CN112851352A - Ultrahigh-temperature high-entropy carbide powder and preparation method thereof - Google Patents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped 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
- C04B35/56—Shaped 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
- C04B35/5607—Shaped 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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses an ultrahigh-temperature high-entropy carbide powder and a preparation method thereofxC, wherein M is 4-5 of Zr, Ti, Hf, Mo, Ta and Nb, wherein x is more than 5% and less than 35%; the invention combines the citric acid complexing sol-gel method with the ball milling mixing technology, and is obtained after high-temperature heat treatment, the chemical reaction in the liquid phase can obtain the mixing at the molecular level in a short time, the precise control of the chemical proportion of the material is easy to realize, the preparation process is simple, the synthesis temperature is low, and the cost is low; the prepared high-entropy carbide powder has the advantages of small particle size, high purity and the like.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to ultrahigh-temperature high-entropy carbide powder and a preparation method thereof.
Background
Under the extremely severe environmental service conditions of hypersonic long-time flight, atmosphere reentry, atmospheric layer crossing flight, rocket propulsion system and the like of a new generation of aircraft, and the background of strong requirements on high-performance heat-proof materials of nose cones, wing leading edges, engine hot-end parts and the like of the aircraft, the existing mature materials are difficult to meet the application requirements.
The term "high entropy" appears in multi-principal element high entropy alloy materials provided by professor of Taiwan scholars in leaf-yu in the 90 s of the 20 th century for the first time, and a great deal of research shows that the high entropy alloy has more excellent physical and chemical properties than common alloys. The high-entropy carbide serving as a novel ultrahigh-temperature ceramic material has the characteristics of high melting point, high hardness, excellent thermal conductivity and electric conductivity, thermal shock resistance and the like, and has great potential in the fields of ultrahigh temperature, aerospace propulsion, energy and the like.
Lefei et al, university of east China, published the document "Liquid precursor-derived high-entry copy nanoparticles [ J]Ceramics International,2019,45(17): 22437-. The high-entropy carbide liquid-phase precursor is obtained by a sol-gel reaction between transition metal salt and an organic carbon source, wherein all components are uniformly mixed at a molecular level, and the high-entropy carbide liquid-phase precursor is obtained by drying and high-temperature heat treatment. The raw materials of partial chlorides used by the high-entropy carbide ceramic prepared by the method are expensive, and the wide application of the high-entropy carbide ceramic is not facilitated. The Chu Yan of the university of south China published the document "First-principles study, failure, and characterization of (Hf)0.2Zr0.2Ta0.2Nb0.2Ti0.2)C high-entropy ceramic[J]Journal of the American Ceramic Society,2019,102(7): 4344-4352 "and patent CN 108911751A disclose a ZrHfTaNbTiC ultra-high temperature high entropy Ceramic material. The high-entropy ceramic material consists of Zr, Hf, Ta, Nb, Ti and C elements and has a single rock-salt phase structure. The high-entropy ceramic material is prepared by ball-milling five carbides to obtain a uniformly mixed suspension, and then sintering at high temperature and high pressure. However, the ball milling method introduces a large amount of impurity elements, and the raw materials are expensive, so that the wide application of the ball milling method is limited. Chen Lei's hair of Harbin industry universityTABLE "microstuctures and mechanical properties of (TiZrNbTaMo) C high-entry ceramic [ J]Journal of Materials Science and Technology,2020,39: 99-105 and patent CN 110330341 a disclose a transition metal carbide single-phase high-entropy ceramic powder and a preparation method thereof. And (2) mixing the metal oxide and the reductive carbon powder, then carrying out high-energy ball milling to obtain mixed powder, putting the mixed powder into a graphite crucible, calcining under a vacuum condition, and sieving to obtain the single-phase high-entropy ceramic powder of the transition metal carbide. The carbothermic reduction process needs to regulate and control parameters such as synthesis temperature, vacuum degree and the like, and the used oxide raw material has poor activity, so that the powder synthesis temperature is up to 2200 ℃.
Disclosure of Invention
In order to avoid the defects of the technology, the invention aims to provide the ultrahigh-temperature high-entropy carbide powder with simple preparation process and low synthesis temperature and the preparation method thereof, and the prepared high-entropy carbide powder has the advantages of small particle size, high purity and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
the superhigh temperature high entropy carbide powder is single phase solid solution with rock salt phase structure and molecular formula of MxC, wherein M is 4-5 of Zr, Ti, Hf, Mo, Ta and Nb, and x is more than 5% and less than 35%.
The preparation method of the ultrahigh-temperature high-entropy carbide powder comprises the following steps:
(1) mixing 2-3 transition metal salts of Mo, Zr and Ti, polyethylene glycol and a carbon source, obtaining a liquid-phase precursor by a citric acid complexing sol-gel method, mixing and ball-milling the liquid-phase precursor and 2-3 transition metal oxide powders of Ta, Hf and Nb, then carrying out water bath gelation, and drying to obtain dry gel;
(2) and grinding and tabletting the obtained xerogel, and then carrying out heat treatment at 1500-2000 ℃ in a protective atmosphere to obtain single-phase ultrahigh-temperature high-entropy carbide powder.
Further, the liquid phase precursor in the step (1) is synthesized by mixing citric acid and transition metal ions in the transition metal salt according to the molar ratio of 1 (1-5), adding polyethylene glycol according to the mass ratio of (1-8) to 1 of citric acid to polyethylene glycol, adding a carbon source according to the molar ratio of 1:1 of the carbon source to the transition metal ions in the transition metal salt, adding 2-10% more carbon source, and adjusting the pH of the sol to 3-8 by ammonia water. .
Further, in the water bath gelation process in the step (1), the liquid-phase precursor and the transition metal oxide powder are subjected to ultrasonic dispersion and ball milling, so that the liquid-phase precursor and the transition metal oxide powder are uniformly mixed, and then water bath gelation is performed, so that the transition metal oxide powder is uniformly distributed in the gel.
Further, the temperature of the water bath gelation reaction is 60-90 ℃, and the stirring time is 5-15 h.
Further, the drying temperature in the step (1) is 60-80 ℃.
Further, the transition metal salt is an oxychlorination salt, an ammonium salt or a sulfate of a transition metal.
Further, the carbon source is one or more of sucrose, fructose, glucose, furfuryl alcohol resin and phenolic resin.
Compared with the prior art, the invention has the following technical effects:
the molecular formula of the high-entropy carbide powder is MxAnd C is a single-phase solid solution and has a rock salt phase structure. Part of transition metal inorganic salt is complexed with citric acid to create liquid phase condition to reduce synthesis temperature, and part of metal is selected from its oxide to reduce cost.
The invention adopts citric acid as complexing agent, which has complexing effect with metal ions to form chain structure. The ionization degree of citric acid is increased by adding ammonia water dropwise, so that the complex reaction of citric acid and metal ions is promoted. Polyethylene glycol is firstly used as an additive, has a wrapping effect on colloidal particles, and prevents the colloidal particles from excessively growing. And secondly, hydroxyl in the polyethylene glycol structure reacts with carboxyl of citric acid to form a ring network structure, which is favorable for stabilizing sol.
The invention is obtained by uniformly mixing oxide powder and liquid phase precursor by ball milling mixing technology, stirring in water bath, and performing high temperature heat treatment. The chemical reaction in liquid phase can obtain molecular level mixture in short time, and has easy control of chemical compounding ratio, simple preparation process, low synthesis temperature (1550-1850 deg.c) and low cost.
The high-entropy carbide powder prepared by the invention has the advantages of small particle size, high purity and the like.
Drawings
FIG. 1 is an XRD picture of (ZrTiTaNb) C high-entropy carbide powder obtained in example 1
FIG. 2 is an XRD picture of (ZrTiTaNbHf) C high-entropy carbide powder obtained in example 3
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1
(1) 2.8102gZrOCl is weighed according to the molar ratio of the metal elements being 1:1 respectively2·8H2O、2.1819gTi(SO4)2Dissolving in deionized water, weighing 1.2655g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions being 1:3, dissolving in the deionized water, adding the above solutions respectively, and mixing the two solutions.
(2) 0.3021g of polyethylene glycol is weighed according to the mass ratio of the polyethylene glycol to citric acid monohydrate of 1:5, and then dissolved in deionized water, and the solution is added. 4.0312g of glucose was weighed out and dissolved in deionized water and added to the above solution to form a sol. And its pH was adjusted to 6 using ammonia.
(3) 1.9167g of tantalum oxide and 1.1529g of niobium oxide were weighed out in a molar ratio of metal element in oxide to metal element of inorganic salt in step 1 of 1: 1. Adding the sol, ball-milling for 13h, carrying out water bath, uniformly wrapping oxide particles in gel in the gelation process of the water bath at 60 ℃, then placing the obtained wet gel in an oven at 80 ℃ for drying, grinding into powder and tabletting. And (3) placing the pressed sheet in a tubular furnace for carrying out 1550 ℃ heat treatment for 3h to finally obtain the single-phase (ZrTiTaNb) C high-entropy carbide.
Example 2
(1) Respectively according to the metal2.3588gZrOCl is weighed according to the element molar ratio of 1:12·8H2O、1.7569gTi(SO4)2Dissolving in deionized water, mixing, weighing 1.1235g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions of 1:5, dissolving in the deionized water, adding the above solution to precipitate, and adding a proper amount of ammonia water to remove the precipitate.
(2) 0.3426g of polyethylene glycol is weighed according to the mass ratio of the polyethylene glycol to citric acid monohydrate of 1:1, then dissolved in deionized water, and precipitation appears after the solution is added.
Example 3
(1) 1.9787gZrOCl is weighed according to the molar ratio of the metal elements being 1:1 respectively2·8H2O、1.4737gTi(SO4)2Dissolving in deionized water, weighing 0.8602g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions being 1:3, dissolving in the deionized water, adding the above solutions respectively, and mixing the two solutions.
(2) 0.1852 of polyethylene glycol is weighed according to the mass ratio of the polyethylene glycol to the citric acid monohydrate of 1:5, and then dissolved in deionized water, and the solution is added. 3.4070g of glucose was weighed out and dissolved in deionized water and added to the above solution to form a sol. And its pH was adjusted to 8 using ammonia.
(3) 1.3567g of tantalum oxide, 0.8161g of niobium oxide and 1.2925g of hafnium oxide were weighed out in a molar ratio of metal elements in the oxide to metal elements of the inorganic salt in step 1 of 1: 1. Adding the sol, ball-milling for 13h, carrying out water bath, uniformly wrapping oxide particles in gel in the water bath gelation process at 80 ℃, drying the obtained wet gel in an oven at 80 ℃, grinding into powder, and tabletting. And (3) carrying out heat treatment on the pressed sheet at 1850 ℃ for 1h to finally obtain the single-phase (ZrTiTaNbHf) C high-entropy carbide.
Example 4
(1) 1.9335gZrOCl is weighed according to the molar ratio of the metal elements being 1:1 respectively2·8H2O、1.4401gTi(SO4)2And 1.0593g (NH)4)6Mo7O24·4H2Dissolving O in deionized water, weighing 0.5161g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions being 1:5, dissolving in deionized waterAdding the above solutions into water, and mixing.
(2) 0.2580g of polyethylene glycol was weighed out in a mass ratio of 1:2 to citric acid monohydrate, and dissolved in deionized water, and added to the above solution to form a precipitate. After the precipitate disappeared after the addition of ammonia water, 3.3352g of glucose was weighed and dissolved in deionized water, and added to the above solution to form a sol. And its pH was adjusted to 3 using ammonia water.
(3) 1.3257g of tantalum oxide and 1.2629g of hafnium oxide were weighed out in a molar ratio of metal element in oxide to metal element of inorganic salt in step 1 of 1: 1. Adding the sol, ball-milling for 5h, performing water bath, uniformly wrapping oxide particles in the gel in the water bath gelation process at 90 ℃, forming a precipitate in the water bath process, and obtaining the non-uniform gel. And then the obtained wet gel is placed in an oven at 70 ℃ for drying, ground into powder and then tabletted. The pressed sheet was heat treated at 1500 ℃ for 2 h.
(4) Analysis of this by XRD revealed that the material was not a single-phase high entropy carbide.
Example 5
(1) 2.2658gZrOCl is weighed according to the molar ratio of the metal elements being 1:1 respectively2·8H2O、1.6876gTi(SO4)2And 1.2414g (NH)4)6Mo7O24·4H2Dissolving O in deionized water, weighing 0.1642g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions of 1:1, dissolving in the deionized water, adding the above solutions respectively, and mixing the three solutions.
(2) 0.2955g of polyethylene glycol is weighed according to the mass ratio of the polyethylene glycol to citric acid monohydrate of 1:5, and then dissolved in deionized water, and the solution is added. 4.0234g of glucose was weighed out and dissolved in deionized water and added to the above solution to form a sol. And its pH was adjusted to 5 using ammonia water.
(3) 1.5535g of tantalum oxide and 0.9345g of niobium oxide were weighed out in a molar ratio of metal element in oxide to metal element of inorganic salt in step 1 of 1: 1. Adding the sol, ball-milling for 15h, carrying out water bath, uniformly wrapping oxide particles in gel in the water bath gelation process at 75 ℃, then placing the obtained wet gel in a 60 ℃ oven for drying, grinding into powder, and tabletting. The pressed sheet was heat treated at 2000 ℃ for 1 h.
(4) Analysis of the high-entropy carbide by XRD shows that the synthesized high-entropy carbide is not a single rock-salt phase structure and contains two phases.
Example 6
(1) 2.7952gZrOCl is weighed according to the molar ratio of the metal elements being 1:1 respectively2·8H2O、2.0819gTi(SO4)2Dissolving in deionized water, weighing 2.4806g of citric acid monohydrate according to the molar ratio of the citric acid monohydrate to the metal ions being 1:2, dissolving in the deionized water, adding the above solutions respectively, and mixing the two solutions.
(2) 4.9612g of polyethylene glycol was weighed out in a mass ratio of 1:8 to citric acid monohydrate, and dissolved in deionized water, and added to the above solution to form a precipitate.
Both example 1 and example 3 gave single-phase high-entropy carbide powders, the XRD results of which are shown in fig. 1 and 2.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (8)
1. The ultrahigh-temperature high-entropy carbide powder is characterized in that: the carbide powder is single-phase solid solution, has rock salt phase structure, and has molecular formula of MxC, wherein M is 4-5 of Zr, Ti, Hf, Mo, Ta and Nb, and x is more than 5% and less than 35%.
2. The method for preparing ultra-high temperature high entropy carbide powder of claim 1, comprising the steps of:
(1) mixing 2-3 transition metal salts of Mo, Zr and Ti, polyethylene glycol and a carbon source, obtaining a liquid-phase precursor by a citric acid complexing sol-gel method, mixing and ball-milling the liquid-phase precursor and 2-3 transition metal oxide powders of Ta, Hf and Nb, then carrying out water bath gelation, and drying to obtain dry gel;
(2) and grinding and tabletting the obtained xerogel, and then carrying out heat treatment at 1500-2000 ℃ for 1-3h under a protective atmosphere to obtain single-phase ultrahigh-temperature high-entropy carbide powder.
3. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: the synthesis method of the liquid phase precursor in the step (1) comprises the steps of mixing citric acid and transition metal ions in transition metal salt according to the molar ratio of 1 (1-5), adding polyethylene glycol according to the mass ratio of (1-8) to 1 of citric acid to polyethylene glycol, adding a carbon source according to the molar ratio of 1:1 of the carbon source to the transition metal ions in the transition metal salt, adding 2-10% more carbon source, and adjusting the pH value of the sol to 3-8 through ammonia water.
4. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: and (2) in the water bath gelation process in the step (1), performing ultrasonic dispersion on the liquid-phase precursor and the transition metal oxide powder, performing ball milling, uniformly mixing the liquid-phase precursor and the transition metal oxide powder, and performing water bath gelation to uniformly distribute the transition metal oxide powder in the gel.
5. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: the water bath gelation reaction temperature is 60-90 ℃, and the stirring time is 5-15 h.
6. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: the drying temperature in the step (1) is 60-80 ℃.
7. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: the transition metal salt is an oxychlorination salt, an ammonium salt or a sulfate of transition metal.
8. The method for preparing ultra-high temperature high entropy carbide powder according to claim 2, characterized in that: the carbon source is one or more of sucrose, fructose, glucose, furfuryl alcohol resin and phenolic resin.
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| CN114315370A (en) * | 2022-01-17 | 2022-04-12 | 哈尔滨工业大学 | Method for synthesizing (TiZrHfNbTa) CN high-entropy ultrahigh-temperature carbonitride ceramic powder |
| CN115073183A (en) * | 2022-06-27 | 2022-09-20 | 山东大学 | High-entropy boride nano powder and sol-gel preparation method thereof |
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Application publication date: 20210528 |