CN117430430A - Preparation method of uranium dioxide-carbon composite phase porous material - Google Patents
Preparation method of uranium dioxide-carbon composite phase porous material Download PDFInfo
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Abstract
A preparation method of uranium dioxide-carbon composite phase porous material comprises the following steps: 1) Preparing resorcinol-formaldehyde sol; 2) The resorcinol-formaldehyde sol is preserved in a constant temperature sealing way and is dried in air to prepare resorcinol-formaldehyde aerogel; 3) Carrying out high-temperature treatment on resorcinol-formaldehyde aerogel in an argon atmosphere to obtain a porous carbon material; 4) Preparing uranium oxide precursor solution; 5) Soaking a porous carbon material in uranium oxide precursor solution, then drying in air, and circulating for multiple times to obtain a porous material blank; 6) And (3) carrying out high-temperature treatment on the porous material blank in a low-pressure environment to obtain the uranium dioxide-carbon complex phase porous material. The preparation process is simple, and expensive equipment is not needed. The uranium dioxide-carbon composite phase porous material has high phase purity and good structural stability, and the density, specific surface area, conductivity and the like of the material can be regulated and controlled in a larger range according to design requirements, so that the application of the material in the fields of catalysis, thermoelectricity and the like can be satisfied.
Description
Technical Field
The invention belongs to the technical field of porous ceramic material preparation, and particularly relates to a preparation method of a uranium dioxide-carbon composite porous material.
Background
Uranium dioxide is an important nuclear material and has found wide application as a reactor fuel. In recent years, uranium dioxide is paid attention to as a thermoelectric material, the seebeck coefficient of the uranium dioxide is obviously higher than that of the conventional thermoelectric material at room temperature, meanwhile, the uranium dioxide is a p-type intrinsic material, the forbidden band width of the uranium dioxide is close to the peak of a solar energy absorption band gap-efficiency curve, the uranium dioxide is a high-efficiency solar cell material, and the uranium dioxide also has excellent anti-radiation performance and has application potential in a high-energy radiation environment as an electronic device. In addition, the potential application of uranium dioxide in the fields of optical materials, catalysis and the like is also receiving a great deal of attention.
However, uranium dioxide is not widely used in other fields than as a nuclear fuel element. The reason for this is on the one hand that the uranium dioxide material properties are to be improved further. For example, in the thermoelectric field, the thermoelectric performance is the result of the combined action of the seebeck coefficient, the thermal conductivity and the electrical conductivity of the material, and the extremely low electrical conductivity of uranium dioxide causes the thermoelectric figure of merit of the material to be unobtrusive although the uranium dioxide has a higher seebeck coefficient; in the field of catalysis, the high specific surface area of the catalyst is beneficial to the catalytic activity of the catalyst, and meanwhile, the material also needs to have certain structural strength, so that the environmental problem caused by the running loss of the catalyst in the use process is avoided. On the other hand, the preparation method of uranium dioxide materials is limited, the preparation, molding and performance evaluation of the uranium dioxide materials are mainly concentrated on compact block materials and film materials at present, reports on the preparation of uranium dioxide porous ceramics are very few, zhao Ran et al take silica colloid crystals as templates, molten uranyl nitrate is immersed and cast into the templates, reduction treatment is carried out under hydrogen atmosphere after high-temperature calcination, and finally the templates are removed through chemical etching to obtain uranium dioxide mesoporous materials, but the uranium dioxide porous materials prepared by the method have low structural strength and are difficult to obtain complete porous ceramic block materials.
With the development of technology, the requirements on material performance are continuously improved, single-component materials and structures are more and more powerful in meeting the use requirements, the traditional materials have remarkable achievements in the aspects of multi-material compounding, microstructure design and the like, and compared with uranium oxide materials, the uranium oxide materials have larger gaps in the aspects of material design, preparation technology and the like, and the application range of the uranium oxide materials is limited to a great extent.
Disclosure of Invention
The invention aims to overcome the problems in the background art and provide a preparation method of a uranium dioxide-carbon composite phase porous material, wherein the prepared uranium dioxide-carbon composite phase porous material has high phase purity and good structural stability, and the density, specific surface area, conductivity and the like of the material can be regulated and controlled in a larger range according to design requirements. The uranium dioxide-carbon composite phase porous material prepared by the method is particularly suitable for being used as a catalyst or a thermoelectric material.
The invention relates to a preparation method of uranium dioxide-carbon composite phase porous material, which is carried out according to the following contents:
(1) Resorcinol and formaldehyde solution are used as raw materials, glacial acetic acid is used as a catalyst, dissolved in deionized water, and stirred uniformly to prepare resorcinol-formaldehyde sol;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 50-90 ℃, the preservation time is 1-10 days, and then drying in air for 1-5 days to obtain resorcinol-formaldehyde aerogel;
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tubular furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 600-1200 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-5 h, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving uranium oxide precursor, a structure directing agent and an organic additive in a mixed solvent of deionized water and ethanol, uniformly stirring, standing and ageing for 1-7 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), standing in a low vacuum environment to remove residual gas in the porous carbon material, and then drying in air, wherein the steps are circulated for 1-10 times to obtain a porous material blank; wherein, the vacuum treatment time is 1-5 min, the vacuum degree is 10-50 kPa, and the drying time is 12-96 h;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, performing high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 100-10000 Pa, the treatment temperature is 900-1200 ℃, the heating rate is 0.5-3 ℃/min, the heat preservation time is 1-5 h, and cooling to room temperature to obtain the uranium dioxide-carbon complex phase porous material.
Further, in the step (1), resorcinol is dissolved in deionized water, and formaldehyde solution and glacial acetic acid are added; the mol ratio of the resorcinol to the formaldehyde is 1:2; wherein the mass volume ratio of resorcinol, deionized water, formaldehyde solution and glacial acetic acid is (1-15) g: (5-100) mL: (1-30) mL: (20-1000) mu L.
Further, the mass fraction of the formaldehyde solution is 37%.
Further, in the step (4), the molar mass volume ratio of uranium oxide precursor, structure directing agent/organic additive, deionized water and ethanol is (0.01-0.05) mol: (0.5-8.0) g: (1.0-6.0) g: (1.0-10.0) mL: (10-60) mL.
Further, the uranium oxide precursor in the step (4) is uranyl nitrate, uranyl chloride or uranyl acetate.
Further, the structure directing agent in the step (4) is F127 or P123.
Further, the organic additive in the step (4) is acetylacetone or polyethyleneimine.
Further, the constant temperature in the step (2) is 60-80 ℃, the preservation time is 1-10 days, and then the resorcinol-formaldehyde aerogel is obtained after drying in the air for 1-5 days.
Further, the treatment temperature in the step (3) is 800-1000 ℃, the heating rate is 2-4 ℃/min, and the heat preservation time is 1-5 h.
Further, the vacuum degree in the step (6) is 1000-5000 Pa, the treatment temperature is 1000-1100 ℃, the heating rate is 1-2 ℃/min, and the heat preservation time is 1-5 h.
The invention has the following beneficial effects:
1. the uranium dioxide-carbon composite phase porous material prepared by the method has high phase purity and good structural stability, and the density, specific surface area, conductivity and the like of the material can be regulated and controlled in a larger range according to design requirements.
2. On one hand, the porous carbon has higher strength as a framework, so that the stability of the structure of the complex-phase porous material is ensured; on the other hand, carbon source is provided to participate in carbothermic reduction reaction to obtain UO 2 The phase also avoids the problem that the material is easy to shrink and crack in the high-temperature reduction treatment process under the hydrogen atmosphere.
3. The uranium dioxide-carbon multiphase porous material prepared by the invention can give consideration to the specific surface area and the structural strength (390 m) 2 g@1.2MPa), has great application value in the uranium oxide catalysis field.
4. In the uranium dioxide-carbon multiphase porous material prepared by the method, the uranium dioxide has a higher Seebeck coefficient, the introduction of carbon compensates for the defect of the electrical conductivity of the uranium dioxide, and meanwhile, the porous structure is beneficial to the maintenance of the material with a lower thermal conductivity, so that the multiphase porous material has higher thermoelectric performance.
5. The preparation method of the uranium dioxide-carbon composite porous material provided by the invention has the advantages of simple experimental process, convenience in operation control and no need of expensive experimental equipment.
Drawings
FIG. 1 is a photograph of a sample of uranium dioxide-carbon composite porous material;
figure 2 is an XRD pattern of a uranium dioxide-carbon composite porous material.
Detailed Description
For the purposes of clarity, technical solutions and advantages of embodiments of the present invention, the spirit of the present disclosure will be described in detail below, and any person skilled in the art, after having appreciated the embodiments of the present disclosure, may make changes and modifications to the techniques taught by the present disclosure without departing from the spirit and scope of the present disclosure.
The exemplary embodiments of the present invention and the descriptions thereof are intended to illustrate the present invention, but not to limit the present invention.
Example 1:
the preparation method of the uranium dioxide-carbon composite phase porous material is realized by the following steps:
(1) 2.4g of resorcinol is dissolved in 10mL of deionized water, 4.3mL of formaldehyde solution and 165 mu L of glacial acetic acid are added, and the resorcinol-formaldehyde sol is prepared after uniform stirring;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 80 ℃, the preservation time is 3 days, and then drying in air for 2 days to obtain resorcinol-formaldehyde aerogel;
resorcinol and formaldehyde react to generate resorcinol-formaldehyde aerogel, and porous carbon materials are obtained after carbonization treatment, and the porous carbon materials are used as porous templates in the patent and participate in carbothermic reduction reaction at high temperature to reduce uranium oxide into UO2.
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tubular furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 1000 ℃, the heating rate is 2 ℃/min, the heat preservation time is 2h, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving 8.5g of uranyl acetate, 2g of F127 and 3g of acetylacetone in a mixed solvent of 2mL of deionized water and 30mL of ethanol, uniformly stirring, standing and aging for 2 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), standing in a low vacuum environment to remove residual gas in the porous carbon material, and performing vacuum treatment for 1min with a vacuum degree of 20kPa; drying in air for 24h, and circulating the steps for 2 times to obtain a porous material blank;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, carrying out high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 500Pa, the treatment temperature is 1000 ℃, the heating rate is 0.5 ℃/min, the heat preservation time is 3h, and cooling to room temperature to obtain the uranium dioxide-carbon complex phase porous material.
The macroscopic photograph of the uranium dioxide-carbon multiphase porous material sample obtained by the embodiment is shown in figure 1, the sample structure is perfect and is not defective, the material can be proved to have better structural stability, and the sample density is 0.6g/cm 3 A specific surface area of 470m 2 And/g. Analysis by an X-ray diffractometer shows that the sample phase is UO 2 . The mechanical property of the uranium dioxide-carbon composite phase porous material sample is tested, and the compressive strength is 0.45MPa.
Example 2:
the preparation method of the uranium dioxide-carbon composite phase porous material is realized by the following steps:
(1) 10.0g of resorcinol is dissolved in 40mL of deionized water, 18mL of formaldehyde solution and 520 mu L of glacial acetic acid are added, and the resorcinol-formaldehyde sol is prepared after uniform stirring;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 60 ℃, the preservation time is 7 days, and then drying in air for 4 days to obtain resorcinol-formaldehyde aerogel;
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tubular furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 800 ℃, the heating rate is 1 ℃/min, the heat preservation time is 1h, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving 6.8g of uranyl chloride, 3.5g of P123 and 3g of polyethyleneimine in a mixed solvent of 4mL of deionized water and 50mL of ethanol, uniformly stirring, standing and aging for 5 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), standing in a low vacuum environment to remove residual gas in the porous carbon material, and performing vacuum treatment for 3min with a vacuum degree of 40kPa; drying in air for 48h, and circulating the steps for 5 times to obtain a porous material blank;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, carrying out high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 1000Pa, the treatment temperature is 1200 ℃, the heating rate is 1 ℃/min, the heat preservation time is 2h, and cooling to the room temperature to obtain the uranium dioxide-carbon complex phase porous material.
The XRD pattern of the uranium dioxide-carbon composite porous material sample obtained in the embodiment is shown in figure 2, and the result shows that the main phase of the uranium dioxide-carbon composite porous material is UO 2 . The specific surface area of the uranium dioxide-carbon composite phase porous material sample is 390m 2 And/g, the compressive strength is 1.2MPa. The conductivity at 300K is 16.5S/cm, the Seebeck coefficient is-248 mu V/K, and the power factor is 1.01 mu W/cm.K 2 。
Example 3:
the preparation method of the uranium dioxide-carbon composite phase porous material is realized by the following steps:
(1) 12.0g of resorcinol is dissolved in 20mL of deionized water, 21.7mL of formaldehyde solution and 780 mu L of glacial acetic acid are added, and the resorcinol-formaldehyde sol is prepared after uniform stirring;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 85 ℃, the preservation time is 4 days, and then drying in air for 5 days to obtain resorcinol-formaldehyde aerogel;
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tube furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 1200 ℃, the heating rate is 4 ℃/min, the heat preservation time is 3h, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving 15g of uranyl nitrate, 5g of F127 and 3g of acetylacetone in a mixed solvent of 8mL of deionized water and 55mL of ethanol, uniformly stirring, standing and aging for 5 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), and standing in a low vacuum environment to remove residual gas in the porous carbon material, wherein the vacuum treatment time is 2min, and the vacuum degree is 25kPa; drying in air for 72h, and circulating the steps for 4 times to obtain a porous material blank;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, carrying out high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 200Pa, the treatment temperature is 1100 ℃, the heating rate is 2 ℃/min, the heat preservation time is 4h, and cooling to room temperature to obtain the uranium dioxide-carbon complex phase porous material.
The sample density of the uranium dioxide-carbon composite porous material obtained in the embodiment is 0.95g/cm 3 Specific surface area of 320m 2 Conductivity at 300K is 18.3S/cm, seebeck coefficient is-275. Mu.V/K, and power factor is 1.38. Mu.W/cm.K 2 。
Example 4:
the preparation method of the uranium dioxide-carbon composite phase porous material is realized by the following steps:
(1) 4.0g of resorcinol is dissolved in 5mL of deionized water, 7.2mL of formaldehyde solution and 138 mu L of glacial acetic acid are added, and the resorcinol-formaldehyde sol is prepared after uniform stirring;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 70 ℃, the preservation time is 7 days, and then drying in air for 3 days to obtain resorcinol-formaldehyde aerogel;
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tubular furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 800 ℃, the heating rate is 2 ℃/min, the heat preservation time is 4 hours, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving 6.4g of uranyl acetate, 1.5g of P123 and 1.0g of acetylacetone in a mixed solvent of 1.0mL of deionized water and 30mL of ethanol, uniformly stirring, standing and aging for 2 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), standing in a low vacuum environment to remove residual gas in the porous carbon material, and performing vacuum treatment for 1min with a vacuum degree of 30kPa; drying in air for 48h, and circulating the steps for 5 times to obtain a porous material blank;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, carrying out high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 5000Pa, the treatment temperature is 900 ℃, the heating rate is 1 ℃/min, the heat preservation time is 5h, and cooling to room temperature to obtain the uranium dioxide-carbon complex phase porous material.
The sample density of the uranium dioxide-carbon composite porous material obtained in the embodiment is 1.35g/cm 3 Specific surface area of 240m 2 Per g, a compressive strength of 1.7MPa and a conductivity of 22.3S/cm at 300K.
Claims (10)
1. The preparation method of the uranium dioxide-carbon composite phase porous material is characterized by comprising the following steps of:
(1) Resorcinol and formaldehyde solution are used as raw materials, glacial acetic acid is used as a catalyst, dissolved in deionized water, and stirred uniformly to prepare resorcinol-formaldehyde sol;
(2) Placing the resorcinol-formaldehyde sol obtained in the step (1) in an incubator for constant temperature sealing and preservation, wherein the constant temperature is 50-90 ℃, the preservation time is 1-10 days, and then drying in air for 1-5 days to obtain resorcinol-formaldehyde aerogel;
(3) Placing the resorcinol-formaldehyde aerogel obtained in the step (2) in a tubular furnace, performing high-temperature treatment under argon atmosphere, wherein the treatment temperature is 600-1200 ℃, the heating rate is 1-5 ℃/min, the heat preservation time is 1-5 h, and cooling to room temperature to obtain a porous carbon material;
(4) Dissolving uranium oxide precursor, a structure directing agent and an organic additive in a mixed solvent of deionized water and ethanol, uniformly stirring, standing and ageing for 1-7 days to prepare uranium oxide precursor solution;
(5) Placing the porous carbon material obtained in the step (3) into the uranium oxide precursor solution prepared in the step (4), standing in a low vacuum environment to remove residual gas in the porous carbon material, and then drying in air, wherein the steps are circulated for 1-10 times to obtain a porous material blank; wherein, the vacuum treatment time is 1-5 min, the vacuum degree is 10-50 kPa, and the drying time is 12-96 h;
(6) And (3) placing the porous material blank obtained in the step (5) in a tubular furnace, performing high-temperature treatment under a low-pressure environment, wherein the vacuum degree is 100-10000 Pa, the treatment temperature is 900-1200 ℃, the heating rate is 0.5-3 ℃/min, the heat preservation time is 1-5 h, and cooling to room temperature to obtain the uranium dioxide-carbon complex phase porous material.
2. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1, wherein in the step (1), resorcinol is dissolved in deionized water, and formaldehyde solution and glacial acetic acid are added; the mol ratio of the resorcinol to the formaldehyde is 1:2; wherein the mass volume ratio of resorcinol, deionized water, formaldehyde solution and glacial acetic acid is (1-15) g: (5-100) mL: (1-30) mL: (20-1000) mu L.
3. The method for preparing the uranium dioxide-carbon composite porous material according to claim 1, wherein the mass fraction of the formaldehyde solution is 37%.
4. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1, wherein in the step (4), a molar mass volume ratio of a uranium oxide precursor, a structure directing agent/organic additive, deionized water and ethanol is (0.01 to 0.05) mol: (0.5-8.0) g: (1.0-6.0) g: (1.0-10.0) mL: (10-60) mL.
5. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1 or 4, wherein the uranium oxide precursor in the step (4) is uranyl nitrate, uranyl chloride or uranyl acetate.
6. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1 or 4, wherein the structure directing agent in the step (4) is F127 or P123.
7. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1 or 4, wherein the organic additive in the step (4) is acetylacetone or polyethyleneimine.
8. The method for preparing a uranium dioxide-carbon composite porous material according to claim 1, wherein the constant temperature in the step (2) is 60-80 ℃, the preservation time is 1-10 days, and then the porous material is dried in air for 1-5 days to obtain resorcinol-formaldehyde aerogel.
9. The method for preparing the uranium dioxide-carbon composite porous material according to claim 1, wherein the treatment temperature in the step (3) is 800-1000 ℃, the heating rate is 2-4 ℃/min, and the heat preservation time is 1-5 h.
10. The method for preparing the uranium dioxide-carbon composite porous material according to claim 1, wherein the vacuum degree in the step (6) is 1000-5000 Pa, the treatment temperature is 1000-1100 ℃, the heating rate is 1-2 ℃/min, and the heat preservation time is 1-5 h.
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