HfCxNy ultrahigh-temperature ceramic powder material and preparation method thereof

A technology for ultra-high temperature ceramics and powder materials, which is applied in the field of HfCxNy ultra-high temperature ceramic powder materials and its preparation. It can solve the problems of cumbersome process flow, long holding time, and long preparation cycle, and achieve high melting point and fast heating and cooling rate. , The effect of short preparation cycle

Inactive Publication Date: 2021-02-12
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, existing HfC x N y The material preparation method requires harsh conditions, including extremely high temperature (≥2400°C) and long holding time (≥2h)
in N 2 The self-propagating combustion reaction of the powder is carried out under positive pressure conditions. This preparation method is dangerous, easy to explode, and the preparation cycle is long and the process is cumbersome.

Method used

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  • HfCxNy ultrahigh-temperature ceramic powder material and preparation method thereof
  • HfCxNy ultrahigh-temperature ceramic powder material and preparation method thereof
  • HfCxNy ultrahigh-temperature ceramic powder material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] First, 23.30 g of Hf powder with a particle size of 1 μm, 1.57 g of C powder with a particle size of 1 μm, and 25.13 g of HfN powder with a particle size of 1 μm (the prepared HfC x N y Material stoichiometry is HfC 0.5 N 0.5 ) into a nylon ball mill jar for ball milling for 12 hours. The mixture was dried in a rotary evaporator (evaporating pressure 5 kPa) at 60° C. at a speed of 65 rpm and passed through an 80-mesh sieve to obtain a mixed ceramic powder. Then, it was put into a stainless steel mold with a diameter of 20mm and cold-pressed at 10kN for 5min. Then, the cold-pressed mixed powder was placed in a graphite crucible, and placed in an induction heating furnace under protective N 2 Medium pressureless sintering, heating to 2400°C at a heating rate of 80°C / min, and holding for 0.5h. After the heat preservation is over, cool down to 1000°C at a cooling rate of 60°C / min, and air cool to room temperature to obtain HfC 0.5 N 0.5 Ultra-high temperature ceramic...

Embodiment 2

[0041] First, 19.61 g of Hf powder with a particle size of 2 μm, 1.32 g of C powder with a particle size of 2 μm, and 9.07 g of HfN powder with a particle size of 2 μm (the prepared HfC x N y Material stoichiometry is HfC 0.7 N 0.3 ) into a nylon ball mill jar for ball milling for 10 hours. Rotate and dry in a rotary evaporator (evaporating pressure 3 kPa) at 65° C. at a speed of 70 rpm and pass through a 100-mesh sieve to obtain a mixed ceramic powder. Then, it was put into a stainless steel mold with a diameter of 8mm and cold-pressed at 15kN for 8min. Then, the cold-pressed mixed powder was placed in a graphite crucible, and placed in an induction heating furnace under protective N 2 Medium pressureless sintering, heating to 2420°C at a heating rate of 90°C / min, and holding for 0.5h. After the heat preservation is over, cool down to 900°C at a cooling rate of 80°C / min, and air cool to room temperature to obtain HfC 0.7 N 0.3 Ultra-high temperature ceramic materials. ...

Embodiment 3

[0044] First, 11.20 g of Hf powder with a particle size of 0.5 μm, 0.75 g of C powder with a particle size of 1 μm, and 8.05 g of HfN powder with a particle size of 0.5 μm (the prepared HfC x N y Material stoichiometry is HfC 0.6 N 0.4 ) into a nylon ball mill jar for ball milling for 9 hours. Rotate drying in a rotary evaporator (evaporating pressure 6 kPa) at 55° C. at a speed of 75 rpm and pass through a 100-mesh sieve to obtain a mixed ceramic powder. Then, it was put into a stainless steel mold with a diameter of 10 mm and cold-pressed at 18 kN for 10 min. Then, the cold-pressed mixed powder was placed in a graphite crucible, and placed in an induction heating furnace under protective N 2 Medium pressureless sintering, heating to 2410°C at a heating rate of 100°C / min, and holding for 1h. After the heat preservation is over, cool down to 1000°C at a cooling rate of 90°C / min, and air cool to room temperature to obtain HfC 0.6 N 0.4 Ultra-high temperature ceramic mate...

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Abstract

The invention relates to the field of ultrahigh-temperature ceramic materials, in particular to an HfCxNy ultrahigh-temperature ceramic powder material and a preparation method thereof, wherein the sum of x and y is more than 0 and less than and equal to 1. The material is prepared by induction heating pressureless sintering, the preparation method includes: (1) adding Hf, C and HfN powder into anylon tank according to the proportion, adopting absolute ethyl alcohol as a medium and conducting wet milling to obtain powder paste; (2) performing rotary evaporation of the powder paste and dryingand screening to obatin Hf-C-HfN mixing powder, and conducting cold press molding in a stainless steel mould; and (3) placing the formed blank into a graphite crucible and puting the formed blank withthe graphite crucible into an ultrahigh-temperature induction heater, perfroming pressureless sintering under nitrogen atmosphere to obtain HfCxNy ultrahigh-temperature ceramic. The HfCxNy superhigh-temperature material prepared by the method has the advantages of high purity, simple preparation process flow, short preparation period and the like.

Description

technical field [0001] The invention relates to the field of ultra-high temperature ceramic materials, specifically a HfC x N y Ultra-high temperature ceramic powder material and preparation method thereof. Background technique [0002] Ultra-high temperature ceramics refer to a class of non-oxide ceramic materials with a melting point exceeding 3000°C, mainly including borides, carbides and nitrides of early transition metals, among which carbides and nitrides have a series of unique properties, including high density , chemical thermal stability, corrosion resistance and extremely high melting point, making it an ideal candidate material system for ultra-high temperature thermal structures and thermal protection systems. Among them, HfC has a very high melting point (3890°C), which is the highest melting point among known single compounds. According to theoretical calculations, it is known that the Hf-C-N system of the ternary phase has a record high melting point. Due...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/66C04B35/64C04B35/626B28B3/00
CPCB28B3/00C04B35/58007C04B35/6261C04B35/62655C04B35/64C04B35/66C04B2235/3886C04B2235/404C04B2235/422C04B2235/5436C04B2235/5445C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/668
Inventor 徐敬军张鑫涛钱余海李美栓左君
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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