CN110698201A - Ceramic and preparation method thereof - Google Patents
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Abstract
A ceramic and a method for preparing the same, wherein the ceramic comprises: rare earth elements and metal elements; the molar ratio of the rare earth element to the metal element is 1: 1; the rare earth elements comprise dysprosium, ytterbium, holmium, yttrium and gadolinium; the metal element is niobium, or the metal element is niobium and tantalum. According to the technical scheme, 5 different rare earth elements and niobium or niobium and tantalum are adopted, and the prepared rare earth tantalum niobate ceramic and niobate ceramic is high in hardness and toughness and overcomes the contradiction between high hardness and high toughness.
Description
Technical Field
The invention relates to the technical field of high-entropy ceramics, in particular to a ceramic and a preparation method thereof.
Background
"high entropy" is a new material design theory appearing in recent years, and has become a big hot spot in the field of material research, and the concept of the high entropy alloy is originally developed. With the continuous deepening of research, the concept of high entropy is gradually expanded to other materials, the high entropy ceramic is one of the materials, the high entropy ceramic is a novel ceramic appearing in recent years, the research is less at present, but the high entropy ceramic is concerned by researchers due to the unique characteristics of the high entropy ceramic, the high entropy ceramic belongs to a multi-principal-element high entropy material, the high entropy ceramic is a novel material provided based on the design idea of 'multiple high chaos', the high entropy ceramic has the advantages of high strength, high hardness, corrosion resistance, wear resistance, good high-temperature thermal stability and the like, and the high entropy ceramic is used for fighting eyes in many fields at present, such as ultrahigh temperature, high corrosion resistance, energy and the like, and has great application value.
The research on the high-entropy ceramics can be traced back to 2015 for the earliest time, and due to the short research time, the preparation method of the high-entropy ceramics is still in the exploration stage at present, and the preparation method of the high-entropy ceramics mainly comprises the following steps: a spray granulation method; a magnetron sputtering method; ball milling method combined with heat treatment; a method in which a high-energy ball milling method and a discharge plasma are combined, or the like; however, the ceramics prepared by these methods are often not dense enough, cracks are easily generated in the ceramics when stressed, and materials with high hardness are often not good in toughness, while materials with good toughness are lower in hardness.
Disclosure of Invention
Objects of the invention
The invention aims to provide a high-entropy ceramic with high hardness and high toughness and a preparation method thereof.
(II) technical scheme
To solve the above problems, a first aspect of the present invention provides a ceramic comprising: rare earth elements and metal elements; the molar ratio of the rare earth element to the metal element is 1: 1; the rare earth elements comprise dysprosium, ytterbium, holmium, yttrium and gadolinium; the metal element is niobium, or the metal element is niobium and tantalum.
Further, the metal elements are the niobium and the tantalum; (ii) a The molar ratio of niobium to tantalum is in the range of 2:8 to 8: 2.
Further, the metal elements are the niobium and the tantalum; the molar ratio of the rare earth element, the niobium and the tantalum is 5:2.5: 2.5.
Further, the molar ratio of dysprosium, ytterbium, holmium, yttrium to gadolinium is 1:1:1: 1.
Another aspect of the present invention provides a method for preparing the above ceramic, comprising: dropwise adding the mixed solution containing the raw materials with the preset molar ratio into ammonia water to obtain precipitated colloid; centrifuging the precipitation colloid to obtain a precipitate; drying the precipitate; grinding the dried precipitate into powder; pre-crystallizing and sintering the powder; grinding and sieving the pre-crystallized and sintered powder again and pressing to obtain a compact block; and sintering the compact block at a high temperature to obtain the ceramic.
Further, the method for preparing the mixed solution containing the raw materials at the predetermined molar ratio includes: weighing raw material powder containing rare earth elements in a preset molar ratio, and dissolving the raw material powder with deionized water to obtain a dissolved solution; weighing niobium pentachloride with a preset content, or mixing the niobium pentachloride and the tantalum pentachloride with absolute ethyl alcohol to obtain a mixed solution; and mixing the dissolved solution and the mixed solution, and uniformly stirring to obtain a mixed solution.
Further, the rare earth element powder includes DyCl3∙6H2O、YbCl3∙6H2O、HoCl3∙6H2O、Y(NO3)3∙6H2O、GdCl3∙6H2O。
Further, the PH of the ammonia is > 10.
Further, the drying temperature of the drying treatment is 80-110 ℃, and the time is 12-24 hours.
Further, the sintering temperature of the pre-crystallization sintering is 1000-1200 ℃, and the sintering time is 5-10 h.
Furthermore, the sintering temperature of the high-temperature sintering is 1500-1600 ℃, and the sintering time is 10-20 h.
Further, the screening mesh is 300-500 meshes.
Further, pressing the sieved powder by using a press, wherein the pressure of the press is 300-400 MPa, and the pressing time is 10-20 min. .
(III) advantageous effects
The technical scheme of the invention has the following beneficial technical effects:
1. according to the technical scheme, 5 different rare earth elements and niobium or niobium and tantalum are adopted, and the prepared rare earth tantalum niobate ceramic and niobate ceramic is high in hardness and greatly improved in toughness, so that the contradiction between high hardness and high toughness is overcome;
2. the tantalum niobate ceramic and niobate ceramic prepared by the technical scheme of the application have low internal porosity and certain iron elasticity, so that the toughness of the high-entropy rare earth tantalum niobate and niobate is improved, specifically, due to the existence of the iron elasticity, a domain wall (a transition layer between two adjacent iron elastic domains) deflects under the action of external force, and absorbs certain strain energy, so that the expansion of microcracks is slowed down, and the toughness of the material is enhanced.
Drawings
FIG. 1 is an XRD spectrum of the ceramic of example 1;
FIG. 2 is an impression of the ceramic of example 1 using a micro Vickers hardness tester;
FIG. 3 is an XRD spectrum of the ceramic of example 2;
FIG. 4 is an impression of the ceramic of example 2 using a micro Vickers hardness tester;
FIG. 5 is a flow chart of a method of preparing the ceramic of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The present invention provides a ceramic comprising: rare earth elements, tantalum and niobium; the molar ratio of the rare earth element to the tantalum and niobium or the niobium is 1: 1; the rare earth elements include dysprosium, ytterbium, holmium, yttrium and gadolinium.
The ceramic of the invention adopts 5 different rare earth materials, and the prepared rare earth tantalum niobate ceramic and niobate ceramic not only have high hardness and greatly improved toughness, but also overcome the contradiction between high hardness and high toughness.
In addition, the five rare earth elements are selected, so that the five rare earth elements have small radius, and are favorable for forming a pure high-entropy toughened tantalum niobate phase or niobate phase, and the 5 rare earth elements can be used for improving the chaos degree of the prepared ceramic material, so that the ceramic has higher entropy.
Preferably, the molar ratio of niobium to tantalum is in the range of 2:8 to 8: 2.
Preferably, the molar ratio of niobium to tantalum is 5:2.5: 2.5.
Preferably, the molar ratio of dysprosium, ytterbium, holmium, yttrium to gadolinium is 1:1:1: 1.
The preparation method provided by the invention is used for preparing the ceramic, as shown in fig. 5, the ceramic is prepared by high-temperature sintering through a powder metallurgy method, and the preparation method comprises the following steps: dropwise adding the mixed solution containing the raw materials with the preset molar ratio into ammonia water to obtain precipitated colloid; centrifuging the precipitation colloid to obtain a precipitate; drying the precipitate; grinding the dried precipitate into powder; pre-crystallizing and sintering the powder; grinding and sieving the pre-crystallized and sintered powder again and pressing to obtain a compact block; and sintering the compact block at a high temperature to obtain the ceramic.
The tantalum niobate ceramic and niobate ceramic prepared by the technical scheme of the application have low internal porosity and certain iron elasticity, so that the toughness of the high-entropy rare earth tantalum niobate and niobate is improved, specifically, due to the existence of the iron elasticity, a domain wall (a transition layer between two adjacent iron elastic domains) deflects under the action of external force, and absorbs certain strain energy, so that the expansion of microcracks is slowed down, the toughness of the material is enhanced, and the ceramic has high hardness and high toughness.
Pre-crystallization sintering, the precipitate prepared by a chemical coprecipitation method is not crystal, and the purpose of pre-sintering is to sinter the compound at high temperature to generate crystal. Pre-crystallizing and sintering to generate crystals, and sintering at high temperature to obtain the desired tantalum niobate phase or niobate phase.
Preferably, the method for preparing the mixed solution containing the raw materials at the predetermined molar ratio includes: weighing raw material powder containing rare earth elements in a preset molar ratio, and dissolving the raw material powder with deionized water to obtain a dissolved solution; weighing niobium pentachloride with a preset content, or mixing the niobium pentachloride and the tantalum pentachloride with absolute ethyl alcohol to obtain a mixed solution; and mixing the dissolved solution and the mixed solution, and uniformly stirring to obtain a mixed solution. Dissolving raw material powder containing rare earth elements by deionized water and dissolving tantalum pentachloride and niobium pentachloride by absolute ethyl alcohol, mixing the solutions, and then stirring the solutions to ensure that all the elements are uniformly mixed.
Preferably, the purity of the used raw material powder containing rare earth elements and tantalum pentachloride and niobium pentachloride materials is not less than 99.95%, and a powder raw material with higher purity is adopted to reduce the content of introduced impurity elements, avoid the introduction of the impurity elements into crystals to form micro cracks and reduce the compactness of a finally sintered block.
Preferably, the rare earth element powder includes DyCl3∙6H2O、YbCl3∙6H2O、HoCl3∙6H2O、Y(NO3)3∙6H2O、GdCl3∙6H2O。
Preferably, the ammonia has a PH > 10. The mixed solution is in the alkaline solution atmosphere to generate the compound precipitation.
Preferably, the drying temperature of the drying treatment is 80-110 ℃, and the time is 12-24 h.
Preferably, the sintering temperature of the pre-crystallization sintering is 1000-1200 ℃, and the sintering time is 5-10 h.
Preferably, the sintering temperature of the high-temperature sintering is 1500-1600 ℃, the sintering time is 10-20 hours, and the tantalum niobate or niobate can reach the phase transition point within the temperature range of 1500-1600 ℃, so that the single-phase ceramic material is obtained.
Preferably, the screening mesh is 300-500 meshes. The powder has similar particle size, better adhesion among the powders and easier obtaining of compact blocks during pressing.
Preferably, the sieved powder is pressed by a press, wherein the pressure of the press is 300-400 MPa, and the pressing time is 10-20 min. So that the gas in the powder is less during sintering, and a compact blank is obtained.
Example 1
FIG. 1 is an XRD spectrum of the ceramic of example 1; FIG. 2 is an impression of the ceramic of example 1 using a micro Vickers hardness tester.
As shown in fig. 1 and 2, the present example provides a ceramic and a method for preparing the same, wherein the ceramic comprises the rare earth elements of tantalum and niobium, the molar ratio of the rare earth elements to the niobium is 1:1, and the rare earth elements are dysprosium, ytterbium, holmium, yttrium and gadolinium; the molar ratio of dysprosium, ytterbium, holmium, yttrium to gadolinium is 1:1:1: 1. Obtaining the high-entropy rare earth toughened niobate ceramic.
The preparation method provided by the embodiment comprises the following steps:
s1: weighing the mole ratio of rare earth elements dysprosium, ytterbium, holmium, yttrium and gadolinium to be 1:1:1:1, and DyCl3∙6H2O、YbCl3∙6H2O、HoCl3∙6H2O、Y(NO3)3∙6H2O、GdCl3∙6H2Dissolving O powder in deionized water to obtain a solution; mixing niobium pentachloride with absolute ethyl alcohol to obtain a mixed solution; mixing the dissolved solution and the mixed solution, and uniformly stirring to obtain a mixed solution, wherein the ratio of the sum of the mole numbers of the 5 rare earth elements to the mole number of niobium is 1: 1;
s2: dropwise adding the mixed solution into ammonia water with the pH value of more than 10 to obtain precipitated colloid;
s3: centrifuging the precipitation colloid to obtain a precipitate;
s4: drying the precipitate at the temperature of 80-110 ℃ for 12-24 h;
s5: grinding the dried precipitate by using an agate grinding pot into powder;
s6: pre-crystallizing and sintering the powder obtained in the step S5, wherein the sintering temperature is 1000-1200 ℃, and the sintering time is 5-10 h;
s7: and grinding and sieving the pre-crystallized and sintered powder again, and pressing to obtain a compact block, wherein the sieving mesh is 300-500 meshes, the pressure of the press is 300-400 MPa, and the pressing time is 10-20 min.
S8: and sintering the compact block at high temperature, wherein the sintering temperature is 1500-1600 ℃, and the sintering time is 10-20 h, so as to obtain the ceramic, and the expression of the ceramic is Y1/5 Gd 1/5 Dy 1/5 Yb1/5 Ho 1/5) NbO 4.
The ceramic of example 1 was examined with an X-ray diffractometer and the XRD pattern obtained is shown in fig. 1, where the diffraction peaks in the XRD test results of the ceramic samples correspond to the standard peaks of its standard PDF card JCPDS: No.23-1486, one-to-one, and no second phase diffraction peaks exist, indicating that the prepared ceramic material has a single-phase crystal structure and no impurity phase.
The hardness of the ceramic of example 1 was measured using a micro vickers hardness tester, and the results are shown in fig. 2, and then the fracture toughness of the material was calculated from the diagonal length of the indentation and the crack lengths of the four corners.
The involved formula is that Vickers hardness:
(in GPa), wherein Hv represents the Vickers hardness of the high-entropy ceramic, and F and d refer to the test applied load and the indentation diagonal length, respectively. Fracture toughness: kIC＝0.0725*(P/c3/2) (unit MPa. m)1/2) Where P represents the test applied load and c represents the average crack length. The Vickers hardness of the obtained product is 3.61GPa, and the fracture toughness is 4.90MPa1/2。
Example 2
FIG. 3 is an XRD spectrum of the ceramic of example 2; FIG. 4 is an impression of the ceramic of example 2 using a micro Vickers hardness tester.
As shown in fig. 3 and 4, the present example provides a ceramic and a method for preparing the same, wherein the ceramic includes rare earth elements, niobium and tantalum, the molar ratio of the rare earth elements, the niobium and the tantalum is 5:2.5:2.5, and the rare earth elements are dysprosium, ytterbium, holmium, yttrium and gadolinium; the molar ratio of dysprosium, ytterbium, holmium, yttrium to gadolinium is 1:1:1: 1. Obtaining the high-entropy rare earth toughened tantalum niobate ceramic.
The preparation method provided by the embodiment comprises the following steps:
s1: weighing the mole ratio of rare earth elements dysprosium, ytterbium, holmium, yttrium and gadolinium to be 1:1:1:1, and DyCl3∙6H2O、YbCl3∙6H2O、HoCl3∙6H2O、Y(NO3)3∙6H2O、GdCl3∙6H2Dissolving O powder in deionized water to obtain a solution; mixing niobium pentachloride and tantalum pentachloride with absolute ethanol to obtain a mixed solution; mixing the dissolving solution and the mixed solution, and uniformly stirring to obtain a mixed solution, wherein the mole number of the 5 rare earth elements and the mole ratio of the niobium to the tantalum are 5:2.5: 2.5;
s2: dropwise adding the mixed solution into ammonia water with the pH value of more than 10 to obtain precipitated colloid;
s3: centrifuging the precipitation colloid to obtain a precipitate;
s4: drying the precipitate at the temperature of 80-110 ℃ for 12-24 h;
s5: grinding the dried precipitate by using an agate grinding pot into powder;
s6: pre-crystallizing and sintering the powder obtained in the step S5, wherein the sintering temperature is 1000-1200 ℃, and the sintering time is 5-10 h;
s7: and grinding and sieving the pre-crystallized and sintered powder again, and pressing to obtain a compact block, wherein the sieving mesh is 300-500 meshes, the pressure of the press is 300-400 MPa, and the pressing time is 10-20 min.
S8: and (3) sintering the compact block at high temperature, wherein the sintering temperature is 1500-1600 ℃, and the sintering time is 10-20 h, so as to obtain the ceramic, and the expression of the ceramic is (Y1/5 Gd 1/5 Dy 1/5 Yb1/5 Ho 1/5) (Ta 1/2 Nb 1/2) O4.
The hardness of the ceramic of example 1 was measured using a micro vickers hardness tester, and the results are shown in fig. 4, and then the fracture toughness of the material was calculated from the diagonal length of the indentation and the crack lengths of the four corners.
The involved formula is that Vickers hardness:
(in GPa), wherein Hv represents the Vickers hardness of the high-entropy ceramic, and F and d refer to the test applied load and the indentation diagonal length, respectively. Fracture toughness: kIC＝0.0725*(P/c3/2) (unit MPa. m)1/2) Where P represents the test applied load and c represents the average crack length. The Vickers hardness of the obtained product is 4.36GPa, and the fracture toughness is 3.38MPa1/2。
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (10)
1. A ceramic, comprising: rare earth elements and metal elements;
the molar ratio of the rare earth element to the metal element is 1: 1;
the rare earth elements comprise dysprosium, ytterbium, holmium, yttrium and gadolinium;
the metal element is niobium, or the metal element is niobium and tantalum.
2. The ceramic of claim 1,
the metal elements are the niobium and the tantalum;
the molar ratio of niobium to tantalum is in the range of 2:8 to 8: 2.
3. The ceramic of claim 1,
the metal elements are the niobium and the tantalum;
the molar ratio of the rare earth element, the niobium and the tantalum is 5:2.5: 2.5.
4. The ceramic according to any one of claims 1 to 3,
the molar ratio of dysprosium, ytterbium, holmium, yttrium to gadolinium is 1:1:1: 1.
5. A method for producing a ceramic, which is used for producing the ceramic according to any one of claims 1 to 4, comprising:
dropwise adding the mixed solution containing the raw materials with the preset molar ratio into ammonia water to obtain precipitated colloid;
centrifuging the precipitation colloid to obtain a precipitate;
drying the precipitate;
grinding the dried precipitate into powder;
pre-crystallizing and sintering the powder;
grinding and sieving the pre-crystallized and sintered powder again and pressing to obtain a compact block;
and sintering the compact block at a high temperature to obtain the ceramic.
6. The method for producing a ceramic according to claim 5,
the preparation method of the mixed solution containing the raw materials in the preset molar ratio comprises the following steps:
weighing raw material powder containing rare earth elements in a preset molar ratio, and dissolving the raw material powder with deionized water to obtain a dissolved solution;
weighing niobium pentachloride with a preset content, or mixing the niobium pentachloride and the tantalum pentachloride with absolute ethyl alcohol to obtain a mixed solution;
and mixing the dissolved solution and the mixed solution, and uniformly stirring to obtain a mixed solution.
7. The method for producing a ceramic according to claim 6,
the rare earth element powder comprises DyCl3∙6H2O、YbCl3∙6H2O、HoCl3∙6H2O、Y(NO3)3∙6H2O、GdCl3∙6H2O。
8. The method for preparing the ceramic according to claim 5, wherein the sintering temperature of the pre-crystallization sintering is 1000 to 1200 ℃, and the sintering time is 5 to 10 hours.
9. The method for preparing the ceramic according to claim 5, wherein the sintering temperature of the high-temperature sintering is 1500-1600 ℃, and the sintering time is 10-20 h.
10. The method for preparing ceramic according to claim 5, wherein the sieve mesh is 300-500 mesh.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685165A (en) * | 2022-04-08 | 2022-07-01 | 桂林理工大学 | High-entropy oxide ceramic with ten-component brown yttrium niobium ore structure and preparation method thereof |
| CN114933477A (en) * | 2022-04-28 | 2022-08-23 | 昆明理工大学 | High-toughness phase-change-free niobate ceramic and preparation method thereof |
| CN114956814A (en) * | 2022-05-16 | 2022-08-30 | 昆明理工大学 | High-entropy tantalum/niobium ceramic with high sintering resistance, high CMAS corrosion resistance and preparation method thereof |
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| CN114685165A (en) * | 2022-04-08 | 2022-07-01 | 桂林理工大学 | High-entropy oxide ceramic with ten-component brown yttrium niobium ore structure and preparation method thereof |
| US11673839B1 (en) | 2022-04-08 | 2023-06-13 | Guilin University Of Technology | Ten-membered fergusonite structure high-entropy oxide ceramic and preparation method thereof |
| CN114933477A (en) * | 2022-04-28 | 2022-08-23 | 昆明理工大学 | High-toughness phase-change-free niobate ceramic and preparation method thereof |
| CN114956814A (en) * | 2022-05-16 | 2022-08-30 | 昆明理工大学 | High-entropy tantalum/niobium ceramic with high sintering resistance, high CMAS corrosion resistance and preparation method thereof |
| CN114956814B (en) * | 2022-05-16 | 2023-08-18 | 昆明理工大学 | Sintering-resistant high-CMAS corrosion-resistant high-entropy tantalum/niobium ceramic and preparation method thereof |
| CN115403380A (en) * | 2022-08-29 | 2022-11-29 | 中国科学院兰州化学物理研究所 | Application of excellent wear-resistant fluorite structure high-entropy ceramic material |
| CN115467048A (en) * | 2022-09-21 | 2022-12-13 | 山东大学 | High-entropy rare earth niobate or tantalate ceramic fiber and preparation method thereof |
| CN115467048B (en) * | 2022-09-21 | 2023-11-17 | 山东大学 | High-entropy rare earth niobate or tantalate ceramic fiber and preparation method thereof |
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