CN110407213A - One kind (Ta, Nb, Ti, V) C high entropy carbide nano powder and preparation method thereof - Google Patents
One kind (Ta, Nb, Ti, V) C high entropy carbide nano powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses one kind (Ta, Nb, Ti, V) C high entropy carbide nano powders and preparation method thereof.The preparation method comprises the following steps: (1) by Ta powder, Nb powder, Ti powder, V powder, C powder and KCl ground and mixed;(2) by mixed powder high temperature sintering, it is passed through Ar gas shielded in sintering process, is cooled to room temperature after the completion of sintering;(3) mixed powder through oversintering finally obtains (Ta, Nb, Ti, V) C high entropy carbide nano powder through deionized water washing, filtering and drying.The method of the invention not only used by low in raw material price, synthesis temperature is low, equipment requirement is low, and (the Ta of synthesis, Nb, Ti, V) C high entropy carbide nano powder crystallite dimension small (average grain size is 80 ~ 90 nm), purity is high and ingredient are uniform, these advantages make this method have the potentiality for developing into large-scale industrial production.
Description
Technical field
The invention belongs to high entropy compound technicals, and in particular to one kind (Ta, Nb, Ti, V) C high entropy carbide is received
Rice flour body and preparation method thereof.
Background technique
The concept of high entropy material was proposed by TaiWan, China Tsinghua University professor Ye Junwei for the first time in 2004, and was defined
For element species >=4, without dominant element, and the content of every kind of element is between 5% ~ 35%.So far, both at home and abroad
Researcher is concentrated mainly on alloy field about the research of high entropy material, less for the research of ceramic field.High entropy ceramics
Material is a kind of new ceramic material occurred in recent years, is reported for the first time from the concept of 2015 high entropy oxide ceramic material
Since, high entropy ceramic material becomes research hotspot in recent years, all kinds of high entropy oxides, boride, nitride and carbonization
Object ceramic material is reported in succession.Wherein, high entropy carbide ceramics material is because having high fusing point, lower thermal conductivity, excellent
The characteristics such as different mechanical property and good high-temperature physics chemical stability and the extensive concern by domestic and international researcher.
However, the high generally existing crystallite dimension of entropy carbide ceramics material prepared at present is big, porosity is high, elemental constituent is uneven etc.
Some problems.The synthesis of the high entropy carbide ceramics powder of high pure and ultra-fine for solve the above problems play the role of it is vital.
However, less about the synthetic method report of the high entropy carbide ceramics powder of high pure and ultra-fine both at home and abroad at present.
Document: " Zhou J, Zhang J, Zhang F, et al. High-entropy carbide:A novel
class of multicomponent ceramics. Ceramics International, 2018, 44(17): 22014
~ 22018. " are described and a kind of are sintered using five kinds of carbide powders of TiC, ZrC, HfC, NbC, TaC as raw material, using SPS
The method that technology prepares (Hf, Ta, Ti, Zr, Nb) C high entropy carbide powder at 2000 DEG C.This method not only raw material valence
Lattice valuableness, preparation temperature high (2000 DEG C), equipment requirement are high, and (Hf, Ta, Ti, Zr, Nb) the C high entropy carbonization synthesized
Powder crystallite dimension big (micron order), uneven components and purity is not high, these disadvantages seriously limit pushing away for this method
Wide and application.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the purpose of the present invention is to provide one kind (Ta, Nb, Ti, V) C
High entropy carbide nano powder and preparation method thereof.This method using Ta powder, Nb powder, Ti powder, V powder and C powder as raw material, with KCl
As fused-salt medium, by raw material, directly one kind (Ta, Nb, Ti, V) C high entropy carbon is prepared in reaction in fused salt at low temperature
Compound nano-powder, not only low in raw material price, synthesis temperature are low, equipment requirement is low for this method, but also prepare (Ta, Nb,
Ti, V) C high entropy carbide nano powder ingredient uniformly, purity is high and crystallite dimension it is small (average grain size be 80 ~ 90
Nm).
The purpose of the present invention is realized at least through one of following technical solution.
The preparation method of one kind (Ta, Nb, Ti, V) C high entropy carbide nano powder, includes the following steps:
(1) by Ta powder, Nb powder, Ti powder, V powder, C powder and KCl ground and mixed;
(2) by mixed powder high temperature sintering, it is passed through Ar gas shielded in sintering process, is cooled to room temperature after the completion of sintering;
(3) mixed powder through oversintering is through deionized water washing, filtering and dry, finally obtain it is described (Ta, Nb, Ti,
V) C high entropy carbide nano powder.
Further, in the step (1), Ta powder, Nb powder, Ti powder, V powder partial size be 1 ~ 3 μm, purity >=
The partial size of 99.5%, C powder is 0.7 ~ 0.9 μm, purity >=99.9%.
Further, in the step (1), Ta powder, Nb powder, Ti powder, V powder molar ratio be 1:1:1:1, Ta powder, Nb powder,
The molar ratio of Ti powder, the total amount of V powder and C powder is 1:1.0 ~ 1:1.2;The quality of KCl salt be Ta powder, Nb powder, Ti powder, V powder and
10 ~ 20 times of C powder gross mass.
Further, in the step (1), the hand-ground time is 10 ~ 30 min.
Further, in the step (2), heating rate is 5 ~ 10 DEG C/min in sintering process, and sintering temperature is
1200 ~ 1300 DEG C, soaking time is 30 ~ 90 min, and the flow for being passed through Ar gas is 300 ~ 400 sccm.
Further, in the step (3), the temperature of deionized water is 80 ~ 100 DEG C.
Further, in the step (3), drying temperature is 40 ~ 80 DEG C, and drying time is 2 ~ 5 h.
(Ta, Nb, Ti, V) C high entropy carbide nano powder as made from above-mentioned preparation method.
The preparation method is using Ta powder, Nb powder, Ti powder, V powder and C powder as raw material, using KCl as fused-salt medium, by it
Be mixed in a certain ratio uniformly after under conditions of 1200 ~ 1300 DEG C be heat-treated 30 ~ 90 min, by raw material in fused salt
In directly react (Ta, Nb, Ti, V) C high entropy carbide nano powder be made, then clean removal with hot deionized water
KCl salt finally obtains (Ta, Nb, Ti, V) C high entropy carbide nano powder.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) low in raw material price used by preparation method of the present invention, synthesis temperature is low, equipment requirement is low, production cost
It is low, be conducive to large-scale industrial production;
(2) (Ta, Nb, Ti, V) C high entropy carbide nano powder crystallite dimension of preparation method synthesis of the present invention is small
(average grain size be 80 ~ 90 nm), purity is high and ingredient is uniform, these advantages have this method to develop into big rule
The industrial potentiality of mould.
Detailed description of the invention
Fig. 1 is the XRD spectrum of (Ta, Nb, Ti, V) C high entropy nanometer powder synthesized in embodiment 2;
Fig. 2 is that the SEM figure of (Ta, Nb, Ti, V) C high entropy nanometer powder synthesized in embodiment 2 and EDS can spectral elements point
Butut.
Specific embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiments and drawings, but guarantor of the invention
It protects range and embodiment is without being limited thereto.
In the specific embodiment of the invention, the Ta powder of use, Nb powder, Ti powder, V powder partial size be 1 ~ 3 μm, purity >=
The partial size of 99.5%, C powder is 0.7 ~ 0.9 μm, purity >=99.9%;Used KCl purity salt is that analysis is pure.
Embodiment 1
(1) the C powder of the Ta powder of 0.45 g, the Nb powder of 0.23 g, the Ti powder of 0.12 g, the V powder of 0.13 g, 0.12 g are weighed respectively
It is placed in agate mortar with the KCl salt of 10.50 g and 10 min of hand-ground is uniformly mixed powder, above-mentioned powder is transferred to
In corundum Noah's ark;
(2) Noah's ark is put into atmosphere furnace, vacuumize process is carried out to atmosphere furnace, reaches vacuum degree after vacuumizing 10 min
10-1MPa, fidelity 10 min of sky, observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is intact, this process weight
Again three times.Ar gas is passed through to normal pressure, furnace temperature is risen to 1200 DEG C from room temperature with the heating rate of 5 DEG C/min later, heat preservation 30
min;It is then turned off power supply cooled to room temperature, leads to Ar gas shielded in whole process, the flow of Ar gas is maintained at 300 sccm;
(3) it is filtered after washing obtained mixture in 80 DEG C of deionized water and is put into dry 2 h in 40 DEG C of baking oven and obtained
To target product.(Ta, Nb, Ti, V) C high entropy carbide powder synthesized under this condition is pure phase, and pattern is graininess, is put down
About 85 nm of equal crystallite dimension.
Embodiment 2
(1) the C powder of the Ta powder of 0.45 g, the Nb powder of 0.23 g, the Ti powder of 0.12 g, the V powder of 0.13 g, 0.13 g are weighed respectively
It is placed in agate mortar with the KCl salt of 15.90 g and 20 min of hand-ground is uniformly mixed powder, above-mentioned powder is transferred to
In corundum Noah's ark;
(2) Noah's ark is put into atmosphere furnace, vacuumize process is carried out to atmosphere furnace, reaches vacuum values after vacuumizing 10 min
To 10-1MPa, fidelity 10 min of sky, observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is intact, this process
In triplicate.Ar gas is passed through to normal pressure, furnace temperature is risen to 1250 DEG C from room temperature with the heating rate of 8 DEG C/min later, heat preservation 60
min;It is then turned off power supply cooled to room temperature, leads to Ar gas shielded in whole process, the flow of Ar gas is maintained at 350 sccm;
(3) it is filtered after washing obtained mixture in 90 DEG C of deionized water and is put into dry 4 h in 60 DEG C of baking oven and obtained
To target product.
Fig. 1 is the XRD spectrum of (Ta, Nb, Ti, V) C high entropy carbide powder manufactured in the present embodiment, the map table
Bright, synthesized powder is by single (Ta0.25Nb0.25Ti0.25V0.25) C phase composition, other miscellaneous phases are not found, and institute is in this way
The high entropy carbide nano powder purity of preparation is higher.Fig. 2 is (Ta, Nb, Ti, V) C high entropy carbonization of the present embodiment synthesis
The SEM of powder schemes and EDS power spectrum distribution diagram of element.In Fig. 2 (a) it is found that synthesized in the present embodiment (Ta, Nb,
Ti, V) C high entropy carbide powder be nano-powder, their average grain size is about 80 nm, from EDS energy spectrum analysis
In ((b)-(e) in Fig. 2) synthetic powder, tetra- kinds of metallic elements of Ta, Nb, Ti, V are uniformly distributed.
Embodiment 3
(1) the C powder of the Ta powder of 0.45 g, the Nb powder of 0.23 g, the Ti powder of 0.12 g, the V powder of 0.13 g, 0.14 g are weighed respectively
It is placed in agate mortar with the KCl salt of 25.00 g and 30 min of hand-ground is uniformly mixed powder, above-mentioned powder is transferred to
In corundum Noah's ark;
(2) Noah's ark is put into atmosphere furnace, vacuumize process is carried out to atmosphere furnace, reaches vacuum values after vacuumizing 10 min
To 10-1MPa, fidelity 10 min of sky, observation vacuum meter indicates whether to change, such as unchanged, illustrates that system sealing is intact, this process
In triplicate.Ar gas is passed through to normal pressure, furnace temperature is risen to 1300 DEG C from room temperature with the heating rate of 10 DEG C/min later, heat preservation 90
min;It is then turned off power supply cooled to room temperature, leads to Ar gas shielded in whole process, the flow of Ar gas is maintained at 400 sccm;
(3) it is filtered after washing obtained mixture in 100 DEG C of deionized water and is put into dry 5 h in 80 DEG C of baking oven and obtained
To target product.(Ta, Nb, Ti, V) C high entropy carbide powder synthesized under this condition is pure phase, and pattern is nano particle
Shape, average grain size are about 90 nm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. the preparation method of one kind (Ta, Nb, Ti, V) C high entropy carbide nano powder, which is characterized in that including walking as follows
It is rapid:
(1) by Ta powder, Nb powder, Ti powder, V powder, C powder and KCl ground and mixed;
(2) by mixed powder high temperature sintering, it is passed through Ar gas shielded in sintering process, is cooled to room temperature after the completion of sintering;
(3) mixed powder through oversintering is through deionized water washing, filtering and dry, finally obtain it is described (Ta, Nb, Ti,
V) C high entropy carbide nano powder.
2. preparation method according to claim 1, which is characterized in that in the step (1), Ta powder, Nb powder, Ti powder, V powder
Partial size be 1 ~ 3 μm, purity >=partial size of 99.5%, C powder is 0.7 ~ 0.9 μm, purity >=99.9%.
3. preparation method according to claim 1, which is characterized in that in the step (1), Ta powder, Nb powder, Ti powder, V powder
Molar ratio be 1:1:1:1, Ta powder, Nb powder, Ti powder, V powder total amount and C powder molar ratio be 1:1.0 ~ 1:1.2;KCl salt
Quality is 10 ~ 20 times of Ta powder, Nb powder, Ti powder, V powder and C powder gross mass.
4. preparation method according to claim 1, which is characterized in that in the step (1), milling time is 10 ~ 30
min。
5. preparation method according to claim 1, which is characterized in that in the step (2), heating rate in sintering process
For 5 ~ 10 DEG C/min, sintering temperature is 1200 ~ 1300 DEG C, and soaking time is 30 ~ 90 min, and the flow for being passed through Ar gas is
300 ~ 400 sccm。
6. preparation method according to claim 1, which is characterized in that in the step (3), the temperature of deionized water is 80
~100℃。
7. preparation method according to claim 1, which is characterized in that in the step (3), drying temperature is 40 ~ 80 DEG C,
Drying time is 2 ~ 5 h.
8. (Ta, Nb, Ti, V) C high entropy carbide nanometer powder made from the described in any item preparation methods of claim 1-7
Body.
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Cited By (5)
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CN112851352A (en) * | 2021-01-27 | 2021-05-28 | 陕西科技大学 | Ultrahigh-temperature high-entropy carbide powder and preparation method thereof |
CN113548898A (en) * | 2021-08-19 | 2021-10-26 | 郑州大学 | (Mo)0.2W0.2V0.2Cr0.2Ni0.2) B high-entropy ceramic powder and preparation method thereof |
CN113716580A (en) * | 2021-08-15 | 2021-11-30 | 吉林大学 | High-entropy boride micro-nano ceramic particle and preparation method thereof |
CN114180965A (en) * | 2021-12-27 | 2022-03-15 | 安徽工业大学 | High-entropy carbide nano powder material with high sphericity and high activity, and preparation method and application thereof |
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CN112441837A (en) * | 2020-12-09 | 2021-03-05 | 安徽工业大学 | High-performance (VNbTaMoW) C high-entropy carbide ceramic and preparation method thereof |
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CN113716580A (en) * | 2021-08-15 | 2021-11-30 | 吉林大学 | High-entropy boride micro-nano ceramic particle and preparation method thereof |
CN113548898A (en) * | 2021-08-19 | 2021-10-26 | 郑州大学 | (Mo)0.2W0.2V0.2Cr0.2Ni0.2) B high-entropy ceramic powder and preparation method thereof |
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