CN114031401A - Low-temperature sintered nickel niobate ceramic material with high hardness and high strength - Google Patents
Low-temperature sintered nickel niobate ceramic material with high hardness and high strength Download PDFInfo
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- CN114031401A CN114031401A CN202111396147.3A CN202111396147A CN114031401A CN 114031401 A CN114031401 A CN 114031401A CN 202111396147 A CN202111396147 A CN 202111396147A CN 114031401 A CN114031401 A CN 114031401A
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- nickel niobate
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 89
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000000227 grinding Methods 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910005805 NiNb Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 10
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 8
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 6
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 5
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 5
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 5
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 5
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 5
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 5
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 5
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 5
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 33
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 32
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 22
- 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 22
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 239000011812 mixed powder Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 37
- 238000002360 preparation method Methods 0.000 abstract description 17
- 238000007873 sieving Methods 0.000 abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 16
- 239000013078 crystal Substances 0.000 description 13
- 239000010955 niobium Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 239000000395 magnesium oxide Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000012720 thermal barrier coating Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 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 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229910001936 tantalum oxide Inorganic materials 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 3
- 229910000449 hafnium oxide Inorganic materials 0.000 description 3
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 3
- 229910003443 lutetium oxide Inorganic materials 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 3
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 2
- 229940075613 gadolinium oxide Drugs 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 229910001954 samarium oxide Inorganic materials 0.000 description 2
- 229940075630 samarium oxide Drugs 0.000 description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 2
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 2
- 229940075624 ytterbium oxide Drugs 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a low-temperature sintered nickel niobate ceramic material with high hardness and high strength, which consists of nickel niobate and metal oxide and has a general formula (NiNb)2O6）（RaOb）yWherein R isaObRepresents Ta2O5、Al2O3、MgO、ZrO2、HfO2Or one or more rare earth oxides, wherein the rare earth oxides are oxides of Sc, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tm, Dy, Ho, Er, Yb or Lu; y represents RaObAccounts for the mass percent of the nickel niobate ceramic material, and y is more than or equal to 0.1 and less than or equal to 0.7. The preparation method of the ceramic material is to use nickel niobate powder NiNb2O6And the metal oxide particles or powders are subjected to grindingGrinding and mixing in a machine, sieving after grinding, and placing the obtained powder in a die for spark plasma sintering to obtain the powder. Compared with the traditional high-temperature solid phase method, the nickel niobate ceramic provided by the invention has higher compactness, hardness and strength, and simultaneously, oxides of different types and different mass fractions can be added according to the requirements so as to regulate and control the thermophysical properties of the nickel niobate ceramic.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a low-temperature sintered nickel niobate ceramic material with high hardness and high strength.
Background
The combustion temperature of fuel oil used in an aircraft engine, a gas turbine and an automobile engine is in direct proportion to the utilization efficiency of the fuel oil, and the improvement of the combustion temperature is beneficial to improving the utilization efficiency of the fuel oil and simultaneously can improve the thrust-weight ratio of the equipment so as to provide stronger power, thereby further improving the speed of the aircraft and the automobile and the power generation efficiency of a generator set in a thermal power station. While limiting the efficiency of fuel combustionOne reason for this is that the melting point of the high-temperature components in the equipment is low, and currently, the limit of 1100 ℃ cannot be broken through, while the temperature of the air inlet of the aircraft engine already exceeds 1500 ℃, so that it is necessary to prepare a layer of thermal insulation protective coating material with low thermal conductivity on the surface of the high-temperature components, and this coating material is referred to as thermal barrier coating material in the gas turbine and aircraft engine. The thermal barrier coating material currently in use is Yttria Stabilized Zirconia (YSZ), which has a high thermal conductivity (2.5-3.5W/m/K) and a coefficient of thermal expansion (10 × 10)-6 K-1) Far lower than that of the alloy matrix material (12-14 multiplied by 10)-6K-1) Resulting in a mismatch between the thermal expansion coefficients of the coating and the base material, and thus the working temperature thereof cannot meet the current industrial development requirements. In order to replace the current YSZ material, a novel nickel niobate ceramic is proposed to be used as a thermal barrier coating, wherein nickel niobate has the characteristics of low thermal conductivity, excellent high-temperature chemical stability and high melting point, but the defects of low hardness and low fracture toughness make the nickel niobate not be directly used as the thermal barrier coating. Moreover, the nickel niobate ceramic prepared by common high-temperature sintering has a certain porosity and a certain influence on the mechanical properties of the nickel niobate ceramic, and only increasing the sintering temperature leads to melting of the nickel niobate ceramic, so that obtaining a dense nickel niobate ceramic with excellent mechanical properties (high hardness, high modulus and high fracture toughness) has been a current difficulty.
Disclosure of Invention
The invention aims to provide a low-temperature sintered nickel niobate ceramic material with high hardness and high strength.
The invention aims to realize the purpose that the low-temperature sintered nickel niobate ceramic material with high hardness and high strength consists of nickel niobate and metal oxide and has the general formula (NiNb)2O6）（RaOb）yWherein:
RaObrepresents Ta2O5、Al2O3、MgO、ZrO2、HfO2Or one or more of rare earth oxides,
the rare earth oxide is an oxide of Sc, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tm, Dy, Ho, Er, Yb or Lu;
y represents RaObAccounts for the mass percent of the nickel niobate ceramic material, and y is more than or equal to 0.1 and less than or equal to 0.7;
the density of the nickel niobate ceramic material is more than 99 percent, the hardness is more than 9GPa, the Young modulus is more than 160GPa, and the fracture toughness value is 1.3-2.5MPa.m1/2；
The low-temperature sintered nickel niobate ceramic material is prepared by the following process steps:
A. nickel niobate powder NiNb2O6And metal oxide particles or powder are put into a grinding machine to be ground and mixed to obtain mixed powder;
B. the mixed powder is placed in a mould after being sieved to be subjected to spark plasma sintering to obtain a target ceramic material;
wherein the temperature of the spark plasma sintering is 600-800 ℃, the heat preservation time is 10-30 minutes, and the heating rate is 50 ℃/min.
The principle of the invention is as follows:
the invention adds Ta with excellent mechanical property2O5、Al2O3、MgO、ZrO2、HfO2And rare earth oxide (RE)2O3And one or more (two or more) oxides of RE = Sc, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tm, Dy, Ho, Er, Yb and Lu) optimize the mechanical property of the nickel niobate, so that the nickel niobate ceramic with high hardness, high strength, high modulus and high fracture toughness is obtained, and the problem that the nickel niobate ceramic cannot be directly used as a thermal barrier coating due to insufficient mechanical property is solved. The added oxide does not react with nickel niobate at low temperature, and can be used as a crystallization point in the sintering process, so that nickel niobate is promoted to crystallize at low temperature, and simultaneously, the nickel niobate is used as hard particles to play a pinning effect at a crystal boundary to inhibit the growth of crystal grains, so that the crystal grains are refined, and the mechanical property of the material is further improved.
In addition, the oxides have different thermal conductivity, thermal expansion coefficient and other thermophysical properties, so that the thermophysical properties of the required materials can be effectively regulated according to different working environments.
The invention can effectively lead the grain diameter of the powder to reach the nanometer level by regulating and controlling the rotating speed and the time during grinding according to the grain diameter of the original powder, and simultaneously, the invention combines the functions of promoting the nucleation of the crystal grains and inhibiting the growth of the crystal grains by the hard oxide, and can obtain compact ceramic materials under the condition of lower than 800 ℃. The fine powder grain size, the promotion of the nucleation position of the crystal grains, the obvious pinning effect and the high melting point of the added oxide are all important factors for ensuring that the compact high-strength and high-hardness nickel niobate ceramic is prepared by low-temperature sintering.
The invention has the beneficial effects that:
1. the method solves the problem that the common high-temperature sintering can not prepare the compact nickel niobate ceramic, and compared with the condition that the material has many and non-compact pores under the condition of low temperature in the common sintering, the material is melted due to high temperature, and the compact nickel niobate ceramic block can not be obtained, the preparation method of the nickel niobate ceramic has the advantages that the density of the high-hardness and high-strength nickel niobate ceramic prepared by sintering at the temperature of 600-800 ℃ is more than 99 percent, and the porosity is less than 1 percent.
2. Compared with the nickel niobate ceramic prepared by the traditional high-temperature solid phase method, the nickel niobate ceramic prepared by the invention has higher hardness and strength: the hardness of the nickel niobate ceramic prepared by the method is more than 9GPa, the nickel niobate ceramic is improved by over 110% compared with the nickel niobate ceramic (4 GPa) prepared by the traditional method, and the maximum value of fracture toughness can reach 2.5MPa.m1/2Compared with nickel niobate ceramic (1.1 MPa. m) prepared by the traditional method1/2) The Young modulus is improved by over 100 percent and is more than 160GPa, and the Young modulus is improved by over 70 percent compared with nickel niobate ceramic (-90 GPa).
3. The invention utilizes the added oxide as a crystallization point and a crystal boundary pinning point, and simultaneously plays the roles of promoting the nucleation of crystal grains and inhibiting the excessive growth of the crystal grains. Oxides of different types and different mass fractions can be added simultaneously according to the requirements so as to regulate and control the thermophysical properties of the nickel niobate ceramic, for example, the thermal expansion coefficient of the nickel niobate can be regulated from 6-7 multiplied by 10 by adding magnesium oxide-6 K-1Increase by more than 10X 10-6 K-1The heat conductivity of the nickel niobate can be effectively reduced by adding the rare earth oxide, so that the nickel niobate can be in service at different service levelsThe product is used in the environment.
Drawings
FIG. 1 is a schematic representation of the ceramics according to examples 1, 6 to 8 of the present invention from left to right;
FIG. 2 shows, from left to right, 30% Al obtained in example 3 of the present invention2O3+70%NiNb2O6NiNb prepared by ceramic and common sintering method2O6Scanning a ceramic electron microscope;
FIG. 3 is a graph of NiNb with different alumina contents obtained in examples 1-52O6A ceramic hardness variation trend graph;
FIG. 4 shows 65% MgO +35% NiNb prepared in example 72O6A schematic thermal expansion coefficient of the ceramic;
FIG. 5 is 20% Y obtained in example 82O3+20% Yb2O3+60%NiNb2O6Thermal conductivity of ceramics is plotted against temperature.
The specific implementation mode is as follows:
the invention is further described with reference to the following drawings and detailed description.
The invention relates to a low-temperature sintered nickel niobate ceramic material with high hardness and high strength, which consists of nickel niobate and metal oxide and has a general formula (NiNb)2O6）（RaOb）yWherein:
RaObrepresents Ta2O5、Al2O3、MgO、ZrO2、HfO2Or one or more of rare earth oxides,
the rare earth oxide is an oxide of Sc, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tm, Dy, Ho, Er, Yb or Lu;
y represents RaObAccounts for the mass percent of the nickel niobate ceramic material, and y is more than or equal to 0.1 and less than or equal to 0.7;
the density of the nickel niobate ceramic material is more than 99 percent, the hardness is more than 9GPa, the Young modulus is more than 160GPa, and the fracture toughness value is 1.3-2.5MPa.m1/2；
The low-temperature sintered nickel niobate ceramic material is prepared by the following process steps:
A. nickel niobate powder NiNb2O6And metal oxide particles or powder are put into a grinding machine to be ground and mixed to obtain mixed powder;
B. the mixed powder is placed in a mould after being sieved to be subjected to spark plasma sintering to obtain a target ceramic material;
wherein the temperature of the spark plasma sintering is 600-800 ℃, the heat preservation time is 10-30 minutes, and the heating rate is 50 ℃/min.
The grinding speed is 1000-.
The preparation method of the nickel niobate powder comprises the following steps: and ball-milling and mixing the nickel oxide powder and the niobium oxide powder in a ball mill at a ratio of 0.9-1:0.9-1, wherein the ball-milling medium is distilled water or absolute ethyl alcohol, drying after ball-milling, sintering at high temperature in a high-temperature furnace, and cooling to obtain the nickel niobate powder.
The mass of the ball milling medium is 5-20 times of the total mass of the nickel oxide powder and the niobium oxide powder.
The rotation speed of the ball mill is 200-500r/min, the ball milling time is 5-20 hours, the ball milling medium is zirconia balls, and the ball-material ratio is 10:1-30: 1; drying by a rotary evaporator after ball milling, wherein the rotating speed is 60-200r/min and the temperature is 50-90 ℃.
In the high-temperature sintering process, the temperature is raised to 600 ℃ at the rate of 2-5 ℃/min, then raised to 1500 ℃ at the rate of 1-3 ℃/min, and the temperature is kept at 1500 ℃ for 2-10 hours.
Example 1
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 1.5196g of alumina
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 10 hours at a rotating speed of 360r/min, volatilizing the solvent by using a rotary evaporator (100 r/min, 1 hour), sintering at 1200 ℃ for 5 hours, and cooling to room temperature to obtain the nickel niobate powder. Grinding the prepared nickel niobate powder and 1.5196g of alumina powder in a grinding machine at the rotating speed of 3000r/min for 24 hours to obtain the nickel niobate powderSieving the mixture with 800 mesh sieve to obtain mixed powder; 2.5g of the mixed powder is weighed and placed in a die, and spark plasma sintering is carried out for 15 minutes at 600 ℃ to obtain 10 percent Al2O3+90%NiNb2O6A ceramic material.
Example 2
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 3.4192g of alumina
The preparation method comprises the following steps: the sintering temperature is 620 ℃, the sintering time is 10min, and other parameters are the same as those of the example 1.
Example 3
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 5.8615g of alumina
The preparation method comprises the following steps: the sintering temperature is 700 ℃, the sintering time is 20min, the preparation method of other steps is the same as that of the example 1, and the prepared ceramic material entity is shown in figure 1A.
30% Al obtained in example 32O3+90%NiNb2O6Ceramics and NiNb prepared by a common sintering method (the common sintering process is that powder dried by ball milling is pressurized to obtain a block, the block is placed in a high-temperature furnace for pressureless sintering with temperature rise and heat preservation, the sintering temperature is 1500 ℃, and the heat preservation time is 6 hours)2O6The microstructure of the ceramics was measured as shown in fig. 2A and 2B. As can be seen from the figure, the material prepared by the method of the invention is compact and basically has no pores, and simultaneously, the surfaces of the crystal grains are smooth and the combination among the crystal grains is tight; the sample crystal grains prepared by the common sintering method have uneven surfaces, obvious pores exist, and the combination between the crystal grains is poor, so that the mechanical property of the material is insufficient.
Example 4
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 9.1179g of alumina
The preparation method comprises the following steps: the sintering temperature is 730 ℃, the sintering time is 12min, and the preparation method of other steps is the same as that of the example 1.
Example 5
Raw materials: oxidation by oxygenNickel (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 13.6769g of alumina
The preparation method comprises the following steps: the sintering temperature is 785 ℃, the sintering time is 18min, and the preparation method of other step parameters is the same as that of the example 1.
Example 6
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g powder, 13.6769g tantalum oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 8 hours at a rotating speed of 360r/min, volatilizing the solvent by using a rotary evaporator (200 r/min, 0.5 hour), sintering for 2 hours at 1500 ℃ in a muffle furnace, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder and 13.6769g tantalum oxide powder in a grinding machine at the rotating speed of 2000r/min for 20 hours, and sieving the obtained mixture with a 800-mesh sieve to obtain mixed powder; 3g of the mixed powder is weighed and placed in a die, and spark plasma sintering is carried out for 20 minutes at 800 ℃ to obtain a ceramic material with the density of 99.8%, wherein a physical graph is shown in figure 1B.
Example 7
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 25.4g of magnesium oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, carrying out ball milling for 12 hours at a rotating speed of 420r/min, volatilizing the solvent by using a rotary evaporator (120 r/min, 0.5 hour), sintering at 1300 ℃ for 3 hours in a muffle furnace, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder and 25.4g of magnesium oxide powder in a grinding machine at the rotating speed of 2800r/min for 30 hours, and sieving the obtained mixture with a 800-mesh sieve to obtain mixed powder; 3.6g of mixed powder is weighed and placed in a die, and discharge plasma sintering is carried out for 30 minutes at 750 ℃ to obtain 65 percent MgO with the density of more than 99.3 percent and 35 percent NiNb2O6Ceramic material, as shown in fig. 1C.
The thermal expansion coefficient of the ceramic material prepared in this example was measured and compared with that of NiNb prepared by ordinary sintering2O6In comparison, as can be seen from fig. 4: prepared in this exampleThe thermal expansion coefficient of the ceramic material is higher than that of NiNb prepared by common sintering2O6The improvement is remarkable.
Example 8
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) Powders 10.6769g, 4.5590g yttrium oxide and 4.5590g ytterbium oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 6 hours at a rotating speed of 500r/min, volatilizing the solvent by using a rotary evaporator (160 r/min, 0.75 hour), sintering at 1450 ℃ in a muffle furnace for 3.5 hours, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder, 4.5590g g yttrium oxide powder and 4.5590g g ytterbium oxide powder in a grinding machine for 15 hours at the rotating speed of 1900r/min, and sieving the obtained mixture with a 800-mesh sieve to obtain mixed powder; 2.2g of the mixed powder is weighed and placed in a die, and spark plasma sintering is carried out for 15 minutes at 730 ℃ to obtain 20 percent Y with the density of 9.7 percent2O3+20% Yb2O3+60%NiNb2O6Ceramic material, as shown in fig. 1D.
For 20% Y obtained in this example2O3+20% Yb2O3+60%NiNb2O6The thermal conductivity of the ceramic material is measured, and as can be seen from fig. 5, the thermal conductivity of the ceramic material prepared in the embodiment is higher than that of NiNb prepared by common sintering2O6The thermal conductivity of the material is obviously reduced, so that the thermal insulation and protection performance of the material is more excellent.
Example 9
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) Powders 10.6769g, 4.5590g zirconium oxide and 4.5590g hafnium oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 6 hours at a rotating speed of 500r/min, volatilizing the solvent by using a rotary evaporator (160 r/min, 0.75 hour), sintering at 1450 ℃ in a muffle furnace for 3.5 hours, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder, 4.5590g of zirconium oxide and 4.5590g of hafnium oxide powder in a grinding machine at the speed of 1900r/min for 15 hours, and passing the obtained mixtureSieving with 800 mesh sieve to obtain mixed powder; 2.2g of the mixed powder was weighed and placed in a mold, and spark plasma sintering was carried out at 730 ℃ for 15 minutes to obtain 20% ZrO having a density of 99.7%2+20% HfO2+60%NiNb2O6A ceramic material.
Example 10
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 4.5590g of zirconium oxide, 4.5590g of hafnium oxide and 4.5591g of tantalum oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 6 hours at a rotating speed of 500r/min, volatilizing the solvent by using a rotary evaporator (160 r/min, 0.75 hour), sintering at 1450 ℃ in a muffle furnace for 3.5 hours, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder, 4.5590g of zirconium oxide, 4.5590g of hafnium oxide and 4.5591g of tantalum oxide in a grinding machine at the rotating speed of 3000r/min for 12 hours, and sieving the obtained mixture with a 800-mesh sieve to obtain mixed powder; 2.3g of the mixed powder was weighed and placed in a mold, and spark plasma sintering was carried out at 750 ℃ for 15 minutes to obtain 16.6% ZrO having a density of 99.8%2+16.6% HfO2+16.7%Ta2O5+60%NiNb2O6A ceramic material.
Example 11
Raw materials: nickel oxide (NiO) 3g, niobium oxide (Nb)2O5) 10.6769g of powder, 9.1179g of samarium oxide, 9.1179g of gadolinium oxide and 13.6769g of lutetium oxide
The preparation method comprises the following steps: adding nickel oxide and niobium oxide into a ball mill using absolute ethyl alcohol as a medium, mixing, ball milling for 6 hours at a rotating speed of 500r/min, volatilizing the solvent by using a rotary evaporator (160 r/min, 0.75 hour), sintering at 1450 ℃ in a muffle furnace for 3.5 hours, and cooling to room temperature to obtain the nickel niobate powder. Grinding nickel niobate powder, 9.1179g of samarium oxide, 9.1179g of gadolinium oxide and 13.6769g of lutetium oxide in a grinding machine at the rotating speed of 3000r/min for 10 hours, and sieving the obtained mixture with a 800-mesh sieve to obtain mixed powder; 2.0g of mixed powder is weighed and placed in a die, and spark plasma sintering is carried out for 12 minutes at 700 ℃, so as to obtain 20 percent Sm with the density of 99.1 percent2O3+20% Gd2O3+30% Lu2O3+30%NiNb2O6A ceramic material.
The densification and mechanical properties of the ceramic materials prepared in examples 1-11 were measured and compared with those of nickel niobate ceramics prepared by conventional methods, and the results are shown in table 1.
TABLE 1 comparison of the densification and mechanical properties of nickel niobate ceramic materials prepared by the conventional methods and examples 1-11
As can be seen from Table 1 and FIG. 3, in examples 1-5, as the content of alumina in the nickel niobate ceramic material increases, the hardness and Young's modulus of the prepared ceramic material also increase. The hardness of the nickel niobate ceramics prepared in the embodiments 2-11 is more than 9GPa, the nickel niobate ceramics prepared by the traditional method (4 GPa) is improved by over 110%, and the maximum value of the fracture toughness can reach 2.5MPa.m1 /2Compared with nickel niobate ceramic (1.1 MPa. m) prepared by the traditional method1/2) The Young modulus is improved by over 100 percent and is more than 160GPa, and the Young modulus is improved by over 70 percent compared with nickel niobate ceramic (-90 GPa). The high-hardness and high-strength nickel niobate ceramics prepared in examples 1 to 11 all have a density of more than 99% and a porosity of less than 1%, that is, the ceramics contain very few pores, cracks and the like, and can effectively prevent air, water vapor and low-melting-point oxides from permeating into the materials.
Claims (6)
1. A low-temperature sintered nickel niobate ceramic material with high hardness and high strength is characterized in that the ceramic material consists of nickel niobate and metal oxide and has a general formula (NiNb)2O6）（RaOb）yWherein:
RaObrepresents Ta2O5、Al2O3、MgO、ZrO2、HfO2Or one or more of rare earth oxides,
the rare earth oxide is an oxide of Sc, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tm, Dy, Ho, Er, Yb or Lu;
y represents RaObAccounts for the mass percent of the nickel niobate ceramic material, and y is more than or equal to 0.1 and less than or equal to 0.7;
the density of the nickel niobate ceramic material is more than 99 percent, the hardness is more than 9GPa, the Young modulus is more than 160GPa, and the fracture toughness value is 1.3-2.5MPa.m1/2；
The low-temperature sintered nickel niobate ceramic material is prepared by the following process steps:
A. nickel niobate powder NiNb2O6And metal oxide particles or powder are put into a grinding machine to be ground and mixed to obtain mixed powder;
B. the mixed powder is placed in a mould after being sieved to be subjected to spark plasma sintering to obtain a target ceramic material;
wherein the temperature of the spark plasma sintering is 600-800 ℃, the heat preservation time is 10-30 minutes, and the heating rate is 50 ℃/min.
2. The low-temperature sintered nickel niobate ceramic material as claimed in claim 1, wherein the grinding speed is 1000-.
3. The low-temperature sintered nickel niobate ceramic material of claim 1, wherein the nickel niobate powder is prepared by a method comprising: and ball-milling and mixing the nickel oxide powder and the niobium oxide powder in a ball mill at a ratio of 0.9-1:0.9-1, wherein the ball-milling medium is distilled water or absolute ethyl alcohol, drying after ball-milling, sintering at high temperature in a high-temperature furnace, and cooling to obtain the nickel niobate powder.
4. The method for preparing the nickel niobate ceramic material sintered at the low temperature according to claim 3, wherein the mass of the ball milling medium is 5 to 20 times of the total mass of the nickel oxide powder and the niobium oxide powder.
5. The method for preparing the nickel niobate ceramic material sintered at the low temperature as claimed in claim 3, wherein the rotation speed of the ball mill is 200-; drying by a rotary evaporator after ball milling, wherein the rotating speed is 60-200r/min and the temperature is 50-90 ℃.
6. The method for preparing low-temperature sintered nickel niobate ceramic material as claimed in claim 3, wherein the temperature is raised to 600 ℃ at a rate of 2-5 ℃/min, then raised to 1500 ℃ at a rate of 1-3 ℃/min, and then kept at 1500 ℃ for 2-10 hours.
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