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CN-121974348-A - Porous tantalum carbide and preparation method and application thereof

CN121974348ACN 121974348 ACN121974348 ACN 121974348ACN-121974348-A

Abstract

The invention discloses porous tantalum carbide, a preparation method and application thereof, the preparation method of the porous tantalum carbide comprises the following steps of uniformly mixing tantalum powder with a carbon-based binder under continuous stirring, adding a pore-forming agent, continuously stirring until the mixture is completely and uniformly mixed to obtain a mixture, standing the mixture for 1-3 h under low pressure, sequentially carrying out first calcination treatment and second calcination treatment under a protective atmosphere condition, cooling to room temperature along with a furnace after the second calcination treatment is finished to obtain a calcination product, soaking the calcination product in dilute hydrochloric acid, washing with water to be neutral, and drying to obtain the porous tantalum carbide. The tantalum carbide prepared by the method has high porosity of 65-78%, pore diameters are intensively distributed in a range of 150-300 nm, and mechanical strength is excellent.

Inventors

  • XU KAIHUA
  • FENG HAO
  • SHE HAIYANG
  • CAI XIANG
  • ZHANG ZHENZHEN

Assignees

  • 湖北绿钨资源循环有限公司

Dates

Publication Date
20260505
Application Date
20260120

Claims (10)

  1. 1. A method for preparing porous tantalum carbide, which is characterized by comprising the following steps: (1) Uniformly mixing tantalum powder and a carbon-based binder under continuous stirring, adding a pore-forming agent, and continuously stirring until the tantalum powder and the carbon-based binder are completely uniformly mixed to obtain a mixture; the carbon-based binder is Resol type phenolic resin, furan resin or polyimide resin; (2) Standing the mixture obtained in the step (1) for 1-3 hours under low pressure, and then sequentially carrying out first calcination treatment and second calcination treatment under the condition of protective atmosphere, wherein after the second calcination treatment is finished, cooling to room temperature along with a furnace to obtain a calcination product; (3) And (3) soaking the calcined product in the step (2) in dilute hydrochloric acid, washing with water to be neutral, and drying to obtain the porous tantalum carbide.
  2. 2. The method for preparing porous tantalum carbide according to claim 1, wherein the mass ratio of the tantalum powder to the carbon-based binder in the step (1) is 1:1-2.
  3. 3. The method for preparing porous tantalum carbide according to claim 1, wherein the addition amount of the pore-forming agent in the step (1) is 20-40 wt% of the total amount of tantalum powder and carbon-based binder.
  4. 4. The method for producing a porous tantalum carbide according to any of claims 1 to 3, wherein the pore-forming agent in step (1) is at least one of polyethylene glycol, corn starch and polymethyl methacrylate, and/or The protective atmosphere in the step (2) is at least one of inert gas and nitrogen.
  5. 5. The method of producing porous tantalum carbide according to claim 1, wherein the stirring rate of the continuous stirring in the step (1) is 50 to 300rpm, and/or And (3) the gauge pressure of the low pressure in the step (2) is 0.5-0.8 atm.
  6. 6. The method for preparing the porous tantalum carbide according to claim 1, wherein the specific mode of the first calcination treatment in the step (2) is that the temperature is raised to 900-500 ℃ at a temperature raising rate of 5-20 ℃ per minute and the temperature is kept for 5-10 hours.
  7. 7. The method for producing porous tantalum carbide according to claim 1, wherein the second calcination treatment in step (2) is performed by continuously heating to 2000-3000 ℃ at a heating rate of 5-20 ℃ per minute and keeping the temperature for 25-40 hours after the first calcination treatment, and/or And (2) after the second calcination treatment is finished, firstly reducing the temperature to 600-900 ℃ at the speed of 5-20 ℃ per minute, and then cooling to room temperature along with a furnace.
  8. 8. The method for preparing porous tantalum carbide according to claim 1, wherein the concentration of the dilute hydrochloric acid in the step (3) is 5-20wt%, and the soaking treatment time is 10-20 hours.
  9. 9. The porous tantalum carbide produced by the method of any one of claims 1 to 8.
  10. 10. The use of the porous tantalum carbide of claim 9 in the fields of extreme environmental filtration, aerospace thermal protection, energy electrodes and wear and corrosion resistance.

Description

Porous tantalum carbide and preparation method and application thereof Technical Field The invention belongs to the technical field of refractory metal porous material preparation, and particularly relates to porous tantalum carbide, a preparation method and application thereof. Background Tantalum carbide (TaC) is used as a typical refractory metal carbide, has an ultra-high melting point (3880 ℃), excellent high-temperature stability, high hardness (HV 1800-2200) and strong corrosion resistance, and has irreplaceable application value in high-end fields such as extreme environment filtration, aerospace thermal protection, energy electrodes, wear resistance and corrosion resistance due to the fact that the porous structure of the tantalum carbide has both the intrinsic performance and controllable pore characteristics of the material. In a high-temperature filtering scene, the high-performance armor-piercing bullet core can be suitable for purifying molten steel above 1500 ℃, filtering aeroengine fuel gas and separating nuclear industrial radioactive waste, can be used as a rocket engine jet pipe lining, a spacecraft thermal protection coating substrate or be compounded with a metal matrix to prepare the high-performance armor-piercing bullet core in the field of aerospace military industry, can be used as a Solid Oxide Fuel Cell (SOFC) electrode support and a nuclear reactor neutron absorbing material in the field of energy, can meet the requirements of gas diffusion, electric conduction and heat dissipation, and can also be used as a hard alloy reinforcing phase or a chemical equipment corrosion-resistant lining to improve the wear resistance and corrosion resistance of the material. However, the existing preparation process of the porous tantalum carbide still has a plurality of technical bottlenecks, which limit the industrialized application and the performance improvement of the porous tantalum carbide. The powder sintering method needs high temperature (2000-2400 ℃) and long-time sintering, is high in energy consumption and easy to cause grain growth, the pore structure is uncontrollable (the deviation of pore diameter distribution is larger than 30%), products with high porosity (more than 50%) and excellent connectivity are difficult to prepare, the gel casting method is complex in forming process, shrinkage deformation is easy to occur in the drying and degreasing processes of blanks, the yield is low (less than 60%), parts with complex shapes or large sizes are difficult to prepare, the chemical vapor deposition method is high in equipment cost, low in deposition rate and low in preparation efficiency, the porosity is difficult to accurately regulate (error is larger than 15%), the method is not suitable for batch production, the pore-forming agent adding method is poor in compatibility between a traditional pore-forming agent (such as ammonium bicarbonate) and TaC powder, agglomeration and forming cracking problems are easy to occur, and residual impurities of the pore-forming agent can cause the reduction of product purity and the corrosion resistance is damaged. In addition, the porous tantalum carbide prepared by the prior art has the common problems of uneven pore distribution, poor cooperativity between mechanical strength and porosity, easy collapse of pore structure at high temperature and the like, and cannot meet the comprehensive requirements of high-end application scenes on materials such as high porosity, accurate pore size distribution, excellent mechanical stability and high purity. Therefore, development of porous tantalum carbide with controllable porosity, uniform pore size distribution, excellent mechanical strength and high-temperature stability, simple preparation process and controllable cost has become a technical problem to be solved in the current refractory metal porous material field. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide porous tantalum carbide and a preparation method and application thereof. In a first aspect, the present invention provides a method for preparing porous tantalum carbide, comprising the steps of: (1) Uniformly mixing tantalum powder and a carbon-based binder under continuous stirring, adding a pore-forming agent, and continuously stirring until the tantalum powder and the carbon-based binder are completely uniformly mixed to obtain a mixture; the carbon-based binder is Resol type phenolic resin, furan resin or polyimide resin; (2) Standing the mixture obtained in the step (1) for 1-3 hours under low pressure (mainly used for removing residual bubbles in the mixture), and then sequentially carrying out first calcination treatment and second calcination treatment under the condition of protective atmosphere, and cooling to room temperature along with a furnace after the second calcination treatment is finished to obtain a calcination product; (3) And (3) soaking the calcined product in the step (