CN116947497A - Medium-entropy or high-entropy carbide nano powder and preparation method thereof - Google Patents

Medium-entropy or high-entropy carbide nano powder and preparation method thereof Download PDF

Info

Publication number
CN116947497A
CN116947497A CN202310988127.8A CN202310988127A CN116947497A CN 116947497 A CN116947497 A CN 116947497A CN 202310988127 A CN202310988127 A CN 202310988127A CN 116947497 A CN116947497 A CN 116947497A
Authority
CN
China
Prior art keywords
source
entropy
mixed solution
medium
nano powder
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
Application number
CN202310988127.8A
Other languages
Chinese (zh)
Inventor
欧阳海波
陈子浩
李翠艳
高瑞楠
申天展
王锦涛
祁思怡
杨骞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN202310988127.8A priority Critical patent/CN116947497A/en
Publication of CN116947497A publication Critical patent/CN116947497A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention provides a medium-entropy or high-entropy carbide nano powder and a preparation method thereof, comprising the following steps: 1) Adding a Ta source, a Nb source, a Ti source, a Zr source and a Hf source into ethanol to prepare a mixed solution A; or adding a Hf source, a Zr source and a Ti source into ethanol to prepare a mixed solution B; 2) Adding phenolic resin and furfuryl alcohol into the mixed solution A or the mixed solution B, and uniformly mixing to obtain a mixed solution C; 3) Stirring the mixed solution C under the heating condition, performing polycondensation reaction, obtaining a cured product G after the reaction is completed, and drying the cured product; 4) The dried cured product G was carbonized at high temperature to obtain (Ta 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C high entropy powder or(HfZrTi) C. The preparation method has the advantages of simple process flow, no need of other process assistance, short preparation period and low process cost, and is suitable for large-scale industrial production.

Description

Medium-entropy or high-entropy carbide nano powder and preparation method thereof
Technical Field
The invention relates to the field of nanocomposite materials, in particular to a medium-entropy or high-entropy carbide nano powder and a preparation method thereof.
Background
In recent years, a medium-entropy and high-entropy material is an object of extensive research in the scientific community at home and abroad as a novel material, and the medium-entropy and high-entropy material is the biggest difference compared with the traditional material in that the medium-entropy and high-entropy material is a solid solution formed by elements with various equimolar or nearly equimolar ratios, and has excellent properties which are not possessed by the conventional materials. The concept of medium entropy and high entropy is only widely studied in the alloy field, but with the deep research, the medium entropy and high entropy ceramics are also widely studied, and the medium entropy and high entropy ceramics are taken as a new ceramic material type, and become research hot spots due to the unique composition and excellent performance of the ceramic material type. The thermodynamic stability of the material is improved through multi-component solid solution reaction. (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) The C carbide ceramic combines Ta, nb, ti, zr, hf metal elements with C atoms, so as to form a high-entropy solid solution; and (HfZrTi) C carbide ceramic is formed by combining metallic elements of Hf, zr and Ti with C atoms to form a medium entropy solid solution. The high-entropy ceramic plays a vital role in the field of ultra-high temperature application due to the excellent ablation resistance.
Chinese patent application 202010842711.9 reports a preparation method of (HfZrTi) C-based entropy ceramic, which comprises the steps of mixing an oxide corresponding to a metal component with a carbon source, and reacting the metal oxide with the carbon source at 1300-1700 ℃ under vacuum to generate (HfZrTi) C-based entropy ceramic composite powder; and then sintering the ceramic material to obtain the high-temperature-resistant high-strength (HfZrTi) C medium-entropy ceramic material. The preparation method has the advantages of complex process, high cost and high time cost, thus limiting the further development of the method.
The literature "Li F, lu Y, wang X G, et al, liquid pre-reactor-derived high-entropy carbide nano powders [ J ]. Ceramics International,2019,45 (17): 22437-22441" reports that a brown liquid precursor of high-entropy carbide is obtained by a sol-gel method, and then further heated under flowing argon atmosphere at 1600-2000 ℃ to obtain single-phase high-entropy carbide powder. But the method has long preparation period, high cost and environmental pollution.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the medium-entropy or high-entropy carbide nano powder and the preparation method thereof, and the preparation method has the advantages of simple process flow, no need of other process assistance, short preparation period and low process cost, and is suitable for large-scale industrial production.
The invention is realized by the following technical scheme:
the preparation method of the medium-entropy or high-entropy carbide nano powder comprises the following steps:
1) Adding a Ta source, a Nb source, a Ti source, a Zr source and a Hf source into ethanol to prepare a mixed solution A; or adding a Hf source, a Zr source and a Ti source into ethanol to prepare a mixed solution B;
2) Adding phenolic resin and furfuryl alcohol into the mixed solution A or the mixed solution B, and uniformly mixing to obtain a mixed solution C;
3) Stirring the mixed solution C under the heating condition, performing polycondensation reaction, obtaining a cured product G after the reaction is completed, and drying the cured product;
4) The dried cured product G was carbonized at high temperature to obtain (Ta 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C high entropy powder or (HfZrTi) C medium entropy powder.
Preferably, in the mixed solution A, the Ta source, the Nb source, the Ti source, the Zr source and the Hf source are TaCl respectively 5 、NbCl 5 、TiCl 4 、ZrCl 4 HfCl 4
Preferably, in the mixed solution A, the molar ratio of the Ta source, the Nb source, the Ti source, the Zr source and the Hf source is 1:1:1:1.
PreferablyIn the mixed solution B, the Hf source, the Zr source and the Ti source are HfCl respectively 4 、ZrCl 4 And TiCl 4
Preferably, in the mixed solution B, the mol ratio of the Hf source to the Zr source to the Ti source is 1:1:1.
Preferably, in step 2), the molar ratio of furfuryl alcohol to phenolic resin is 1 (1-3).
Preferably, in step 2), the molar ratio of the total amount of metal in the mixed liquor A or the mixed liquor B to furfuryl alcohol is 1 (1-5).
Preferably, in step 3), the heating temperature is 40 to 60 ℃.
Preferably, in step 4), the high temperature carbonization is specifically: and in Ar atmosphere, heating from room temperature to 2000-2100 ℃ at a heating rate of 3-6 ℃/min, and calcining for 2-4 h.
The medium-entropy or high-entropy carbide nano powder is obtained by adopting the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
compared with the technology of preparing nano powder by using water heat, the method for preparing nano powder by using the medium-entropy or high-entropy carbide does not need external force conditions, but prepares five or three transition metal sources, furfuryl alcohol and phenolic resin into precursor liquid, and performs polycondensation reaction on furfuryl alcohol and phenolic resin in the precursor liquid by regulating and controlling the reaction temperature to obtain a cross-linked and solidified product, and performs carbon heat reduction to obtain the nano powder by using the medium-entropy or high-entropy carbide. The method disclosed by the invention is simple in operation process, does not need other process assistance, is low in cost of raw materials, low in equipment requirement and low in synthesis temperature, and the synthesized carbide nano powder is small in grain size (average grain size is 80 nm), high in purity and uniform in distribution of elements, so that the method has the potential of being developed into large-scale industrial production.
The medium-entropy or high-entropy carbide nano powder prepared by the invention has small grain size (average grain size is 80 nm), high purity and uniform distribution of each element.
Drawings
FIGS. 1 and 2 show the results of examples 3 and 4 of the present invention (HfZ)rTi) entropy powder in C (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) XRD pattern of high-entropy powder;
FIGS. 3 and 4 are (HfZrTi) C medium entropy powder and (Ta) synthesized according to examples 3 and 4, respectively, of the present invention 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C, surface Scanning Electron Microscopy (SEM) and X-ray energy spectrum analysis (EDS) images of the high-entropy powder.
Detailed Description
For a further understanding of the present invention, the present invention is described below in conjunction with the following examples, which are provided to further illustrate the features and advantages of the present invention and are not intended to limit the claims of the present invention.
Example 1:
(1) HfCl in amounts of 0.01mol each 4 、ZrCl 4 And TiCl 4 Preparing a mixed solution B with the concentration of 0.3mol/L by the three precursors and an ethanol solvent, and stirring the mixed solution B at room temperature until the mixed solution B is uniform;
(2) taking 20ml of the mixed solution B, and dropwise adding furfuryl alcohol and phenolic resin (n=1:1) into the mixed solution B to obtain a mixed solution C;
(3) placing the mixed solution C in a magnetic stirrer to stir at 60 ℃, and obtaining a cured product G3-1 after the polycondensation reaction of furfuryl alcohol is finished;
(4) and (3) placing the cured product G3-1 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and cured products G3-1 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 3 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the (HfZrTi) C medium entropy carbide nano powder is obtained after the mixture is cooled to the room temperature along with the furnace.
Example 2:
(1) TaCl in amounts of 0.02mol each 5 、NbCl 5 、TiCl 4 、ZrCl 4 HfCl 4 Preparing a mixed solution A with the concentration of 1.0mol/L from the five precursors and an ethanol solvent, and stirring the mixed solution A to be uniform at room temperature;
(2) taking 20ml of the mixed solution A, and dropwise adding furfuryl alcohol and phenolic resin (n=1:1) into the mixed solution A to obtain a mixed solution C;
(3) placing the mixed solution C in a magnetic stirrer to stir at 60 ℃, and obtaining a cured product G5-1 after the polycondensation reaction of furfuryl alcohol is finished;
(4) and (3) placing the cured product G5-1 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and cured products G5-1 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 3 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the mixture is cooled to the room temperature along with the furnace, thus obtaining (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C, high-entropy carbide nano powder.
Example 3:
(1) HfCl with 0.02mol of each substance 4 、ZrCl 4 And TiCl 4 Preparing a mixed solution B with the concentration of 0.6mol/L by the three precursors and an ethanol solvent, and stirring the mixed solution B at room temperature until the mixed solution B is uniform;
(2) taking 20ml of the mixed solution B, and then dropwise adding furfuryl alcohol and phenolic resin (n=1:2) into the mixed solution B to obtain a mixed solution C;
(3) placing the mixed solution C under the heating of a magnetic stirrer at 50 ℃, and obtaining a cured product G3-2 after the polycondensation reaction of furfuryl alcohol is finished;
(4) and (3) placing the cured product G3-2 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and cured products G3-2 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 2 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the (HfZrTi) C medium entropy carbide nano powder is obtained after the mixture is cooled to the room temperature along with the furnace.
Example 4:
(1) TaCl in amounts of 0.04mol each 5 、NbCl 5 、TiCl 4 、ZrCl 4 HfCl 4 The five precursors and ethanol solvent are prepared into mixed solution with the concentration of 2.0mol/LA, stirring to be uniform at room temperature;
(2) taking 20ml of the mixed solution A, and then dropwise adding furfuryl alcohol and phenolic resin (n=1:2) into the mixed solution A to obtain a mixed solution C;
(3) placing the mixed solution C under the heating of a magnetic stirrer at 50 ℃, and obtaining a cured product G5-2 after the polycondensation reaction of furfuryl alcohol is finished;
(4) and (3) placing the cured product G5-2 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and solidified products G5-2 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 2 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the mixture is cooled to the room temperature along with the furnace, thus obtaining (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C, high-entropy carbide nano powder.
Example 5:
(1) HfCl with 0.03mol of each substance 4 、ZrCl 4 And TiCl 4 Preparing a mixed solution B with the concentration of 0.9mol/L by the three precursors and an ethanol solvent, and stirring the mixed solution B at room temperature until the mixed solution B is uniform;
(2) taking 20ml of the mixed solution B, and then dropwise adding furfuryl alcohol and phenolic resin (n=1:3) into the mixed solution B to obtain a mixed solution C;
(3) placing the mixed solution C in a magnetic stirrer to heat at 40 ℃, and obtaining a cured product G3-3 after the furfuryl alcohol polycondensation reaction is finished;
(4) and (3) placing the cured product G3-3 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and cured products G3-3 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 4 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the (HfZrTi) C medium entropy carbide nano powder is obtained after the mixture is cooled to the room temperature along with the furnace.
Example 6:
(1) TaCl in amounts of 0.05mol each 5 、NbCl 5 、TiCl 4 、ZrCl 4 HfCl 4 Preparing a mixed solution A with the concentration of 2.5mol/L from the five precursors and an ethanol solvent, and stirring the mixed solution A to be uniform at room temperature;
(2) taking 20ml of the mixed solution A, and then dropwise adding furfuryl alcohol and phenolic resin (n=1:3) into the mixed solution A to obtain a mixed solution C;
(3) placing the mixed solution C in a magnetic stirrer to heat at 40 ℃, and obtaining a cured product G5-3 after the furfuryl alcohol polycondensation reaction is finished;
(4) and (3) placing the cured product G5-3 obtained in the step (3) in a constant-temperature blast drying oven, setting the temperature to 100 ℃, and taking out after heat preservation for 2 hours.
(5) And (3) respectively placing the dried and solidified products G5-3 obtained in the step (4) into graphite crucibles, then placing the graphite crucibles into a vertical atmosphere high temperature furnace, and heating the furnace to 2100 ℃ and preserving heat for 4 hours under the protection of Ar gas with the flow of 300 sccm. The temperature rising rate is 3 ℃/min, and the mixture is cooled to the room temperature along with the furnace, thus obtaining (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C, high-entropy carbide nano powder.
FIGS. 1 and 2 show the results of the synthesis of examples 3 and 4 (Ta 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) XRD patterns of the high-entropy powder and the entropy powder in (HfZrTi) C show that the synthesized powder is single (Ta) 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) The C phase (HfZrTi) C phase has no other hetero-phase, so that the purity of the intermediate-entropy and high-entropy carbide nano powder prepared by the method is higher.
FIGS. 3 and 4 show the results of the synthesis of examples 3 and 4, respectively, (Ta 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C high entropy powder, surface Scanning Electron Microscope (SEM) and X-ray energy spectrum analysis (EDS) images of (HfZrTi) C medium entropy powder, and the images show that the medium entropy and high entropy carbide nano powder prepared by the method of the invention is composed of particles with the size of about 80nm, generally aggregated into clusters and uniformly distributed elements.
The medium-entropy and high-entropy carbide nano powder prepared by the invention has at least the following advantages: according to the invention, a liquid phase method synthesis thought is utilized, the proportion of furfuryl alcohol and phenolic resin is regulated, three transition metal principal elements of Hf, zr and Ti or five transition metal elements of Ta, nb, ti, zr, hf are introduced by utilizing the characteristic of spontaneous polymerization of the furfuryl alcohol and the phenolic resin under a specific temperature condition, so that simple synthesis of the intermediate-entropy and high-entropy carbide nano powder precursor is realized, and the key effect on the expanded production and preparation of the intermediate-entropy and high-entropy carbide nano powder precursor is realized.
The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (10)

1. The preparation method of the medium-entropy or high-entropy carbide nano powder is characterized by comprising the following steps of:
1) Adding a Ta source, a Nb source, a Ti source, a Zr source and a Hf source into ethanol to prepare a mixed solution A; or adding a Hf source, a Zr source and a Ti source into ethanol to prepare a mixed solution B;
2) Adding phenolic resin and furfuryl alcohol into the mixed solution A or the mixed solution B, and uniformly mixing to obtain a mixed solution C;
3) Stirring the mixed solution C under the heating condition, performing polycondensation reaction, obtaining a cured product G after the reaction is completed, and drying the cured product;
4) The dried cured product G was carbonized at high temperature to obtain (Ta 0.2 Nb 0.2 Ti 0.2 Zr 0.2 Hf 0.2 ) C high entropy powder or (HfZrTi) C medium entropy powder.
2. The method for preparing the nano powder of the medium-entropy or high-entropy carbide according to claim 1, wherein in the mixed solution A, the Ta source, the Nb source, the Ti source, the Zr source and the Hf source are TaCl respectively 5 、NbCl 5 、TiCl 4 、ZrCl 4 HfCl 4
3. The method for preparing the nano powder of the medium-entropy or high-entropy carbide according to claim 1, wherein in the mixed solution A, the molar ratio of the Ta source, the Nb source, the Ti source, the Zr source and the Hf source is 1:1:1:1:1.
4. The method for preparing the nano powder of the medium-entropy or high-entropy carbide according to claim 1, wherein in the mixed solution B, the Hf source, the Zr source and the Ti source are HfCl respectively 4 、ZrCl 4 And TiCl 4
5. The method for preparing the nano powder of the medium-entropy or high-entropy carbide according to claim 1, wherein the molar ratio of the Hf source to the Zr source to the Ti source in the mixed solution B is 1:1:1.
6. The method for preparing the nano powder of the medium-entropy or high-entropy carbide according to claim 1, wherein in the step 2), the molar ratio of the furfuryl alcohol to the phenolic resin is 1 (1-3).
7. The method for preparing nano powder of medium-entropy or high-entropy carbide according to claim 1, wherein in the step 2), the molar ratio of the total metal amount in the mixed solution A or the mixed solution B to furfuryl alcohol is 1 (1-5).
8. The method for preparing nano powder of medium-entropy or high-entropy carbide according to claim 1, wherein in step 3), the heating temperature is 40-60 ℃.
9. The method for preparing the medium-entropy or high-entropy carbide nano powder according to claim 1, wherein in the step 4), the high-temperature carbonization is specifically: and in Ar atmosphere, heating from room temperature to 2000-2100 ℃ at a heating rate of 3-6 ℃/min, and calcining for 2-4 h.
10. A medium-or high-entropy carbide nanopowder obtained by the preparation method according to any one of claims 1 to 9.
CN202310988127.8A 2023-08-07 2023-08-07 Medium-entropy or high-entropy carbide nano powder and preparation method thereof Pending CN116947497A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310988127.8A CN116947497A (en) 2023-08-07 2023-08-07 Medium-entropy or high-entropy carbide nano powder and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310988127.8A CN116947497A (en) 2023-08-07 2023-08-07 Medium-entropy or high-entropy carbide nano powder and preparation method thereof

Publications (1)

Publication Number Publication Date
CN116947497A true CN116947497A (en) 2023-10-27

Family

ID=88444463

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310988127.8A Pending CN116947497A (en) 2023-08-07 2023-08-07 Medium-entropy or high-entropy carbide nano powder and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116947497A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115772034A (en) * 2023-02-13 2023-03-10 中国人民解放军国防科技大学 High-entropy carbide ceramic precursor, high-entropy carbide ceramic and preparation method
CN116514553A (en) * 2023-05-09 2023-08-01 武汉科技大学 Composite carbide ceramic powder material and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115772034A (en) * 2023-02-13 2023-03-10 中国人民解放军国防科技大学 High-entropy carbide ceramic precursor, high-entropy carbide ceramic and preparation method
CN116514553A (en) * 2023-05-09 2023-08-01 武汉科技大学 Composite carbide ceramic powder material and preparation method and application thereof

Similar Documents

Publication Publication Date Title
JPS5934147B2 (en) Silicon carbide sintered ceramic body and its manufacturing method
JPS5921579A (en) Silicon carbide sintered molded body and manufacture
CN110407213B (en) (Ta, nb, ti, V) C high-entropy carbide nano powder and preparation method thereof
CN110467467B (en) Bulk silicon carbide polymer precursor ceramic and blending and cracking preparation method
CN107522485B (en) Spinel fiber reinforced zirconia refractory material and preparation process thereof
CN103508437A (en) Preparation method of phenolic resin base glass carbon microsphere
CN112250440B (en) Method for preparing low-thermal-conductivity high-temperature thermal-barrier ceramic CaWTa2O9 by solid-phase method
Shi et al. Synthesis and characterization of submicron silicon carbide powders with silicon and phenolic resin
CN116514553A (en) Composite carbide ceramic powder material and preparation method and application thereof
CN101734920B (en) Titanium nitride porous ceramics and preparation method thereof
EP1761474A1 (en) Process for manufacturing high density boron carbide
CN113582700B (en) Preparation method of low-cost titanium boride ceramic composite material
Zheng et al. Improving the sinterability of ZrC–SiC composite powders by Mg addition
CN113735590A (en) Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material
CN109231990A (en) A kind of preparation method of tungsten carbide-diamond composite
CN116947497A (en) Medium-entropy or high-entropy carbide nano powder and preparation method thereof
Chkhartishvili et al. Highly Stable Boron Carbide–Based Nanocomposites
CN113683418B (en) Tantalate spherical powder CaMoTa for thermal spraying 2 O 9 And a method for preparing the same
CN116178019A (en) Method for preparing porous MAX phase ceramic material by pressureless wrapping calcination
CN110183229A (en) A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology
CN109019624B (en) Low-temperature synthesized flaky ZrB2Method for preparing superfine powder
CN111732436A (en) Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof
CN114890422B (en) Flaky high-entropy MAX phase material and preparation method thereof
CN111455253A (en) Titanium carbide-based metal ceramic thermal spraying powder and preparation method thereof
CN110357637A (en) Super fine titanium carbonitride powder end and preparation method thereof

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