CN114804864A - Biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering and preparation method thereof - Google Patents
Biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 100
- 238000005245 sintering Methods 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 20
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 17
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 6
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 6
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 59
- 239000010955 niobium Substances 0.000 claims description 56
- 238000000498 ball milling Methods 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 24
- 239000012467 final product Substances 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 12
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 9
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 9
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 9
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 9
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 230000002051 biphasic effect Effects 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 15
- 229910010293 ceramic material Inorganic materials 0.000 description 10
- 230000008859 change Effects 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 230000009977 dual effect Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000012720 thermal barrier coating Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention discloses a biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering and a preparation method thereof. The invention relates to a biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering, which is prepared from t-phase RETaO 4 Ceramics and t-phase zirconia ceramics; wherein RE is Sc, Y and lanthanide rare earth elements, and the preparation method of the biphase high-entropy ceramic can obtain RETaO which can stably exist in t phase at room temperature 4 The ceramic can generate extremely high fracture toughness at room temperature, and simultaneously stably coexists with the high-entropy zirconia ceramic of the t phase, so that the final material has the performance advantages of low thermal conductivity, high thermal expansion coefficient, high hardness and the like, andthe working temperature and the application range of the material are further improved.
Description
Technical Field
The invention belongs to the technical field of high-temperature structural ceramics, and particularly relates to a biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering and a preparation method thereof.
Background
Rare earth tantalate RETaO 4 Ceramic as novel ultra-high temperature thermal insulationThe wear-resistant protective ceramic material has been researched in a large amount at present, and the application range of the wear-resistant protective ceramic material comprises various aspects of thermal barrier coatings, environmental barrier coatings, acid and alkali resistant coatings, impact ablation resistant coatings and the like. The rare earth tantalate used as the thermal barrier coating has the advantages of low thermal conductivity, thermal expansion coefficient matched with a substrate, excellent mechanical property, high-temperature water vapor corrosion resistance and the like, but rare earth elements contained in the rare earth tantalate can react with oxides of calcium, magnesium, aluminum, silicon and the like in the air at high temperature to be corroded. Rare earth tantalate RETaO 4 The important reason for the research of ceramics as high temperature structural materials is that the existence of t-m phase transformation without phase transformation leads to extremely high fracture toughness in high temperature monoclinic phase (t), so that the ceramics are always considered to be novel ultra-high temperature ceramics capable of replacing Yttria Stabilized Zirconia (YSZ). However, phase t is RETaO 4 The high temperature stability of (A) can be stabilized only above 1400 ℃, at which temperature the RETaO is present 4 The fracture toughness of (a) is poor; simultaneous RETaO 4 The problems of low hardness, high thermal conductivity and low Young's modulus at low temperature always limit the application; the t-phase YSZ material has the characteristic of high fracture toughness, but has the problems of high thermal conductivity, low use temperature (less than 1200 ℃) and insufficient thermal expansion coefficient.
Therefore, in order to solve the technical defect problems, it is urgently needed to design and develop a dual-phase high-entropy ceramic prepared by combining high-temperature and high-pressure sintering and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a biphase high-entropy ceramic prepared by combining high-temperature and high-pressure sintering, and also aims to provide a preparation method for preparing the biphase high-entropy ceramic by combining high-temperature and high-pressure sintering.
The first purpose of the invention is realized by that the biphase high-entropy ceramics is composed of t-phase RETaO 4 Ceramics and t-phase zirconia ceramics; wherein RE is Sc, Y and lanthanide rare earth elements.
The other purpose of the invention is realized by the method which is prepared by powder mixing, drying, presintering, weighing again, powder mixing again and final sintering in sequence;
the method specifically comprises the following steps: respectively according to RETaO 4 Chemical formula (RE) of the final product 1/x ) x (Ta 1-y Nb y )O 4 And Zr of the chemical formula of the final zirconia ceramic product 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder, uniformly mixing the two kinds of powder by ball milling and mixing, and using alcohol as a ball milling medium in the ball milling process;
drying the uniformly mixed slurry, sintering at high temperature and cooling to obtain (RE) 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a- b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The starting powder of (a);
grinding the cooled powder, sieving, and pulverizing 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/ 2 Nb b/2 O 2 Weighing the two powders according to the mass ratio, and performing ball milling again to obtain uniformly mixed two-phase powder;
weighing about 2.0g of mixed powder, and preparing into compact dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure of the ceramic is 100-200MPa in the sintering process, the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
The invention relates to a biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering, which is prepared from t-phase RETaO 4 Ceramics and t-phase zirconia ceramics; wherein RE is Sc, Y and lanthanide rare earth elements, and the preparation method of the biphase high-entropy ceramic can obtain RETaO which can stably exist in t phase at room temperature 4 The ceramic can generate extremely high fracture toughness at room temperature, and simultaneously stably coexists with the t-phase high-entropy zirconia ceramic, so that the final material has the performance advantages of low thermal conductivity, high thermal expansion coefficient, high hardness and the like, and the working temperature of the material is further improvedAnd the range of applications.
Drawings
FIG. 1 is an XRD diffractogram of ceramic materials prepared according to examples 1-3 of the present invention and comparative example 1;
FIG. 2 is a graph showing the results of comparing the thermal conductivity of the ceramic materials obtained in examples 1 to 2 of the present invention with that of comparative example 1;
FIG. 3 is a graph showing the results of comparing the thermal expansion coefficients of the ceramic materials obtained in examples 1 to 2 of the present invention with those of comparative example 1;
FIG. 4 is a schematic diagram comparing the fracture toughness of examples 1-3 of the present invention and comparative examples 1-3.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
As shown in fig. 1-4, the present invention provides a dual-phase high-entropy ceramic prepared by high-temperature high-pressure sintering, which consists of t-phase RETaO4 ceramic and t-phase zirconia ceramic;
wherein RE is Sc, Y and lanthanide rare earth elements.
The RETaO 4 The final product of (A) is of the formula (RE) 1/x ) x (Ta 1-y Nb y )O 4 The mass fraction is 10-45%, wherein 1<x<8 and is an integer, and the value of x also represents the amount of the rare earth oxide species added, 0.1<y<0.9; the chemical formula of the final product of the zirconia ceramic is Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The mass fraction is 55-90%, wherein 0.2<a+b<0.4, a = b ≠ 0, RE1 and RE2 represent two different rare earth elements.
The raw material adopted by the biphase high-entropy ceramic is specifically RE 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 Two compounds formed.
The RE 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 Two compounds formed are in particular the RETaO of the t phase 4 Ceramic and RE 2 O 3 +Ta 2 O 5 +Nb 2 O 5 Co-stabilized t-phase zirconia ceramics.
The biphase high-entropy ceramic is specifically a double-t-phase high-entropy ceramic with low thermal conductivity, high thermal expansion, high fracture toughness and high hardness.
The invention also provides a preparation method for preparing the biphase high-entropy ceramic by combining high-temperature high-pressure sintering, which is prepared by powder mixing, drying, presintering, weighing again, powder mixing again and final sintering in sequence;
the method specifically comprises the following steps:
respectively according to RETaO 4 Chemical formula (RE) of the final product 1/x ) x (Ta 1-y Nb y )O 4 And Zr of the chemical formula of the final zirconia ceramic product 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder, uniformly mixing the two kinds of powder by ball milling and mixing, and using alcohol as a ball milling medium in the ball milling process;
drying the uniformly mixed slurry, sintering at high temperature and cooling to obtain (RE) 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a- b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The starting powder of (a);
grinding the cooled powder, sieving, and pulverizing 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/ 2 Nb b/2 O 2 Weighing the two powders according to the mass ratio, and performing ball milling again to obtain uniformly mixed two-phase powder;
weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure of the ceramic is 100-200MPa in the sintering process, the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
The purity of the rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder is more than 99 percent; the ball milling mixing material is used for mixing two kinds of powder, the rotating speed of the ball mill is 200-500 rpm, and the ball milling time is 24-48 h; in the ball milling process, alcohol is used as a ball milling medium, and the mass ratio of powder to alcohol is 1:10-1: 30.
Drying the uniformly mixed slurry at the drying temperature of 90-100 ℃ for 10-20 h; the high-temperature sintering temperature is 1500-1600 ℃, and the sintering time is 5-10 h.
And in the two-phase powder which is uniformly mixed and obtained through ball milling again, the rotating speed of the ball mill is 200-.
That is, in the scheme of the invention, the biphase high-entropy ceramic is prepared by high-temperature high-pressure sintering, and the prepared biphase ceramic is prepared from the high-entropy RETaO of the t phase 4 And zirconia ceramics, wherein RE is Sc, Y and lanthanide rare earth elements;
the raw material is RE 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 The final formed compounds are two kinds, namely, the RETaO of t phase 4 Ceramics and RE 2 O 3 +Ta 2 O 5 +Nb 2 O 5 Co-stabilized t-phase zirconia ceramic;
high entropy RETaO 4 The final product of (A) is of the formula (RE) 1/x ) x (Ta 1-y Nb y )O 4 In which 1 is<x<8 and is an integer, and the value of x also represents the amount of the rare earth oxide species added, and 0.1<y<0.9；
The final product of the high-entropy zirconia ceramic has a chemical formula of Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Wherein 0.2<a+b<0.4，a=b≠0，RE 1 And RE 2 Represents two different rare earth elements;
in the final two-phase high-entropy ceramic product (RE) 1/x ) x (Ta 1-y Nb y )O 4 In a mass fraction of 10-45%, and Zr 1-a- b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The mass fraction of (A) is 55-90%;
the specific preparation process comprises the steps of respectively weighing (RE) according to the stoichiometric ratio 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/ 2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The raw material oxide is prepared into the required double-t-phase high-entropy ceramic with low thermal conductivity, high thermal expansion, high fracture toughness and high hardness by powder mixing, drying, pre-sintering, weighing again, powder mixing again and final sintering.
In other words, it is an object of the present invention to provide a high entropy RETaO of dual t-phase with low thermal conductivity, high coefficient of thermal expansion, high hardness and high fracture toughness 4 +ZrO 2 Ceramics and a method for preparing the same. Firstly realizes the rare earth tantalate RETaO 4 The ceramic can exist in a stable tetragonal phase at room temperature, has no phase change in the temperature range of room temperature to 1600 ℃, and simultaneously carries out cooperative optimization on various mechanical and thermal properties of the material.
The object of the invention is also to use RE as starting material 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 The final formed compounds are two kinds, namely, the RETaO of t phase 4 Ceramics and RE 2 O 3 +Ta 2 O 5 +Nb 2 O 5 Co-stabilized t-phase zirconia ceramic wherein RETaO 4 The final product of (A) is of the formula (RE) 1/x ) x (Ta 1-y Nb y )O 4 The mass fraction is 10-45%; the final product of the zirconia ceramic has the chemical formula of Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The mass fraction is 55-90%
In particular, high entropy RETaO of the two t phases 4 +ZrO 2 The high entropy effect of the ceramic utilization material can effectively enhance phonon dispersionThe thermal conductivity of the material is reduced, the thermal expansion coefficient of the material is improved by improving the non-harmonic vibration of crystal lattices, meanwhile, the zirconia-based ceramic has the characteristics of high hardness and high Young modulus, and the mass fraction of the zirconia-based ceramic in the dual-phase ceramic is larger, so that the problem of insufficient hardness and Young modulus of the rare earth tantalate ceramic material is solved.
Single-phase high-entropy RETaO under normal conditions 4 The ceramics exist in a monoclinic phase (m) form at room temperature and cannot generate the characteristic of high fracture toughness, and the RETaO in the cooling process is inhibited by introducing a second phase, namely a t-phase high-entropy zirconia ceramics and finally sintering at high temperature (the temperature is more than 1500℃) 4 The ceramic t-m phase transition occurs such that RETaO 4 Can stably exist in a t-phase form at room temperature, so that the finally obtained material is high-entropy RETaO of a dual-t phase 4 +ZrO 2 Ceramics, resulting in extremely high fracture toughness.
The common YSZ material is subjected to phase change at 1200 ℃, and in the technical scheme of the invention, zirconium oxide is simultaneously subjected to high-entropy stabilization by using different rare earth elements, tantalum and niobium and is simultaneously subjected to high-entropy stabilization by using a second-phase high-entropy RETaO 4 The addition of the composite material enables the mutual inhibition of two-phase crystal grains in the final material to play a role in refining the crystal grains and improving the mechanical property of the material, and simultaneously effectively inhibits the phase change of two-phase ceramics.
The RETaO which can stably exist in t phase at room temperature is obtained by the scheme of the invention 4 The ceramic generates extremely high fracture toughness, and simultaneously, the material which has no phase change, low thermal conductivity, high thermal expansion coefficient, high hardness and high Young modulus in the temperature range of room temperature to 1600 ℃ is finally obtained by combining the high-entropy zirconia ceramic of the t phase, thereby synergistically solving the problem of RETaO 4 The problems of incapability of being stable in a t phase at room temperature, high thermal conductivity, poor mechanical property and low working temperature of the zirconia-based ceramic are solved.
Further, the method for preparing the biphase high-entropy ceramic by high-temperature high-pressure sintering comprises the following steps:
step (1): respectively according to RETaO 4 Chemical formula (RE) of the final product 1/x ) x (Ta 1-y Nb y )O 4 And Zr of the chemical formula of the final zirconia ceramic product 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder (the purity of the used raw materials is more than 99%), uniformly mixing the two powders by ball milling and mixing (the rotation speed of a ball mill is 200-.
Step (2): drying the uniformly mixed slurry (drying temperature is 90-100 ℃, drying time is 10-20 h), sintering at high temperature and cooling to obtain (RE) 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The initial powder (sintering temperature 1500-.
And (3): the cooled powder was ground and sieved (300 mesh) according to (RE) 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a- b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The two powders are weighed according to the mass ratio, and the two-phase powder which is uniformly mixed is obtained by ball milling again (the rotating speed of the ball mill is 200-.
And (4): weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure of the ceramic is 100-200MPa in the sintering process, the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
Has the advantages that: adopting the materials prepared by the steps (1) to (4) to carry out the phase T RETaO 4 And zirconia ceramics, the RETaO which can stably exist in t phase at room temperature is obtained for the first time 4 Ceramics, obtained by mutual inhibition of two phases, RETaO without phase transition in the temperature range from room temperature to 1600 DEG C 4 And zirconia ceramics (usually R)ETaO 4 The t-m phase transition temperature of the ceramic material is 1300-1450 ℃, the YSZ temperature is 1200 ℃, and the finally obtained ceramic material has fine grains and low thermal conductivity (1.2-1.5 W.m. -1 ·K -1 ) High thermal expansion coefficient (10-13X 10) -6 K -1 ) High fracture toughness (3-5 MPa. m) 1/2 ) High Young's modulus (180-240 GPa) and excellent high-temperature phase stability.
Example 1
Respectively according to RETaO 4 Chemical formula (Sm) of final product 1/3 Y 1/3 Yb 1/3 )(Ta 0.5 Nb 0.5 )O 4 And Zr 0.7 Y 0.075 Yb 0.075 Ta 0.075 Nb 0.075 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder (the purity of the used raw materials is more than 99%), uniformly mixing the two powders by ball milling and mixing (the rotation speed of a ball mill is 200 revolutions per minute, the ball milling time is 48 hours), and using alcohol as a ball milling medium in the ball milling process (the mass ratio of the powder to the alcohol is 1: 10); drying the uniformly mixed slurry (the drying temperature is 90 ℃, the drying time is 20 hours), and sintering and cooling at a high temperature to obtain the (Sm) 1/3 Y 1/3 Yb 1/3 )(Ta 0.5 Nb 0.5 )O 4 And Zr 0.7 Y 0.075 Yb 0.075 Ta 0.075 Nb 0.075 O 2 The initial powder (sintering temperature 1500 ℃ C., sintering time 10 hours), grinding the cooled powder, sieving (300 mesh), according to (RE) 1/x ) x (Ta 1-y Nb y )O 4 (10 wt%) and Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Weighing the two powders according to the mass ratio of 90wt%, and performing ball milling again to obtain uniformly mixed two-phase powder (the rotating speed of the ball mill is 500 revolutions per minute, and the ball milling time is 24 hours); weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure in the sintering process of the ceramic is 100MPa, the sintering temperature is 1500 ℃, and the sintering time is 10 min.
Example 2
Respectively according to RETaO 4 Chemical formula (Y) of the final product 1/2 Lu 1/2 )(Ta 0.7 Nb 0.3 )O 4 And Zr 0.76 Lu 0.06 Yb 0.06 Ta 0.06 Nb 0.06 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder (the purity of the used raw materials is more than 99%), uniformly mixing the two powders by ball milling and mixing (the rotation speed of a ball mill is 500 rpm, the ball milling time is 24 hours), and using alcohol as a ball milling medium in the ball milling process (the mass ratio of the powder to the alcohol is 1: 30); drying the uniformly mixed slurry (drying temperature is 100 ℃, drying time is 10 h), sintering at high temperature and cooling to obtain (Y) 1/2 Lu 1/2 )(Ta 0.7 Nb 0.3 )O 4 And Zr 0.76 Lu 0.0 6 Yb 0.06 Ta 0.06 Nb 0.06 O 2 The sintering temperature is 1600 ℃, the sintering time is 5 hours, the cooled powder is ground and sieved (300 meshes) according to (RE) 1/x ) x (Ta 1-y Nb y )O 4 (45 wt%) and Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 (55 wt%) and then ball-milling to obtain uniformly mixed two-phase powder (ball mill rotation speed 200 rpm, ball milling time 48 h); weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure of the ceramic is 200MPa in the sintering process, the sintering temperature is 1600 ℃, and the sintering time is 5 min.
Example 3
Respectively according to RETaO 4 Chemical formula (Sm) of final product 1/4 Eu 1/4 Y 1/4 Lu 1/4 )(Ta 0.4 Nb 0.6 )O 4 And Zr 0.64 Sm 0.09 Dy 0.09 Ta 0.09 Nb 0.09 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder (the purity of the used raw materials is more than 99%), and uniformly mixing the two powders by ball milling(the rotation speed of the ball mill is 350 r/min, the ball milling time is 30 h), and alcohol is used as a ball milling medium in the ball milling process (the mass ratio of powder to alcohol is 1: 24); drying the uniformly mixed slurry (the drying temperature is 95 ℃, the drying time is 8 hours), and sintering and cooling at a high temperature to obtain the (Sm) 1/4 Eu 1/4 Y 1/4 Lu 1/4 )(Ta 0.4 Nb 0.6 )O 4 And Zr 0.64 Sm 0.09 Dy 0.09 Ta 0.09 Nb 0.09 O 2 The sintering temperature is 1570 ℃ and the sintering time is 7 hours, grinding the cooled powder and sieving (300 meshes) according to the formula (RE) 1/x ) x (Ta 1-y Nb y )O 4 (30 wt.%) and Zr 1-a-b RE 1 a/2 RE 2 a/ 2 Ta b/2 Nb b/2 O 2 Weighing the two powders according to the mass ratio of (70 wt%), and performing ball milling again to obtain uniformly mixed two-phase powder (the rotating speed of the ball mill is 410 revolutions per minute, and the ball milling time is 36 h); weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 And (3) the ceramic is sintered at the pressure of 160MPa and the sintering temperature of 1520 ℃ for 6 min.
Comparative example 1, which differs from example 1 in that the final sintering temperature was 1300 ℃, since the final sintering temperature was lower than RETaO 4 The t-m phase transition temperature of (a) is such that m of ceramic is present in the final sample.
Comparative example 2, which differs from example 1 in that the high-entropy zirconia ceramic has a composition of Zr 0.4 Y 0.15 Yb 0.15 Ta 0.15 Nb 0.15 O 2 The proportion of the stabilizer is more than that of stabilizer atoms which can be contained in a zirconia crystal lattice, so that the final product cannot exist in a t-phase ceramic in a stable way.
Comparative example 3, which differs from example 1 in that the first sintering temperature was 1400 ℃, and that both the initial two-phase powders were obtained with complete reaction, no RETaO in a single phase was obtained 4 And zirconia-based ceramics, so that the final product contains a plurality of precipitated phases.
Preferably, FIG. 1 shows an embodiment of the present invention1-3 and comparative example 1, it can be seen that the materials prepared in examples 1-3 are all high-entropy RETaO in the dual t-phase 4 +ZrO 2 Ceramic, whereas in comparative example 1 a third phase of monoclinic phase zirconia was present;
FIG. 2 is a comparison of the thermal conductivity of the ceramic materials obtained in examples 1-2 of the present invention with that of comparative example 1, showing the high entropy of the double t-phase RETaO 4 +ZrO 2 The thermal conductivity of the ceramic is obviously lower than that of the comparative example 1, which shows that the material prepared by the scheme of the invention has lower thermal conductivity;
FIG. 3 is a graph showing the results of comparing the thermal expansion coefficients of the ceramic materials obtained in examples 1 to 2 of the present invention with that of comparative example 1, and it can be seen that a high-entropy RETaO of a bi-t phase can be seen 4 +ZrO 2 The ceramic has high thermal expansion coefficient (10-13X 10) at 1200 deg.C -6 K -1 ) And no phase change occurs, while in comparative example 1, the phase change occurs due to the presence of the third phase, so that the coefficient of thermal expansion fluctuates with the increase of the temperature;
FIG. 4 is a graph comparing the fracture toughness of inventive examples 1-3 and comparative examples 1-3, and it can be seen that the high entropy RETaO of the dual t phase prepared in inventive examples 1-3 4 +ZrO 2 The fracture toughness of the ceramic is 3-5 MPa.m 1/2 Is obviously higher than 1-3 MPa.m of comparative examples 1-3 1/2 。
Claims (9)
1. The biphase high-entropy ceramic prepared by combining high-temperature high-pressure sintering is characterized by consisting of t-phase RETaO 4 Ceramics and t-phase zirconia ceramics;
wherein RE is Sc, Y and lanthanide rare earth elements.
2. The dual-phase high-entropy ceramic prepared by high-temperature high-pressure sintering according to claim 1, wherein the RETaO is 4 The final product of (A) is of the formula (RE) 1/x ) x (Ta 1-y Nb y )O 4 The mass fraction is 10-45%, wherein 1<x<8 and is an integer, and the value of x also represents the amount of the rare earth oxide species added, 0.1<y<0.9; the chemical formula of the final product of the zirconia ceramic is Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The mass fraction is 55-90%, wherein 0.2<a+b<0.4, a = b ≠ 0, RE1 and RE2 represent two different rare earth elements.
3. The dual-phase high-entropy ceramic prepared by high-temperature high-pressure sintering according to claim 1 or 2, wherein the raw material adopted by the dual-phase high-entropy ceramic is RE 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 Two compounds formed.
4. A biphasic high-entropy ceramic prepared by high-temperature high-pressure sintering according to claim 3, wherein RE 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And ZrO 2 Two compounds formed are in particular the RETaO of the t phase 4 Ceramic and RE 2 O 3 +Ta 2 O 5 +Nb 2 O 5 Co-stabilized t-phase zirconia ceramics.
5. The dual-phase high-entropy ceramic prepared by combining high-temperature high-pressure sintering with the method of claim 1, 2 or 4, wherein the dual-phase high-entropy ceramic is a dual-t-phase high-entropy ceramic with low thermal conductivity, high thermal expansion, high fracture toughness and high hardness.
6. A preparation method for preparing biphase high-entropy ceramic by combining high-temperature high-pressure sintering is characterized in that the method is prepared by powder mixing, drying, presintering, weighing again, powder mixing again and final sintering in sequence;
the method specifically comprises the following steps:
respectively according to RETaO 4 Chemical formula (RE) of the final product 1/x ) x (Ta 1-y Nb y )O 4 And Zr of the chemical formula of the final zirconia ceramic product 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Respectively weighing required rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder, uniformly mixing the two kinds of powder by ball milling and mixing, and using alcohol as a ball milling medium in the ball milling process;
drying the uniformly mixed slurry, sintering at high temperature and cooling to obtain (RE) 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/ 2 RE 2 a/2 Ta b/2 Nb b/2 O 2 The starting powder of (a);
grinding the cooled powder, sieving, and pulverizing 1/x ) x (Ta 1-y Nb y )O 4 And Zr 1-a-b RE 1 a/2 RE 2 a/2 Ta b/2 Nb b/2 O 2 Weighing the two powders according to the mass ratio, and performing ball milling again to obtain uniformly mixed two-phase powder;
weighing about 2.0g of mixed powder, and preparing the dense dual-t-phase high-entropy RETaO by high-temperature high-pressure sintering 4 +ZrO 2 The pressure of the ceramic is 100-200MPa in the sintering process, the sintering temperature is 1500-1700 ℃, and the sintering time is 5-10 min.
7. The method for preparing the biphase high-entropy ceramic by combining the high-temperature high-pressure sintering process with the claim 6, wherein the purity of the rare earth oxide, tantalum oxide, niobium oxide and zirconium oxide powder is greater than 99%;
the ball milling mixing material is used for mixing two kinds of powder, the rotating speed of the ball mill is 200-500 rpm, and the ball milling time is 24-48 h;
in the ball milling process, alcohol is used as a ball milling medium, and the mass ratio of powder to alcohol is 1:10-1: 30.
8. The preparation method for preparing the biphase high-entropy ceramic by combining high-temperature high-pressure sintering according to claim 6, wherein the drying temperature is 90-100 ℃ and the drying time is 10-20h in the drying of the uniformly mixed slurry;
the high-temperature sintering temperature is 1500-1600 ℃, and the sintering time is 5-10 h.
9. The method as claimed in claim 6, wherein the ball milling is performed again to obtain the uniformly mixed two-phase powder, the ball mill rotation speed is 200 and 500 rpm, and the ball milling time is 24-48 h.
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