element lanthanum or cerium doped spinel type infrared radiation material ALa x Fe 2-x O 4 Or ACe x Fe 2-x O 4 Is not yet retrieved.
Disclosure of Invention
The invention aims to provide a spinel type ferrite material with high red reflectivity and based on rare earth element lanthanum or cerium doping.
In order to solve the problems, the spinel type ferrite material doped with rare earth element lanthanum or cerium is characterized in that: the chemical general formula of the material is ALa x Fe 2-x O 4 Or ACe x Fe 2-x O 4 Wherein A is one of Ni, cu, and a mixture of Ni and Cu in any proportion, and x is more than or equal to 0 and less than or equal to 0.50.
The preparation method of the spinel type ferrite material doped with the rare earth element lanthanum or cerium comprises the following steps:
according to the technical scheme, A, la or Ce and Fe metal nitrate is mixed according to the following ratio of 1: x: weighing the metal element molar ratio of 2-x, placing the weighed metal element molar ratio into a container, adding 8-12 mL of ultrapure water, and stirring until the ultrapure water is completely dissolved to obtain a mixed solution;
adding a precipitant into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=7-13;
filling the precipitate into an autoclave, sealing completely, then placing the autoclave into a heating furnace with the temperature of 100-150 ℃ for heat preservation for 3-5 hours, and then cooling the autoclave to room temperature to obtain a solid product;
fourthly, filtering the solid product under reduced pressure, washing the solid product with ultrapure water until the pH value is 6-8, and filtering, separating and precipitating the solid product and drying the solid product to obtain solid powder;
the solid powder passes throughCrystallizing to obtain target with good crystallinity, namely ALa x Fe 2-x O 4 Or ACe x Fe 2-x O 4 。
The precipitant in the step is one or two of sodium carbonate, sodium hydroxide and ammonia water.
The drying condition in the step is that the temperature is 60-90 ℃ and the time is 5-8 h.
The crystallization treatment condition in the step II means that the temperature is 300-600 ℃, the temperature rising rate is 3-10 degrees/min, the heat preservation time is 2-5 h, and the cooling rate is natural cooling along with the furnace.
Compared with the prior art, the invention has the following advantages:
1. the raw materials are mixed under the liquid phase condition, so that the full and uniform mixing of several metal elements can be ensured, and the product realizes the designed stoichiometric ratio.
2. The invention adopts a one-step hydrothermal method and combines crystallization treatment technology to dope rare earth element lanthanum or cerium into spinel type nickel/copper ferrite structure to form ALa x Fe 2-x O 4 Or ACe x Fe 2-x O 4 The infrared radiation material has the advantages of simple method, short reaction period, mild reaction condition, wide raw material sources, low cost, high efficiency, energy saving and no pollution in the reaction process.
3. The spinel type ferrite material prepared by the invention has high normal infrared emissivity in a wave band of 3-12 mu m, and can be applied to the technical field of infrared heating.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
Fig. 1 is an XRD pattern of lanthanum-doped spinel-type nickel ferrite prepared in example 1 of the present invention.
FIG. 2 is a graph showing the infrared radiation performance of the lanthanum-doped spinel type nickel ferrite prepared in example 1 of the present invention.
FIG. 3 shows a lanthanum-doped spinel-type nickel ferrite (NiLa) prepared in example 1 of the present invention 0.2 Fe 1.8 O 4 ) SEM images of (a).
Fig. 4 is an infrared radiation performance graph of the lanthanum-doped spinel type nickel ferrite prepared in example 2 of the present invention.
Fig. 5 is an infrared radiation performance graph of the lanthanum-doped spinel type nickel ferrite prepared in example 3 of the present invention.
Fig. 6 is an XRD pattern of lanthanum-doped spinel type copper ferrite prepared in example 4 of the present invention.
Fig. 7 is an infrared radiation performance graph of the lanthanum-doped spinel type copper ferrite prepared in example 4 of the present invention.
Fig. 8 is an XRD pattern of lanthanum-doped spinel-type nickel copper ferrite prepared in example 5 of the present invention.
FIG. 9 is a graph showing the infrared radiation performance of the lanthanum-doped spinel-type nickel copper ferrite prepared in example 5 of the present invention.
Fig. 10 is an XRD pattern of cerium-doped spinel-type nickel ferrite prepared in example 6 of the present invention.
FIG. 11 is an infrared radiation performance graph of the cerium-doped spinel type nickel ferrite prepared in example 6 of the present invention.
FIG. 12 shows a cerium-doped spinel-type nickel ferrite (NiCe) prepared in example 6 of the present invention 0.2 Fe 1.8 O 4 ) SEM images of (a).
FIG. 13 is a graph showing the infrared radiation performance of the cerium-doped spinel type nickel ferrite prepared in example 7 of the present invention.
FIG. 14 is an infrared radiation performance graph of cerium doped spinel type nickel ferrite prepared in example 8 of the present invention.
Fig. 15 is an XRD pattern of cerium-doped spinel type copper ferrite prepared in example 9 of the present invention.
FIG. 16 is an infrared radiation performance graph of cerium doped spinel type copper ferrite prepared in example 9 of the present invention.
FIG. 17 is an XRD pattern of cerium-doped spinel-type nickel copper ferrite prepared in example 10 of the present invention.
FIG. 18 is a graph showing the IR radiation performance of the cerium-doped spinel type nickel copper ferrite prepared in example 10 according to the present invention.
Detailed Description
Spinel type ferrite material doped with rare earth element lanthanum or cerium, and the chemical general formula of the material is ALa x Fe 2-x O 4 Or ACe x Fe 2-x O 4 Wherein A is one of Ni, cu, and a mixture of Ni and Cu in any proportion, and x is more than or equal to 0 and less than or equal to 0.50.
The preparation method comprises the following steps:
according to the technical scheme, A, la or Ce and Fe metal nitrate is mixed according to the following ratio of 1: x: the metal element molar ratio of 2-x is weighed and placed in a container, 8-12 mL of ultrapure water is added, and stirring is carried out until the mixture is completely dissolved, so that mixed liquid is obtained.
And adding a precipitant into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitant with pH=7-13. The precipitant is one or two of sodium carbonate, sodium hydroxide and ammonia water.
Placing the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 100-150 ℃ for heat preservation for 3-5 hours, and then cooling to room temperature to obtain a solid product.
And (3) performing reduced pressure filtration on the solid product, washing the solid product with ultrapure water until the pH value is=6-8, performing suction filtration to separate precipitate, and drying at 60-90 ℃ for 5-8 hours to obtain solid powder.
Crystallizing the solid powder to obtain a target object with good crystallinity, namely ALa x Fe 2-x O 4 Or ACe x Fe 2- x O 4 。
Wherein: the crystallization treatment condition means that the temperature is 300-600 ℃, the temperature rising rate is 3-10 DEG/min, the heat preservation time is 2-5 h, and the cooling rate is natural cooling along with the furnace.
Example 1 rare earth element La-based 3+ Doped spinel ferrite material with a chemical composition of NiLa x Fe 2-x O 4 。
1）NiLa x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 10 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 500 ℃ for 4 hours at a temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and the spinel type nickel ferrite (NiFe) doped with rare earth lanthanum with good crystallinity is obtained through the crystallization treatment process 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 2.
2）NiLa x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.216 g lanthanum nitrate and 7.878 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiLa 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.93, is measured by using a direct-reading infrared emissivity tester, as shown in figure 2.
3）NiLa x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.433 g lanthanum nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.1 Fe 1.9 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiLa 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.94, is measured by using a direct-reading infrared emissivity tester, as shown in figure 2.
4）NiLa x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.650 g lanthanum nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.15 Fe 1.85 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiLa 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.94, is measured by using a direct-reading infrared emissivity tester, as shown in figure 2.
5）NiLa x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.866 g lanthanum nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiLa 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.947 is measured by a direct-reading infrared emissivity tester, as shown in figure 2. The microscopic morphology of the infrared radiation material was characterized by using an S-3500N type Scanning Electron Microscope (SEM) of japanese hitachi company, and as shown in fig. 3, it can be seen from the graph that the prepared infrared radiation material has a porous structure, irregular particle size and a slight agglomeration phenomenon.
6）NiLa x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 2.165 g lanthanum nitrate and 6.06 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 1). Taking 0.20. 0.20 g of NiLa 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.943 is measured by a direct-reading infrared emissivity tester, as shown in figure 2.
Example 2 rare earth element La-based 3+ Doped spinel ferrite material with a chemical composition of NiLa x Fe 2-x O 4 。
1）NiLa x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 8 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=7.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave in a heating furnace at 100 ℃ for heat preservation treatment for 3 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultrapure water to ph=6, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 300 ℃ for 2 hours at the temperature rising rate of 3 degrees/min, then is cooled along with the furnace, and the spinel type nickel ferrite (NiFe) doped with rare earth lanthanum with good crystallinity is obtained through the crystallization treatment process 2 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.85 is measured by using a direct-reading infrared emissivity tester, as shown in figure 4.
2）NiLa x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.216 g lanthanum nitrate and 7.878 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.05 Fe 1.95 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87, is measured by using a direct-reading infrared emissivity tester, as shown in figure 4.
3）NiLa x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.433 g lanthanum nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.1 Fe 1.9 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 4.
4）NiLa x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.650 g lanthanum nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.15 Fe 1.85 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 4.
5）NiLa x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.866 g lanthanum nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.2 Fe 1.8 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 4.
6）NiLa x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 2.165 g lanthanum nitrate and 6.06 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.5 Fe 1.5 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87, is measured by using a direct-reading infrared emissivity tester, as shown in figure 4.
Example 3 rare earth element La-based 3+ Doped spinel ferrite material with a chemical composition of NiLa x Fe 2-x O 4 。
1）NiLa x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 12 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=10.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 150 ℃ for heat preservation treatment 5 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=8, the precipitate was isolated by suction filtration and dried at 70 ℃ 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 600 ℃ for 5 hours at the temperature rising rate of 10 degrees/min, then is cooled along with the furnace, and the spinel type nickel ferrite (NiFe) doped with rare earth lanthanum with good crystallinity is obtained through the crystallization treatment process 2 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87, is measured by using a direct-reading infrared emissivity tester, as shown in figure 5.
2）NiLa x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.216 g lanthanum nitrate and 7.878 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.05 Fe 1.95 O 4 ) An infrared radiation material.
Taking 0.20 g of the NiLa 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 5.
3）NiLa x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.433 g lanthanum nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.1 Fe 1.9 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 5.
4）NiLa x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.650 g lanthanum nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.15 Fe 1.85 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 5.
5）NiLa x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 0.866 g lanthanum nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.2 Fe 1.8 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.90 measured by a direct-reading infrared emissivity tester, is shown in figure 5.
6）NiLa x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as that of NiLa except that the raw materials are 2.908 g nickel nitrate, 2.165 g lanthanum nitrate and 6.06 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type nickel ferrite (NiLa) 0.5 Fe 1.5 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiLa 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 5.
Example 4 rare earth element La-based 3+ Doped spinel ferrite material with chemical composition formula of CuLa x Fe 2-x O 4 。
1）CuLa x Fe 2-x O 4 Preparation of (x=0):
placing 2.416 g copper nitrate and 8.080 g ferric nitrate in a container, adding 10 mL ultrapure water, and stirring until the copper nitrate and the 8.080 g ferric nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 500 ℃ for 5 hours at a temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and the spinel type copper ferrite (CuFe) doped with rare earth lanthanum with good crystallinity is obtained through the crystallization treatment process 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 7.
2）CuLa x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as that of CuLa except that the raw materials are 2.416 g copper nitrate, 0.216 g lanthanum nitrate and 7.878 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type copper ferrite (CuLa) with good crystallinity 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuLa 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87, is measured by using a direct-reading infrared emissivity tester, as shown in figure 7.
3）CuLa x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as CuLa except that the raw materials are 2.416 g copper nitrate, 0.433 g lanthanum nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type copper ferrite (CuLa) with good crystallinity 0.1 Fe 1.9 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuLa 0.1 Fe 1.9 O 4 Infrared radiation material, and its normal emissivity is measured by direct-reading infrared emissivity tester0.87 as shown in fig. 7.
4）CuLa x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as CuLa except that the raw materials are 2.416 g copper nitrate, 0.650 g lanthanum nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type copper ferrite (CuLa) with good crystallinity 0.15 Fe 1.85 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuLa 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 7.
5）CuLa x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as CuLa except that the raw materials are 2.416 g copper nitrate, 0.866 g lanthanum nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtaining the rare earth element lanthanum doped spinel type copper ferrite (CuLa) with good crystallinity 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuLa 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.907 measured by using a direct-reading infrared emissivity tester, is shown in figure 7.
6）CuLa x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as that of CuLa except that the raw materials are 2.416 g copper nitrate, 2.165 g lanthanum nitrate and 6.06 g ferric nitrate x Fe 2-x O 4 (x=0). Finally getTo rare earth lanthanum doped spinel type copper ferrite (CuLa) 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 6). Taking 0.20. 0.20 g of the CuLa 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.90, is measured by using a direct-reading infrared emissivity tester, as shown in figure 7.
Example 5 rare earth element La-based 3+ Doped spinel ferrite material having a chemical composition formula of Ni 0.8 Cu 0.2 La x Fe 2-x O 4 。
1）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0):
placing 2.327 g nickel nitrate, 0.483 g copper nitrate and 8.080 g ferric nitrate in a container, adding 10 mL ultrapure water, and stirring until the nickel nitrate, the 0.483 g copper nitrate and the 8.080 g ferric nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is kept for 5 hours in a heat preservation furnace at 500 ℃ through the temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and the spinel nickel-copper ferrite (Ni) doped with rare earth lanthanum with good crystallinity is obtained through the crystallization treatment process 0.8 Cu 0.2 Fe 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by the company Panac, netherlands, and the result showed that the obtained material had spinelAnd the structure and crystal form are good (as shown in fig. 8). Taking 0.20. 0.20 g of Ni prepared in this example 0.8 Cu 0.2 Fe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 9.
2）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.216 g lanthanum nitrate and 7.878 g ferric nitrate 0.8 Cu 0.2 La x Fe 2-x O 4 (x=0). Finally obtaining the spinel type nickel-copper ferrite (Ni) doped with rare earth element lanthanum with good crystallinity 0.8 Cu 0.2 La 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 8). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 La 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.90 is measured by using a direct-reading infrared emissivity tester, as shown in figure 9.
3）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.433 g lanthanum nitrate and 7.676 g ferric nitrate 0.8 Cu 0.2 La x Fe 2-x O 4 (x=0). Finally obtaining the spinel type nickel-copper ferrite (Ni) doped with rare earth element lanthanum with good crystallinity 0.8 Cu 0.2 La 0.1 Fe 1.9 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 8). Take 0.20 gThe Ni is 0.8 Cu 0.2 La 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.903 measured by a direct-reading infrared emissivity tester, is shown in figure 9.
4）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.650 g lanthanum nitrate and 7.474 g ferric nitrate 0.8 Cu 0.2 La x Fe 2-x O 4 (x=0). Finally obtaining the spinel type nickel-copper ferrite (Ni) doped with rare earth element lanthanum with good crystallinity 0.8 Cu 0.2 La 0.15 Fe 1.85 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 8). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 La 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.913 is measured by using a direct-reading infrared emissivity tester, as shown in figure 9.
5）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.866 g lanthanum nitrate and 7.272 g ferric nitrate 0.8 Cu 0.2 La x Fe 2-x O 4 (x=0). Finally obtaining the spinel type nickel-copper ferrite (Ni) doped with rare earth element lanthanum with good crystallinity 0.8 Cu 0.2 La 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 8). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 La 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.907 measured by using a direct-reading infrared emissivity tester, is shown in figure 9.
6）Ni 0.8 Cu 0.2 La x Fe 2-x O 4 Preparation of (x=0.50):
except for the raw materials of 2.327 g nickel nitrate, 0.483 g copper nitrate, 2.179 g lanthanum nitrate and 6.06 g ferric nitrate, the preparation process is the same as Ni 0.8 Cu 0.2 La x Fe 2-x O 4 (x=0). Finally obtaining the spinel type nickel-copper ferrite (Ni) doped with rare earth element lanthanum with good crystallinity 0.8 Cu 0.2 La 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 8). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 La 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 9.
Example 6A rare-earth cerium doped spinel ferrite material having the chemical composition formula NiCe x Fe 2-x O 4 。
1）NiCe x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 10 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 500 ℃ for 4 hours at a temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and spinel type nickel ferrite (NiFe) with good crystallinity is obtained through the treatment process 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 11.
2）NiCe x Fe 2-x O 4 Preparation of (x=0.05):
except for the raw materials of 2.908 g nickel nitrate, 0.217 g cerium nitrate and 7.878 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of the NiCe 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.903 measured by a direct-reading infrared emissivity tester, is shown in figure 11.
3）NiCe x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.435 g cerium nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.1 Fe 1.9 O 4 ) An infrared radiation material.
X manufactured by Panac of NetherlandsThe structure of the infrared radiation material was analyzed by a ray diffractometer, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of the NiCe 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.903 measured by a direct-reading infrared emissivity tester, is shown in figure 11.
4）NiCe x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.652 g cerium nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.15 Fe 1.85 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of the NiCe 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.907 measured by using a direct-reading infrared emissivity tester, is shown in figure 11.
5）NiCe x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.869 g cerium nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of the NiCe 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is greater than or equal to 0.917 measured by a direct-reading infrared emissivity tester, is shown in figure 11.The microscopic morphology of the infrared radiation material was characterized by using an S-3500N type Scanning Electron Microscope (SEM) of japanese hitachi company, and as shown in fig. 12, it can be seen that the prepared infrared radiation material has a porous structure and is slightly agglomerated.
6）NiCe x Fe 2-x O 4 Preparation of (x=0.50):
except for the raw materials of 2.908 g nickel nitrate, 2.171 g cerium nitrate and 6.06 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 10). Taking 0.20. 0.20 g of the NiCe 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.90 is measured by using a direct-reading infrared emissivity tester, as shown in figure 11.
Example 7A rare-earth cerium doped spinel ferrite material having the chemical composition formula NiCe x Fe 2-x O 4 。
1）NiCe x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 8 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=7.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave in a heating furnace at 100 ℃ for heat preservation treatment for 3 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultrapure water to ph=6, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
Solid powder is led to by five timesThe mixture is heated for 2 hours in a heat preservation furnace at 300 ℃ after the temperature rising rate of 3 DEG/min, then is cooled along with the furnace, and spinel type nickel ferrite (NiFe) with good crystallinity is obtained through the treatment process 2 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.83, is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
2）NiCe x Fe 2-x O 4 Preparation of (x=0.05):
except for the raw materials of 2.908 g nickel nitrate, 0.217 g cerium nitrate and 7.878 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.05 Fe 1.95 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.85 is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
3）NiCe x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.435 g cerium nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.1 Fe 1.9 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.86 is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
4）NiCe x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.652 g cerium nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0) middle squareA method of manufacturing the same. Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.15 Fe 1.85 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87, is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
5）NiCe x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.869 g cerium nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.2 Fe 1.8 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
6）NiCe x Fe 2-x O 4 Preparation of (x=0.50):
except for the raw materials of 2.908 g nickel nitrate, 2.171 g cerium nitrate and 6.06 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.5 Fe 1.5 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.86 is measured by using a direct-reading infrared emissivity tester, as shown in figure 13.
Example 8A rare-earth cerium doped spinel ferrite material having the chemical composition formula NiCe x Fe 2-x O 4 。
1）NiCe x Fe 2-x O 4 Preparation of (x=0):
placing 2.908 g nickel nitrate and 8.080 g iron nitrate into a container, adding 12 mL ultrapure water, and stirring until the nickel nitrate and the 8.080 g iron nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=10.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 150 ℃ for heat preservation treatment 5 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=8, the precipitate was isolated by suction filtration and dried at 70 ℃ 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 600 ℃ for 5 hours at the temperature rising rate of 10 degrees/min, then is cooled along with the furnace, and the spinel type nickel ferrite (NiFe) with good crystallinity is obtained through the treatment process 2 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of NiFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.85 is measured by using a direct-reading infrared emissivity tester, as shown in figure 14.
2）NiCe x Fe 2-x O 4 Preparation of (x=0.05):
except for the raw materials of 2.908 g nickel nitrate, 0.217 g cerium nitrate and 7.878 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.05 Fe 1.95 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.86 measured by a direct-reading infrared emissivity tester, is shown in figure 14.
3）NiCe x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.435 g cerium nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally obtain good crystallinityGood rare earth cerium doped spinel nickel ferrite (NiCe 0.1 Fe 1.9 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87 measured by a direct-reading infrared emissivity tester, is shown in figure 14.
4）NiCe x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.652 g cerium nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.15 Fe 1.85 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 14.
5）NiCe x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as NiCe except that the raw materials are 2.908 g nickel nitrate, 0.869 g cerium nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type nickel ferrite (NiCe) doped with rare earth element cerium with good crystallinity is obtained 0.2 Fe 1.8 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 14.
6）NiCe x Fe 2-x O 4 Preparation of (x=0.50):
except for the raw materials of 2.908 g nickel nitrate, 2.171 g cerium nitrate and 6.06 g ferric nitrate, the preparation process is the same as that of NiCe x Fe 2-x O 4 (x=0). Finally obtaining rare earth element cerium doped spinel with good crystallinityStone type nickel ferrite (NiCe) 0.5 Fe 1.5 O 4 ) An infrared radiation material.
Taking 0.20. 0.20 g of the NiCe 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.87 measured by a direct-reading infrared emissivity tester, is shown in figure 14.
Example 9A rare-earth cerium doped spinel ferrite material having the chemical composition formula CuCe x Fe 2-x O 4 。
1）CuCe x Fe 2-x O 4 Preparation of (x=0):
placing 2.416 g copper nitrate and 8.080 g ferric nitrate in a container, adding 10 mL ultrapure water, and stirring until the copper nitrate and the 8.080 g ferric nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is subjected to heat preservation in a heat preservation furnace at 500 ℃ for 5 hours at a temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and spinel type copper ferrite (CuFe) with good crystallinity is obtained through the treatment process 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuFe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 16.
2）CuCe x Fe 2-x O 4 Preparation of (x=0.05):
except that the raw materials are 2.416 g copper nitrate and 0.217 The rest preparation process is the same as CuCe except for the cerium nitrate and the 7.878 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type copper ferrite (CuCe) doped with rare earth element cerium with good crystallinity is obtained 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuCe 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.88, is measured by using a direct-reading infrared emissivity tester, as shown in figure 16.
3）CuCe x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as that of CuCe except that the raw materials are 2.416 g copper nitrate, 0.435 g cerium nitrate and 7.676 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type copper ferrite (CuCe) doped with rare earth element cerium with good crystallinity is obtained 0.1 Fe 1.9 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuCe 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.893 measured by a direct-reading infrared emissivity tester, is shown in figure 16.
4）CuCe x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as that of CuCe except that the raw materials are 2.416 g copper nitrate, 0.652 g cerium nitrate and 7.474 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type copper ferrite (CuCe) doped with rare earth element cerium with good crystallinity is obtained 0.15 Fe 1.85 O 4 ) An infrared radiation material.
Using Panac family of NetherlandsThe structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by company, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuCe 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.893 measured by a direct-reading infrared emissivity tester, is shown in figure 16.
5）CuCe x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as that of CuCe except that the raw materials are 2.416 g copper nitrate, 0.869 g cerium nitrate and 7.272 g ferric nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type copper ferrite (CuCe) doped with rare earth element cerium with good crystallinity is obtained 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuCe 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.903 measured by a direct-reading infrared emissivity tester, is shown in figure 16.
6）CuCe x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as that of CuCe except that the raw materials are 2.416 g copper nitrate, 2.171 g cerium nitrate and 6.06 g iron nitrate x Fe 2-x O 4 (x=0). Finally, the spinel type copper ferrite (CuCe) doped with rare earth element cerium with good crystallinity is obtained 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed using an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 15). Taking 0.20. 0.20 g of the CuCe 0.5 Fe 1.5 O 4 Infrared radiation material with normal emissivity greater than or equal to 0.88 measured by direct-reading infrared emissivity testerFig. 16 shows the same.
Example 10 spinel ferrite Material doped with cerium based rare earth element, the chemical composition formula of which is Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 。
1）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0):
placing 2.327 g nickel nitrate, 0.483 g copper nitrate and 8.080 g ferric nitrate in a container, adding 10 mL ultrapure water, and stirring until the nickel nitrate, the 0.483 g copper nitrate and the 8.080 g ferric nitrate are completely dissolved to obtain a mixed solution.
And (3) adding 30-wt% ammonia water into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=9.
Filling the precipitate into an autoclave, sealing completely, placing the autoclave into a heating furnace at 130 ℃ for heat preservation treatment 4 h, and then cooling to room temperature to obtain a solid product.
The solid product was filtered under reduced pressure and washed with ultra pure water to ph=7, the precipitate was isolated by suction filtration and dried at 70 ℃ for 8 h to give a solid powder.
The solid powder is kept for 5 hours in a heat preservation furnace at 500 ℃ through the temperature rising rate of 5 degrees/min, then is cooled along with the furnace, and spinel type nickel-copper ferrite (Ni) with good crystallinity is obtained through the treatment process 0.8 Cu 0.2 Fe 2 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 Fe 2 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.89 measured by a direct-reading infrared emissivity tester, is shown in figure 18.
2）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0.05):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.217 g cerium nitrate and 7.878 g ferric nitrate 0.8 Cu 0.2 Ce x Fe 2-x O 4 (x=0). Finally, the spinel type nickel-copper ferrite (Ni) doped with rare earth element cerium with good crystallinity is obtained 0.8 Cu 0.2 Ce 0.05 Fe 1.95 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 Ce 0.05 Fe 1.95 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.91 is measured by using a direct-reading infrared emissivity tester, as shown in figure 18.
3）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0.10):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.435 g cerium nitrate and 7.676 g ferric nitrate 0.8 Cu 0.2 Ce x Fe 2-x O 4 (x=0). Finally, the spinel type nickel-copper ferrite (Ni) doped with rare earth element cerium with good crystallinity is obtained 0.8 Cu 0.2 Ce 0.1 Fe 1.9 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 Ce 0.1 Fe 1.9 O 4 The infrared radiation material, the normal emissivity of which is greater than or equal to 0.917 measured by a direct-reading infrared emissivity tester, is shown in figure 18.
4）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0.15):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.652 g cerium nitrate and 7.474 g ferric nitrate 0.8 Cu 0.2 Ce x Fe 2-x O 4 (x=0)The method. Finally, the spinel type nickel-copper ferrite (Ni) doped with rare earth element cerium with good crystallinity is obtained 0.8 Cu 0.2 Ce 0.15 Fe 1.85 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of Ni prepared in this example 0.8 Cu 0.2 Ce 0.15 Fe 1.85 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.923 is measured by using a direct-reading infrared emissivity tester, as shown in figure 18.
5）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0.20):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 0.869 g cerium nitrate and 7.272 g ferric nitrate 0.8 Cu 0.2 Ce x Fe 2-x O 4 (x=0). Finally, the spinel type nickel-copper ferrite (Ni) doped with rare earth element cerium with good crystallinity is obtained 0.8 Cu 0.2 Ce 0.2 Fe 1.8 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 Ce 0.2 Fe 1.8 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.913 measured by a direct-reading infrared emissivity tester, is shown in figure 18.
6）Ni 0.8 Cu 0.2 Ce x Fe 2-x O 4 Preparation of (x=0.50):
the preparation process is the same as Ni except that the raw materials are 2.327 g nickel nitrate, 0.483 g copper nitrate, 2.171 g cerium nitrate and 6.06 g ferric nitrate 0.8 Cu 0.2 Ce x Fe 2-x O 4 (x=0). Finally obtain crystallinityGood rare earth cerium doped spinel nickel copper ferrite (Ni 0.8 Cu 0.2 Ce 0.5 Fe 1.5 O 4 ) An infrared radiation material.
The structure of the infrared radiation material was analyzed by an X-ray diffractometer manufactured by panaceae, netherlands, and the result showed that the obtained material had a spinel structure and a good crystal form (as shown in fig. 17). Taking 0.20. 0.20 g of the Ni 0.8 Cu 0.2 Ce 0.5 Fe 1.5 O 4 The infrared radiation material, the normal emissivity of which is more than or equal to 0.91 is measured by using a direct-reading infrared emissivity tester, as shown in figure 18.

Claims (3)

1. A spinel type ferrite material doped with lanthanum or cerium based on rare earth elements, which is characterized in that: the chemical general formula of the material is CuLa x Fe 2-x O 4 、CuCe x Fe 2-x O 4 、Ni 0.8 Cu 0.2 La x Fe 2-x O 4 One of 0<x is less than or equal to 0.50, and the material has infrared radiation performance in a wave band of 3-12 mu m;
the preparation method comprises the following steps:
according to the technical scheme, A, la or Ce and Fe metal nitrate is mixed according to the following ratio of 1: x: weighing the metal element molar ratio of 2-x, placing the weighed metal element molar ratio into a container, adding 8-12 mL of ultrapure water, and stirring until the ultrapure water is completely dissolved to obtain a mixed solution; a is Cu, ni and Cu according to 0.8:0.2 of a mixture mixed in a proportion;
Adding a precipitant into the mixed solution, and continuously stirring for 1.0-2.0 h to obtain a precipitate with pH=7-13;
filling the precipitate into an autoclave, sealing completely, then placing the autoclave into a heating furnace with the temperature of 100-150 ℃ for heat preservation for 3-5 hours, and then cooling the autoclave to room temperature to obtain a solid product;
fourthly, filtering the solid product under reduced pressure, washing the solid product with ultrapure water until the pH value is 6-8, and filtering, separating and precipitating the solid product and drying the solid product to obtain solid powder;
fifthly, crystallizing the solid powder to obtain a target object with good crystallinity, namely CuLa x Fe 2-x O 4 Or CuCe x Fe 2-x O 4 Or Ni 0.8 Cu 0.2 La x Fe 2-x O 4 The method comprises the steps of carrying out a first treatment on the surface of the The crystallization treatment condition means that the temperature is 300-600 ℃, the temperature rising rate is 3-10 degrees/min, the heat preservation time is 2-5 hours, and the cooling rate is natural cooling along with the furnace.
2. A spinel ferrite material based on rare earth lanthanum or cerium doping as claimed in claim 1, characterized in that: the precipitant in the step is one or two of sodium carbonate, sodium hydroxide and ammonia water.
3. A spinel ferrite material based on rare earth lanthanum or cerium doping as claimed in claim 1, characterized in that: the drying condition in the step is that the temperature is 60-90 ℃ and the time is 5-8 h.
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