CN114959905A - Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof - Google Patents
Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof Download PDFInfo
- Publication number
- CN114959905A CN114959905A CN202210216794.XA CN202210216794A CN114959905A CN 114959905 A CN114959905 A CN 114959905A CN 202210216794 A CN202210216794 A CN 202210216794A CN 114959905 A CN114959905 A CN 114959905A
- Authority
- CN
- China
- Prior art keywords
- tac
- catalyst
- whisker
- graphite crucible
- tantalum carbide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910003468 tantalcarbide Inorganic materials 0.000 title claims abstract description 44
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000011775 sodium fluoride Substances 0.000 claims description 11
- 235000013024 sodium fluoride Nutrition 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000006722 reduction reaction Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 230000007480 spreading Effects 0.000 claims description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000002159 nanocrystal Substances 0.000 abstract description 4
- 230000002787 reinforcement Effects 0.000 abstract description 3
- 230000035939 shock Effects 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241001330002 Bambuseae Species 0.000 description 2
- 229920001410 Microfiber Polymers 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000003658 microfiber Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a catalyst-free synthesized tantalum carbide nano whisker and a preparation method thereof. Meanwhile, the required production equipment is simple, the technological process is simple, the parameters are easy to control, the reliability and the repeatability are good, and the large-scale production is easy to realize. The TaC nano crystal whisker prepared by the process method has the obvious advantages of high purity and large length-diameter ratio (125-2000), so that the TaC nano crystal whisker has higher specific strength, can be used as an ideal nano reinforcement to be applied to various composite materials, and can obviously improve the strength and the thermal shock resistance of the materials and also improve the electrical conductivity of the materials.
Description
Technical Field
The invention belongs to a nano material preparation technology, and relates to a catalyst-free synthesized tantalum carbide nano whisker and a preparation method thereof.
Background
As an excellent transition metal carbide, TaC has high hardness (Mohs hardness 9-10), high melting point (3880 ℃), high Young modulus (283-550GPa), good electric conductivity (32.7-117.4 mu omega cm at 25 ℃) and good chemical corrosion resistance and oxidation resistance, and has attractive application prospect in the high-temperature field. The TaC nanowhisker has the advantages of good performance of TaC ceramics, high length-diameter ratio, few defects and high specific strength, is an ideal composite material reinforcement, can obviously improve the strength and thermal shock resistance when being applied to ceramic matrix and C/C composite materials, can obviously improve the strength and modulus of the materials when being applied to polymer composite materials, and can obviously improve the conductivity of the materials. Meanwhile, the TaC nanowhisker also has excellent conductivity and chemical stability, and has potential advantages in the aspects of assembly of electronic probes, microelectronic devices and the like.
At present, few reports about preparation methods of TaC nanowhiskers exist, and metal powder is introduced as a catalyst.
Document 1 "M.Johnson and M.Nygren.Carbothermal synthesis of TaC whiteskers via vapor-liquid growth mechanism, 1997,12(9): 2419- 2 O 5 A C-NaCl reaction system, and growing straight TaC whiskers with smooth surfaces in a relatively low temperature region (1200-1300 ℃) by a carbothermal reduction method. The whiskers prepared by the document have a diameter of 0.1-0.6 μm and a length of 10-30 μm. The main impurities are TaC particles, small amounts of unreacted carbon and residues of Ni catalyst.
Literature3 'X.Y.Tao, J.Du, Y.P.Li, et al.TaC nanowire/activated carbon micro fiber structures from bamboo fibers advanced Energy Materials,2011,1:534 plus 539' the catalyst and tantalum precursor (Ta. precursor) 2 O 5 -NaF-ZnCl 2 -Ni(NO 3 ) 2 ·6H 2 O-Fe(NO 3 ) 3 ·9H 2 O) is loaded on the bamboo fiber, and the TaC nanowire/activated carbon superfine fiber hybrid structure is obtained after heat treatment for 2 hours at 1300 ℃, and a large amount of TaC nanowires grow radially on the carbon microfiber. The surface is smooth, the tip is provided with catalyst particles, the diameter is about 110nm, and the length is more than 20 mu m.
Comprehensive analysis shows that the preparation of TaC nanowhiskers mostly needs metal catalysts, and the introduction of the catalysts influences the purity of the nanowhiskers. Moreover, it can be seen from the above documents that the TaC whiskers produced by the prior art are all shorter in length and therefore have a small aspect ratio (5-482). The TaC nano-whisker prepared by the carbothermic method has the diameter distribution of 0.2-0.4 μm, the length of about 50-400 μm, the length-diameter ratio of 125-2000, no introduction of metal catalyst and higher purity. Meanwhile, the preparation process is simple, the preparation period is short, and the reliability and the repeatability are good.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a catalyst-free synthesized tantalum carbide nano whisker and a preparation method thereof, and provides a process method for preparing high-purity TaC nano whisker with the diameter of 0.2-0.4 mu m and the length of about 50-400 mu m.
Technical scheme
A catalyst-free synthesized tantalum carbide nano whisker is characterized in that: the TaC nano-whisker prepared by the carbothermic method has the diameter distribution of 0.2-0.4 μm, the length of about 50-400 μm and the length-diameter ratio of 125-2000.
A method for preparing the catalyst-free synthesized tantalum carbide nanowhisker is characterized by comprising the following steps:
step 1: activated carbon C and tantalum oxide Ta 2 O 5 And sodium fluoride NaF powder, grinding in a ceramic mortar to uniformly mix, and uniformly spreading the powder in a graphite crucible;
ta is C 2 O 5 The molar ratio of NaF is 1:0.05-0.35: 0.3-1.2;
step 2: placing the graphite crucible containing the mixed powder in a horizontal tubular resistance furnace, carrying out carbothermic reduction reaction under the protection of inert gas, raising the temperature to 1200-1450 ℃ at the heating rate of 5-8 ℃/min, and preserving the temperature for 2-4 h; cooling to 200-400 ℃ at the cooling rate of 4-6 ℃/min, cooling to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
The mixed powder of step 1 is sieved by a 100-300 mesh sieve.
The inert gas in the step 2 is argon Ar or nitrogen N 2 。
The gas flow of the inert gas in the step 2 is 20-60 ml/min.
Advantageous effects
The invention provides a catalyst-free synthesized tantalum carbide nano whisker and a preparation method thereof. Meanwhile, the required production equipment is simple, the technological process is simple, the parameters are easy to control, the reliability and the repeatability are good, and the large-scale production is easy to realize. The TaC nano crystal whisker prepared by the process method has the obvious advantages of high purity and large length-diameter ratio (125-2000), so that the TaC nano crystal whisker has higher specific strength, can be used as an ideal nano reinforcement to be applied to various composite materials, and can obviously improve the strength and the thermal shock resistance of the materials and also improve the electrical conductivity of the materials.
Drawings
FIG. 1 is an X-ray diffraction pattern of TaC nanowhiskers synthesized in example 1
FIG. 2 is a scanning electron micrograph of TaC nanowhiskers synthesized in example 1
Detailed Description
The invention will now be further described with reference to the following examples, and the accompanying drawings:
example 1:
step 1: according to the molar ratio of C to Ta 2 O 5 Raw materials are prepared by adding NaF (1: 0.2: 0.4) into a ceramic mortar and grinding to be uniformly mixed. The mixed powder is sieved by a 100-mesh sieve, and the sieved powder is uniformly laid in a graphite crucible.
And 2, step: and (3) placing the graphite crucible containing the mixed powder in the step (2) in a horizontal tubular resistance furnace, introducing nitrogen with the gas flow of 30ml/min, raising the temperature to 1400 ℃ at the heating rate of 5 ℃/min, and preserving the temperature for 2 h. And reducing the temperature to 400 ℃ at the cooling rate of 4 ℃/min, cooling to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
TaC nanowhiskers were successfully prepared in example 1, and the X-ray diffraction pattern thereof is shown in FIG. 1, and the scanning electron microscopy pattern thereof is shown in FIG. 2. The tip of the TaC nanowhisker is free of catalyst particles, and has a diameter of about 0.28 μm, a length of about 50-200 μm, and an aspect ratio of about 180-715. By integrating X-ray diffraction spectrogram and scanning electron microscope image, it can be seen that no catalyst impurity is introduced, and the purity of the nano-whisker is high.
Example 2:
step 1: according to the molar ratio of C to Ta 2 O 5 Raw materials are prepared by adding NaF (1: 0.3: 0.8) into a ceramic mortar and grinding to be uniformly mixed. The mixed powder is sieved by a 200-mesh sieve, and the sieved powder is uniformly paved into a graphite crucible.
Step 2: and (3) placing the graphite crucible filled with the mixed powder in the step (2) into a horizontal tubular resistance furnace, introducing argon with the gas flow of 40ml/min, raising the temperature to 1350 ℃ at the heating rate of 6 ℃/min, and preserving the temperature for 2 h. And reducing the temperature to 300 ℃ at the cooling rate of 4 ℃/min, cooling to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
Example 3:
step 1: according to the molar ratio of C to Ta 2 O 5 Raw materials are prepared by adding NaF into a ceramic mortar and grinding the raw materials until the NaF is mixed uniformly, wherein the NaF is 1:0.1: 1.0. The mixed powder is sieved by a 300-mesh sieve, and the sieved powder is uniformly paved into a graphite crucible.
Step 2: and (3) placing the graphite crucible containing the mixed powder in the step (2) in a horizontal tubular resistance furnace, introducing nitrogen with the air flow of 60ml/min, heating to 1300 ℃ at the heating rate of 7 ℃/min, and keeping the temperature for 3 hours. And reducing the temperature to 200 ℃ at the cooling rate of 5 ℃/min, cooling to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
Example 4:
step 1: according to the molar ratio of C to Ta 2 O 5 Raw materials are prepared in a ratio of 1:0.2:1.2, and are put into a ceramic mortar to be ground and uniformly mixed. The mixed powder is sieved by a 100-mesh sieve, and the sieved powder is uniformly paved into a graphite crucible.
Step 2: and (3) placing the graphite crucible filled with the mixed powder in the step (2) in a horizontal tubular resistance furnace, introducing argon with the gas flow of 20ml/min, raising the temperature to 1200 ℃ at the heating rate of 8 ℃/min, and preserving the temperature for 4 h. And reducing the temperature to 200 ℃ at the cooling rate of 6 ℃/min, cooling the temperature to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
Claims (5)
1. A catalyst-free synthesized tantalum carbide nano whisker is characterized in that: the TaC nano-whisker prepared by the carbothermic method has the diameter distribution of 0.2-0.4 μm, the length of about 50-400 μm and the length-diameter ratio of 125-2000.
2. A method of preparing the catalyst-free synthetic tantalum carbide nanowhiskers of claim 1, characterized by the steps of:
step 1: activated carbon C and tantalum oxide Ta 2 O 5 And sodium fluoride NaF powder, grinding in a ceramic mortar to uniformly mix, and uniformly spreading the powder in a graphite crucible;
ta is C 2 O 5 The molar ratio of NaF is 1:0.05-0.35: 0.3-1.2;
step 2: placing the graphite crucible containing the mixed powder in a horizontal tubular resistance furnace, carrying out carbothermic reduction reaction under the protection of inert gas, raising the temperature to 1200-1450 ℃ at the heating rate of 5-8 ℃/min, and preserving the temperature for 2-4 h; cooling to 200-400 ℃ at the cooling rate of 4-6 ℃/min, cooling to room temperature along with the furnace, and taking out the graphite crucible to obtain the TaC nanowhisker.
3. The method of claim 2, wherein: the mixed powder of step 1 is sieved by a 100-300 mesh sieve.
4. The method of claim 2, wherein: the inert gas in the step 2 is argon Ar or nitrogen N 2 。
5. The method of claim 2, wherein: the gas flow of the inert gas in the step 2 is 20-60 ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210216794.XA CN114959905A (en) | 2022-03-07 | 2022-03-07 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210216794.XA CN114959905A (en) | 2022-03-07 | 2022-03-07 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114959905A true CN114959905A (en) | 2022-08-30 |
Family
ID=82975456
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210216794.XA Pending CN114959905A (en) | 2022-03-07 | 2022-03-07 | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114959905A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4904622A (en) * | 1987-02-23 | 1990-02-27 | Pechiney Electrometallurgie | Process for the preparation of silicon carbide whiskers |
| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
| CN105502398A (en) * | 2016-03-01 | 2016-04-20 | 郑州大学 | Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction |
| CN105732042A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing ultrafine tantalum carbide powder by using fused salt under assistance of low temperature |
| CN106784667A (en) * | 2016-12-12 | 2017-05-31 | 武汉科技大学 | A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof |
| US20180154435A1 (en) * | 2011-06-17 | 2018-06-07 | Consolidated Nuclear Security, LLC | Titanium-Group Nano-Whiskers and Method of Production |
| CN110042468A (en) * | 2019-04-08 | 2019-07-23 | 西北工业大学 | A kind of preparation method of micrometer silicon carbide zirconium whisker |
| CN112195503A (en) * | 2020-09-24 | 2021-01-08 | 西北工业大学 | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method |
| CN114032607A (en) * | 2021-11-02 | 2022-02-11 | 西北工业大学 | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal |
-
2022
- 2022-03-07 CN CN202210216794.XA patent/CN114959905A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4904622A (en) * | 1987-02-23 | 1990-02-27 | Pechiney Electrometallurgie | Process for the preparation of silicon carbide whiskers |
| CN102051676A (en) * | 2010-10-29 | 2011-05-11 | 山东大学 | In-situ grown tantalum carbide whisker material and preparation method thereof |
| US20180154435A1 (en) * | 2011-06-17 | 2018-06-07 | Consolidated Nuclear Security, LLC | Titanium-Group Nano-Whiskers and Method of Production |
| CN105502398A (en) * | 2016-03-01 | 2016-04-20 | 郑州大学 | Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction |
| CN105732042A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing ultrafine tantalum carbide powder by using fused salt under assistance of low temperature |
| CN106784667A (en) * | 2016-12-12 | 2017-05-31 | 武汉科技大学 | A kind of charcoal material surface SiC Nanometer Whiskers and preparation method thereof |
| CN110042468A (en) * | 2019-04-08 | 2019-07-23 | 西北工业大学 | A kind of preparation method of micrometer silicon carbide zirconium whisker |
| CN112195503A (en) * | 2020-09-24 | 2021-01-08 | 西北工业大学 | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method |
| CN114032607A (en) * | 2021-11-02 | 2022-02-11 | 西北工业大学 | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal |
Non-Patent Citations (3)
| Title |
|---|
| 王富强;郝志彪;闫联生;: "碳化硅纳米晶须的制备研究", 材料导报, no. 2, 25 August 2008 (2008-08-25) * |
| 王骏;李国栋;熊翔;张磊;: "Ta_2O_5-NaF-C体系制备TaC晶须的机理", 粉末冶金材料科学与工程, vol. 21, no. 01, 29 February 2016 (2016-02-29), pages 1 - 3 * |
| 蔡志勇;曹顺华;谢湛;: "TiC晶须的制备及应用", 粉末冶金材料科学与工程, no. 02, 15 April 2007 (2007-04-15) * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5525050B2 (en) | Silicon carbide powder manufacturing method and system | |
| US8951451B2 (en) | Carbon material and method for producing same | |
| Hao et al. | Synthesis and characterization of bamboo-like SiC nanofibers | |
| JP3964381B2 (en) | Vapor grown carbon fiber, production method and use thereof | |
| KR20130085841A (en) | Silicon carbide powder and method for manufacturing the same | |
| Zhao et al. | Catalyst-free growth of single-crystalline alumina nanowire arrays | |
| Tian et al. | Single-crystalline hafnium carbide nanowire growth below the eutectic temperature by CVD | |
| CN111205100B (en) | Method for in-situ growth of silicon carbide nanowire by non-catalytic precursor impregnation pyrolysis method | |
| Chen et al. | Tuning the morphologies of SiC nanowires via the change of the Co x Si y melts | |
| CN112794330B (en) | Preparation method of boron carbide nanowires | |
| US8246743B2 (en) | Single crystal silicon carbide nanowire, method of preparation thereof, and filter comprising the same | |
| Liu et al. | Facile growth of oriented SiC nanowires arrays on carbon fiber cloth via CVD | |
| CN114959905A (en) | Catalyst-free synthesized tantalum carbide nano whisker and preparation method thereof | |
| Li et al. | A simple and efficient route to synthesize hafnium carbide nanowires by catalytic pyrolysis of a polymer precursor | |
| CN113279249A (en) | In-situ self-generated dispersion distributed carbide whisker on surface of carbon fiber and preparation method thereof | |
| CN114032607B (en) | Method for preparing zirconium carbide whisker by adopting zirconium carbide seed crystal | |
| CN113788464B (en) | Method for preparing boron nitride nanotube by using double transition metal oxide as catalyst | |
| Lu et al. | A CVD method for preparing CNTs-grafted carbon fiber fabrics under quasi-vacuum at low temperature | |
| US20210230743A1 (en) | High purity fiber feedstock for loose grain production | |
| CN112195503B (en) | Method for synthesizing hafnium carbide crystal whisker with large length-diameter ratio by carbothermic reduction method | |
| Thiên‐Nga et al. | Catalytic Growth of Carbon Nanorods on a High‐Tc Substrate | |
| CN110228811B (en) | Low-dimensional rare earth boride nano material and solid phase preparation method thereof | |
| CN113088923A (en) | Preparation method of zirconium carbide nanowire with high length-diameter ratio | |
| CN109957859B (en) | Silicon carbide fiber and preparation method thereof | |
| KR101916270B1 (en) | Method of fabricating silicon carbide powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |