CN112570711A - Preparation method of nickel-coated titanium carbide composite powder - Google Patents
Preparation method of nickel-coated titanium carbide composite powder Download PDFInfo
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- CN112570711A CN112570711A CN202011345323.6A CN202011345323A CN112570711A CN 112570711 A CN112570711 A CN 112570711A CN 202011345323 A CN202011345323 A CN 202011345323A CN 112570711 A CN112570711 A CN 112570711A
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- titanium carbide
- nickel
- composite powder
- powder
- coated titanium
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 239000000843 powder Substances 0.000 title claims abstract description 83
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 230000009467 reduction Effects 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 17
- 239000007795 chemical reaction product Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 6
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001994 activation Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
Abstract
The invention relates to a preparation method of nickel-coated titanium carbide composite powder, which comprises the following steps: putting nickel sulfate powder, ammonia water and activated titanium carbide powder into a reaction kettle to form mixed liquid, and sealing the reaction kettle; introducing hydrogen into the reaction kettle, and keeping a preset hydrogen pressure; the reaction kettle is heated and stirred for reaction, and the nickel-coated titanium carbide composite powder is obtained. The invention utilizes the high-pressure hydrogen reduction method to prepare the nickel-coated titanium carbide composite powder, has simple process and is green and pollution-free.
Description
Technical Field
The invention relates to a preparation method of nickel-coated titanium carbide composite powder, belonging to the technical field of nickel-coated titanium carbide.
Background
To the best of the applicant's knowledge, the metal ceramic composite powder is a composite powder material with a ceramic core and a metal layer coated on the outer surface. The material has the high hardness of a ceramic material and the toughness of a metal material. Meanwhile, the existence of the metal shell obviously improves the wettability among ceramic powder particles, and has a decisive role in obtaining compact block materials and high-toughness functional coatings.
TiC (titanium carbide) has excellent physical and chemical properties such as high hardness, good thermal stability, oxidation resistance, corrosion resistance, small density and the like, and is a metal-based particle reinforced material with great development prospect. However, the TiC has poor wettability with metal and weak binding force, so that the physical and mechanical properties of the composite material are greatly influenced, and the development of the TiC particle reinforced composite material is restricted. By adopting a chemical coating method, a layer of metallic nickel is coated on the surface of TiC, so that the wettability among particles and between the particles and a matrix can be effectively improved. However, the industrial titanium carbide powder has low surface activity, and metal particles are difficult to uniformly deposit on the surface of the industrial titanium carbide powder and form nuclei to grow in the chemical coating process, so that the coating rate of the nickel element in the prepared composite powder is low. In addition, chemical plating is a common method for preparing nickel-coated titanium carbide composite powder, but the process has the defects of plating solution pollution, unstable process, low production efficiency and the like.
The applicant finds that the high-pressure hydrogen reduction method is an efficient preparation method of metal-coated ceramic composite powder, has the advantages of controllable stability, high production efficiency and the like, and is widely used for preparing nickel-coated graphite, nickel-coated aluminum oxide and other powder. However, the method for preparing the nickel-coated titanium carbide composite powder is not reported.
Disclosure of Invention
The main purposes of the invention are: the method for preparing the nickel-coated titanium carbide composite powder overcomes the problems in the prior art, is simple in process and green and has no pollution.
The technical scheme for solving the technical problems of the invention is as follows:
a preparation method of nickel-coated titanium carbide composite powder is characterized by comprising the following steps:
firstly, putting nickel sulfate powder, ammonia water and activated titanium carbide powder into a reaction kettle to form mixed liquid, and sealing the reaction kettle;
secondly, introducing hydrogen into the reaction kettle, and keeping a preset hydrogen pressure; the reaction kettle is heated and stirred for reaction, and the nickel-coated titanium carbide composite powder is obtained.
The preparation method comprises the steps of adding activated titanium carbide powder into nickel sulfate serving as a nickel source, hydrogen serving as a reducing agent and ammonia serving as a neutralizing agent by using a high-pressure hydrogen reduction method, and then heating, pressurizing and stirring to react to obtain a mixture of nickel-coated titanium carbide, ammonium sulfate and water, wherein no pollutant is discharged, and the whole preparation process is green and pollution-free. Meanwhile, in the whole reaction process, the reaction solution is very stable, and the problem of decomposition or hydrolysis does not exist; and the TiC content can be accurately controlled, the mass fraction can reach more than 50 percent at most, and the nickel-coated titanium carbide composite powder with corresponding particle size distribution can be directly prepared.
The technical scheme of the invention is further perfected as follows:
preferably, in the first step, the particle size of the titanium carbide powder is 80-150 meshes, and the nickel content in the nickel sulfate powder is more than 21.8%.
Preferably, in the first step, the activation process of the titanium carbide powder is as follows:
activating titanium carbide powder in aqua regia for 30-120 minutes by taking aqua regia as an activating agent to obtain coarsened titanium carbide powder, washing the titanium carbide powder by deionized water until the pH value is neutral, then washing by absolute ethyl alcohol, and then drying in a drying oven at 80-120 ℃ to obtain the activated titanium carbide powder.
Preferably, in the mixed liquid in the first step, the concentration of the nickel sulfate is 160-220g/L, and the concentration of the ammonia water is 20-60 g/L.
By adopting the preferable scheme, the specific details of the first step can be further optimized, and the nickel-coated titanium carbide composite powder can be better prepared.
Preferably, in the second step, the heating temperature of the reaction kettle is 120-160 ℃; the hydrogen pressure of the reaction kettle is 2-5 MPa.
Preferably, in the second step, the reaction is a reduction and neutralization reaction, specifically:
preferably, in the second step, the mass fraction of TiC in the nickel-coated titanium carbide composite powder is 30-60%, and the thickness of the nickel layer is 1-20 microns.
By adopting the preferred scheme, the specific details of the second step can be further optimized, and the nickel-coated titanium carbide composite powder can be better prepared.
Preferably, the preparation method further comprises:
and step three, washing, drying and screening the reaction product to obtain a finished product.
More preferably, the third step comprises the following specific processes:
and taking out a reaction product from the reaction kettle, repeatedly cleaning the reaction product with deionized water until the pH value is neutral, drying the reaction product in an oven, and screening the reaction product in a vibrating screen machine to obtain a finished product with the powder granularity of 80-150 meshes.
More preferably, the drying condition is drying at 120 ℃ for 60 min; the vibrating screen machine is a slapping vibrating screen machine.
By adopting the preferred scheme, the specific details of the third step can be further added and optimized, and the nickel-coated titanium carbide composite powder can be prepared better.
Compared with the prior art, the method for preparing the nickel-coated titanium carbide composite powder by using the high-pressure hydrogen reduction method has the advantages of simple process, greenness, no pollution and very wide application prospect.
Drawings
Fig. 1 and 2 are graphs showing analysis results in example 1 of the present invention.
Fig. 3 and 4 are graphs showing analysis results in example 2 of the present invention.
Detailed Description
In specific implementation, the preparation method of the nickel-coated titanium carbide composite powder comprises the following steps:
firstly, putting nickel sulfate powder, ammonia water and activated titanium carbide powder into a reaction kettle to form mixed liquid, and sealing the reaction kettle.
Wherein the particle size of the titanium carbide powder is 80-150 meshes, and the nickel content in the nickel sulfate powder is more than 21.8%.
The activation process of the titanium carbide powder is as follows: activating titanium carbide powder in aqua regia for 30-120 minutes by taking aqua regia as an activating agent to obtain coarsened titanium carbide powder, washing the titanium carbide powder by deionized water until the pH value is neutral, then washing by absolute ethyl alcohol, and then drying in a drying oven at 80-120 ℃ to obtain the activated titanium carbide powder.
In the mixed liquid, the concentration of the nickel sulfate is 160-220g/L, and the concentration of the ammonia is 20-60 g/L.
Secondly, introducing hydrogen into the reaction kettle, and keeping a preset hydrogen pressure; the reaction kettle is heated and stirred for reaction, and the nickel-coated titanium carbide composite powder is obtained.
Wherein the heating temperature of the reaction kettle is 120-160 ℃; the hydrogen pressure of the reaction kettle is 2-5 MPa. The reaction is reduction and neutralization reaction, and specifically comprises the following steps:
the weight percentage of TiC in the nickel-coated titanium carbide composite powder is 30-60%, and the thickness of a nickel layer is 1-20 microns.
And step three, washing and drying the reaction product to obtain a finished product. The specific process is as follows:
and taking out a reaction product from the reaction kettle, repeatedly cleaning the reaction product with deionized water until the pH value is neutral, drying the reaction product in an oven, and screening the reaction product in a vibrating screen machine to obtain a finished product with the powder granularity of 80-150 meshes.
Wherein the drying condition is drying at 120 ℃ for 60 min; the vibrating screen machine is a slapping vibrating screen machine.
The invention is described in further detail below with reference to embodiments and with reference to the drawings. The invention is not limited to the examples given.
Example 1
The embodiment adopts the technical scheme, and specific parameters are briefly summarized as follows:
200g of activated titanium carbide powder and 909g of nickel sulfate powder are weighed and placed in a reaction kettle, ammonia water is added to form a mixed solution, the concentration of nickel sulfate in the mixed solution is 160g/L, and the concentration of ammonia water is 40 g/L. During the reaction, the heating temperature is 160 ℃, and the hydrogen pressure is 5 MPa. The mass fraction of TiC in the nickel-coated titanium carbide composite powder is 30%.
The results of analyzing the obtained nickel-coated titanium carbide composite powder are shown in fig. 1 and 2.
Fig. 1 is a surface view (scanning electron microscope image) of a nickel-coated titanium carbide composite powder particle, which shows: the surface of the formed particles appears porous and has a fluffy state.
Fig. 2 is an EDS spectrum analysis diagram showing: the Ni content of the A point on the particle surface is 100 percent, which indicates that the surface of the composite powder is completely coated by the metal Ni layer.
Example 2
The embodiment adopts the technical scheme, and specific parameters are briefly summarized as follows:
200g of activated titanium carbide powder and 909g of nickel sulfate powder are weighed and placed into a reaction kettle, ammonia water is added to form a mixed solution, the concentration of nickel sulfate in the mixed solution is 180g/L, and the concentration of ammonia water is 40 g/L. During the reaction, the heating temperature is 150 ℃, and the hydrogen pressure is 5 MPa. The mass fraction of TiC in the nickel-coated titanium carbide composite powder is 50%.
The results of analyzing the obtained nickel-coated titanium carbide composite powder are shown in fig. 3 and 4.
FIG. 3 is a sectional view (scanning electron microscope) of a nickel-coated titanium carbide composite powder particle, and FIG. 4 is a line scan of an EDS particle. It shows that: uniform nickel-coated titanium carbide particles were formed, with the thickness of the nickel (Ni) layer being 15-20 microns.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of nickel-coated titanium carbide composite powder is characterized by comprising the following steps:
firstly, putting nickel sulfate powder, ammonia water and activated titanium carbide powder into a reaction kettle to form mixed liquid, and sealing the reaction kettle;
secondly, introducing hydrogen into the reaction kettle, and keeping a preset hydrogen pressure; the reaction kettle is heated and stirred for reaction, and the nickel-coated titanium carbide composite powder is obtained.
2. The method for preparing the nickel-coated titanium carbide composite powder according to claim 1, wherein in the first step, the particle size of the titanium carbide powder is 80-150 meshes, and the nickel content in the nickel sulfate powder is greater than 21.8%.
3. The method for preparing the nickel-coated titanium carbide composite powder according to claim 2, wherein in the first step, the activation process of the titanium carbide powder is as follows:
activating titanium carbide powder in aqua regia for 30-120 minutes by taking aqua regia as an activating agent to obtain coarsened titanium carbide powder, washing the titanium carbide powder by deionized water until the pH value is neutral, then washing by absolute ethyl alcohol, and then drying in a drying oven at 80-120 ℃ to obtain the activated titanium carbide powder.
4. The method for preparing the nickel-coated titanium carbide composite powder as claimed in claim 3, wherein the concentration of the nickel sulfate in the mixed solution of the first step is 160-220g/L, and the concentration of the ammonia water is 20-60 g/L.
5. The method for preparing the nickel-coated titanium carbide composite powder according to claim 1, wherein in the second step, the heating temperature of the reaction kettle is 120-160 ℃; the hydrogen pressure of the reaction kettle is 2-5 MPa.
6. The method for preparing the nickel-coated titanium carbide composite powder according to claim 5, wherein in the second step, the reaction is a reduction and neutralization reaction, and specifically comprises the following steps:
7. the method for preparing the nickel-coated titanium carbide composite powder according to claim 6, wherein in the second step, the mass fraction of TiC in the nickel-coated titanium carbide composite powder is 30-60%, and the thickness of the nickel layer is 1-20 microns.
8. The method for preparing the nickel-coated titanium carbide composite powder according to claim 1, further comprising:
and step three, washing, drying and screening the reaction product to obtain a finished product.
9. The method for preparing the nickel-coated titanium carbide composite powder according to claim 8, wherein the third step comprises the following specific steps:
and taking out a reaction product from the reaction kettle, repeatedly cleaning the reaction product with deionized water until the pH value is neutral, drying the reaction product in an oven, and screening the reaction product in a vibrating screen machine to obtain a finished product with the powder granularity of 80-150 meshes.
10. The method for preparing the nickel-coated titanium carbide composite powder according to claim 9, wherein the drying is performed at 120 ℃ for 60 min; the vibrating screen machine is a slapping vibrating screen machine.
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| CN202011345323.6A CN112570711A (en) | 2020-11-26 | 2020-11-26 | Preparation method of nickel-coated titanium carbide composite powder |
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| CN202011345323.6A CN112570711A (en) | 2020-11-26 | 2020-11-26 | Preparation method of nickel-coated titanium carbide composite powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115364780A (en) * | 2022-07-20 | 2022-11-22 | 西南科技大学 | Preparation and application of derivative titanium dioxide/reduced graphene oxide composite aerogel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157130A (en) * | 2007-11-08 | 2008-04-09 | 北京科技大学 | A method of preparing nickel silicon carbide complex powder by heavy pressure hydrogen reduction |
| CN109365802A (en) * | 2018-11-13 | 2019-02-22 | 中国科学院过程工程研究所 | A kind of preparation method of core-shell structure metal ceramic composite powder |
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2020
- 2020-11-26 CN CN202011345323.6A patent/CN112570711A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157130A (en) * | 2007-11-08 | 2008-04-09 | 北京科技大学 | A method of preparing nickel silicon carbide complex powder by heavy pressure hydrogen reduction |
| CN109365802A (en) * | 2018-11-13 | 2019-02-22 | 中国科学院过程工程研究所 | A kind of preparation method of core-shell structure metal ceramic composite powder |
Non-Patent Citations (2)
| Title |
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| 朱成才等: "镍包碳化钛复合粉末的制备及活化工艺研究", 《热喷涂技术》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115364780A (en) * | 2022-07-20 | 2022-11-22 | 西南科技大学 | Preparation and application of derivative titanium dioxide/reduced graphene oxide composite aerogel |
| CN115364780B (en) * | 2022-07-20 | 2024-01-26 | 西南科技大学 | Preparation and application of derivative titanium dioxide/reduced graphene oxide composite aerogel |
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Application publication date: 20210330 |