CN114195515B - Oxide particle optimized nickel tantalate ceramic material and application thereof - Google Patents

Oxide particle optimized nickel tantalate ceramic material and application thereof Download PDF

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CN114195515B
CN114195515B CN202111397667.6A CN202111397667A CN114195515B CN 114195515 B CN114195515 B CN 114195515B CN 202111397667 A CN202111397667 A CN 202111397667A CN 114195515 B CN114195515 B CN 114195515B
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powder
nickel
nickel tantalate
ceramic
grinding
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CN114195515A (en
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冯晶
陈琳
王建坤
张陆洋
李柏辉
荣菊
王刚
赵世贤
粱鹏鹏
李红霞
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Kunming University of Science and Technology
Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Kunming University of Science and Technology
Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention discloses an oxide particle optimized nickel tantalate ceramic material and application thereof, wherein the ceramic material consists of nickel tantalate powder and metal oxide powder/particles, and the chemical general formula of the ceramic material is as follows: (NiTa) 2 O 6 ）（R a O b ） y Wherein R is a O b Represents NiO and Ta 2 O 5 、Al 2 O 3 、MgO、CaO、SiO 2 、ZrO 2 、HfO 2 、Nb 2 O 5 Or 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 R a O b The titanium-nickel-tantalate ceramic material is prepared by the following steps, wherein y is more than or equal to 0.1 and less than or equal to 0.5 in percentage by mass. The ceramic material is a nickel tantalate ceramic block with the compactness of more than 98 percent and the thermal conductivity of 1-6W/m/K within the temperature range of 25-900 ℃ or nickel tantalate ceramic powder with the particle size of 0.1-50 mu m, and can be applied to the preparation of the nickel tantalate ceramic coating with the porosity of 0-30 percent and the coating thermal conductivity of 0.5-1.0W/m/K within the temperature range of 25-900 ℃. The density of the nickel tantalate ceramic material provided by the invention is more than 98%, and a ceramic coating further prepared by the material can be used as a high-temperature heat-insulation protective wear-resistant coating.

Description

Oxide particle optimized nickel tantalate ceramic material and application thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to an oxide particle optimized nickel tantalate ceramic material and application thereof.
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. However, one of the main reasons for limiting the fuel combustion efficiency is that the melting point of high-temperature components in the equipment is low, and currently, the limit of 1100 ℃ cannot be broken through, while the temperature of an air inlet of an aero-engine exceeds 1500 ℃, so that a layer of thermal insulation protective coating material with low thermal conductivity needs to be prepared on the surface of the high-temperature components, and the coating material in a gas turbine and an aero-engine is referred to as a thermal barrier coating material for short, and the performance indexes of the coating material include the characteristics of low thermal conductivity, matching of thermal expansion coefficient with a substrate, high hardness, excellent fracture toughness and the like. The thermal barrier coating material currently in use is yttria stabilizedZirconium oxide (YSZ), which has a high thermal conductivity (2.5-3.5W/m/K) and a coefficient of thermal expansion (10X 10) -6 K -1 ) Far lower than that of the alloy base material (12-14 multiplied by 10) -6 K -1 ) The mismatch of the thermal expansion coefficients of the coating and the base material is caused, and most importantly, the working temperature of the coating cannot meet the current industrial development requirement because the YSZ undergoes phase change at 1200 ℃ to cause the coating to fall off. Ceramic-based composite materials are gradually used for replacing alloy materials to manufacture high-temperature parts in aircraft engines and gas turbines, mainly silicon carbide fiber reinforced silicon carbide and carbon fiber reinforced carbon ceramic composite materials have the characteristics of high working temperature (higher than 2000 ℃) and excellent mechanical properties, but the materials are easily corroded by high-temperature water vapor and oxygen, so that a compact protective coating needs to be prepared on the surface of the materials to prevent oxygen and water vapor from entering, and the coating materials are required to have extremely low porosity, thermal expansion coefficient matched with a substrate, water vapor corrosion resistance and oxidation resistance. The protective coating material currently used on the surface of the ceramic matrix composite material is mainly rare earth silicate (RE) 2 SiO 5 ) The working temperature is lower than 1350 ℃, and the coating is easy to corrode by high-temperature water vapor, so that a new coating material is needed to replace the coating.
Disclosure of Invention
The first purpose of the invention is to provide an oxide particle optimized nickel tantalate ceramic material, and the second purpose of the invention is to provide the application of the oxide particle optimized nickel tantalate ceramic material in preparing a nickel tantalate ceramic coating.
The first purpose of the invention is realized by optimizing a nickel tantalate ceramic material by oxide particles, wherein the ceramic material consists of nickel tantalate powder and metal oxide powder/particles and has a chemical general formula (NiTa) 2 O 6 ）（R a O b ） y Wherein:
R a O b represents NiO, ta 2 O 5 、Al 2 O 3 、MgO、CaO、SiO 2 、ZrO 2 、HfO 2 、Nb 2 O 5 Or one or more of rare earth oxidesThe seed of the seed is selected from the group consisting of,
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 R a O b Accounts for the mass percent of the nickel tantalate ceramic material, y is more than or equal to 0.1 and less than or equal to 0.5 2 O 6 The weight percentage of the nickel tantalate ceramic material is 1-y;
the nickel tantalate ceramic material is a nickel tantalate ceramic block with the density of more than 98% and the thermal conductivity of 1-6W/m/K or nickel tantalate ceramic powder with the particle size of 0.1-50 mu m at the temperature of 25-900 ℃, and the nickel tantalate ceramic block is prepared by the following process steps:
a. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, and drying to obtain mixture powder;
b. performing high-temperature pressureless solid phase sintering, discharge plasma sintering or hot pressing on the mixture powder to obtain a target nickel tantalate ceramic block;
the nickel tantalate ceramic powder is prepared by the following process steps:
A. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, wherein the grinding medium is absolute ethyl alcohol, the rotating speed is set to be 2000-3000r/min, and the grinding time is 12-24h, so as to obtain nano-grade powder;
B. and (3) preparing the nanoscale powder into spherical powder through spray granulation and drying treatment.
In the step a, the grinding medium is absolute ethyl alcohol, the grinding speed is 2000-3000r/min, and the grinding time is 12-24h.
The second purpose of the invention is realized by the application of the nickel tantalate ceramic material in the preparation of the nickel tantalate ceramic coating, wherein the porosity of the nickel tantalate ceramic coating is between 0 and 30 percent, the thermal conductivity of the coating is between 0.5 and 1.0W/m/K in the temperature range of between 25 and 900 ℃,
the nickel tantalate ceramic coating is prepared by the following process steps:
1) Grinding the nickel tantalate ceramic block/powder and sieving the ground nickel tantalate ceramic block/powder by a 500-mesh sieve to obtain a powder material with uniform particle size, and performing spray granulation and drying to obtain spherical powder with the particle size of 20-80 microns;
2) And (3) carrying out electron beam physical vapor deposition or atmospheric plasma spraying or sonic flame spraying or plasma spraying-physical vapor deposition on the surface of the high-temperature metal or ceramic matrix composite material part to obtain the nickel tantalate ceramic coating with the thickness of 50-500 mu m.
The principle of the invention is as follows: nickel tantalate (NiTa) 2 O 6 ) The ceramic material has a unique crystal structure, has the characteristics of poor atomic mass and large ionic radius difference between nickel atoms and tantalum atoms, is beneficial to generating violent lattice vibration so as to scatter phonons and reduce the heat conductivity, and has the characteristics of high hardness, high modulus, high melting point, no phase change at the temperature of below 1600 ℃, low heat conductivity, oxidation resistance and the like.
Because the nickel tantalate and the selected oxide particles have excellent high-temperature stability, the invention still ensures that the material can work at extremely high temperature (more than 1200 ℃) after adding different types and qualities of oxides.
The high-temperature water vapor corrosion resistance is related to the water contact angle of the material, and the larger the contact angle is, the better the water vapor corrosion resistance of the material is. According to the invention, the rare earth oxide particles are creatively selected to optimize the nickel tantalate, the water contact angle of the rare earth oxide is increased along with the increase of the atomic number of the rare earth element, and the addition of the rare earth oxide particles with different types and different mass fractions into the nickel tantalate can simultaneously reduce the thermal conductivity of the material, maintain the proper thermal expansion coefficient and enhance the water vapor corrosion resistance of the material by increasing the water contact angle.
The beneficial effects of the invention are as follows:
1) The density of the ceramic material provided by the invention is more than 98%, the thermal conductivity is low (the thermal conductivity is 1.1-3.2W/m/K within the temperature range of 25-900 ℃), and the ceramic material can be used for preparing high-temperature heat-insulating protective wear-resistant coatings used in different service environments.
2) According to different working environments, oxide particles with different properties can be selected, so that the high-temperature heat-insulation wear-resistant protective coating material with different thermal conductivity, thermal expansion coefficient, hardness, modulus, fracture toughness and other thermophysical properties can be obtained. The porosity of the nickel tantalate ceramic coating material provided by the invention is 0-30%, the thermal conductivity of the coating is 0.5-1.0W/m/K in the temperature range of 25-900 ℃, and the use temperature range is room temperature to 1600 ℃ (as can be seen from a phase diagram, namely figure 9, the nickel tantalate ceramic coating material has no phase change when the temperature reaches 1600 ℃, can keep good thermal and mechanical properties, and has a melting point of more than 1800 ℃). YSZ and RE compared with the prior art 2 SiO 5 Compared with other materials, the material has the characteristics of lower heat conductivity, good high-temperature stability, matched thermal expansion coefficient, high hardness, high fracture toughness and the like.
Drawings
FIG. 1 shows the NiO mass fraction of 30% and NiTa prepared in example 3 2 O 6 An X-ray diffraction pattern of a dense block material with the mass fraction of 70% is compared with a standard PDF card;
FIG. 2 shows NiO mass fraction of 30% and NiTa prepared in example 3 2 O 6 A scanning electron microscope image of the compact block material with the mass fraction of 70%, wherein dark-colored crystal grains are nickel oxide, and light-colored crystal grains are nickel tantalate;
FIG. 3 shows NiO mass fraction of 30% and NiTa prepared in example 3 2 O 6 A thermal conductivity comparison graph of the compact block material with the mass fraction of 70% and nickel tantalate;
FIG. 4 shows NiO mass fraction of 30% and NiTa prepared in example 3 2 O 6 A compact block ceramic photo with the mass fraction of 70%;
FIG. 5 shows NiO mass fraction of 30% and NiTa in example 4 2 O 6 A scanning electron microscope image of the coating material microstructure with the mass fraction of 70%;
FIG. 6 is a photograph prepared in example 5SiO 2 Mass fraction of 20% and NiTa 2 O 6 Scanning electron microscope images of coating material microstructures with the mass fraction of 80%;
FIG. 7 shows a mass fraction of MgO of 50% and NiTa prepared in example 6 2 O 6 The picture of the powder material with the mass fraction of 50 percent, the left picture is a powder object picture, and the right picture is a corresponding scanning electron microscope microscopic structure picture;
FIG. 8 shows Al prepared in example 7 2 O 3 45 percent of NiTa 2 O 6 A picture of a block material object with mass fraction of 55%;
fig. 9 is a binary phase diagram of nickel oxide and nickel tantalate, both of which are shown to be capable of simultaneous stabilization, with the melting point of nickel tantalate exceeding 1600 ℃.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
The invention relates to an oxide particle optimized nickel tantalate ceramic material, which consists of nickel tantalate powder and metal oxide powder/particles and has a chemical general formula (NiTa) 2 O 6 ）（R a O b ） y Wherein:
R a O b represents NiO, ta 2 O 5 、Al 2 O 3 、MgO、CaO、SiO 2 、ZrO 2 、HfO 2 、Nb 2 O 5 Or 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 R a O b The mass percentage of the NiTa ceramic material is more than or equal to 0.1 and less than or equal to 0.5 2 O 6 The weight percentage of the nickel tantalate ceramic material is 1-y;
the nickel tantalate ceramic material is a nickel tantalate ceramic block with the density of more than 98 percent and the thermal conductivity of 1-6W/m/K at the temperature range of 25-900 ℃ or nickel tantalate ceramic powder with the grain size of 0.1-50 mu m,
the nickel tantalate ceramic block is prepared by the following process steps:
a. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, and drying to obtain mixture powder;
b. performing high-temperature pressureless solid phase sintering, discharge plasma sintering or hot pressing on the mixture powder to obtain a target nickel tantalate ceramic block;
the nickel tantalate ceramic powder is prepared by the following process steps:
A. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, wherein the grinding medium is absolute ethyl alcohol, the rotating speed is set to be 2000-3000r/min, and the grinding time is 12-24h, so as to obtain nano-grade powder;
B. and (3) preparing the nanoscale powder into spherical powder through spray granulation and drying treatment.
In the step a, the grinding medium is absolute ethyl alcohol, the grinding speed is 2000-3000r/min, and the grinding time is 12-24h.
The high-temperature pressureless solid phase sintering process in the step b is as follows: and (2) placing the mixture powder into a tabletting mold, maintaining the pressure for 3-7 minutes at 150-300MPa, sintering in a high-temperature furnace, heating to 400-600 ℃ at the speed of 4-6 ℃/min, heating to 1100-1300 ℃ at the speed of 2-4 ℃/min, heating to 1500-1600 ℃ at the speed of 0.5-1.5 ℃/min, preserving the heat for 8-12 hours, and cooling to obtain the nickel tantalate ceramic block.
And (c) during the spark plasma sintering in the step (b), firstly heating to 500-700 ℃ at the speed of 80-120 ℃/min, then heating to 1000-1100 ℃ at the speed of 40-60 ℃/min, preserving the heat for 10-30min, and then cooling along with the furnace.
The preparation method of the nickel tantalate powder comprises the following steps: ball-milling nickel oxide powder and tantalum oxide powder in a ball mill at a rotation speed of 320r/min for 12h according to a molar ratio of 1.
The nickel tantalate ceramic material is applied to preparing a nickel tantalate ceramic coating, the porosity of the nickel tantalate ceramic coating is 0-30%, the thermal conductivity of the coating is 0.5-1.0W/m/K within the temperature range of 25-900 ℃, and the nickel tantalate ceramic coating is prepared by the following process steps:
1) Grinding the nickel tantalate ceramic block/powder and sieving the powder by a 500-mesh sieve to obtain a powder material with uniform particle size, and performing spray granulation and drying to obtain spherical powder with the particle size of 20-80 microns;
2) And (3) performing electron beam physical vapor deposition or atmospheric plasma spraying or sonic flame spraying or plasma spraying-physical vapor deposition on the surface of the high-temperature metal or ceramic matrix composite material component to obtain the nickel tantalate ceramic coating with the thickness of 50-500 mu m.
Example 1 MgO mass fraction of 50% and NiTa 2 O 6 Preparing block with mass fraction of 50%
Weighing 2g of nickel oxide and 11.8302g of tantalum oxide according to the stoichiometric ratio, adding the nickel oxide and the tantalum oxide into a nylon ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, zirconia balls are used as milling balls, the volume of the materials is less than 2/3 of the volume of the ball milling tank, sealing the ball milling tank, placing the ball milling tank in a planetary ball mill for ball milling and mixing, and rotating at 320r/min for 12 hours. Then putting the solution in the ball mill into a rotary evaporator to evaporate alcohol, setting the rotation speed at 60 revolutions per minute and the temperature at 55 ℃, setting the required time at 45 minutes, putting the dried powder into a high-temperature furnace to carry out heat preservation sintering, wherein the sintering temperature parameters are that the heating rate is 3 ℃ per minute between room temperature and 500 ℃, the heating rate is 2 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1500 ℃, finally, preserving the heat at 1300 ℃ for 5 hours, cooling to room temperature, taking out the cooled solution to obtain pure nickel tantalate (NiTa) 2 O 6 ) And (3) powder. Weighing magnesium oxide powder with the same mass as the nickel tantalate powder, placing the two kinds of powder in a grinding machine for grinding and mixing, wherein a grinding medium is absolute ethyl alcohol, the rotating speed is set to 3000r/min, and the grinding time is 24 hours, so that nanoscale powder is obtained. After drying, 2g of powder is weighed and is sintered by discharge plasma to prepare compact ceramic, and the sintering process is from room temperature to 600 DEG CThe temperature rise speed is 100 ℃ per minute, the temperature rise speed is 50 ℃ per minute between 600 ℃ and 1050 ℃, the temperature is kept at 1050 ℃ for 20 minutes, and then the mixture is cooled along with the furnace to obtain the compact MgO with the mass fraction of 50 percent and the NiTa 2 O 6 The mass fraction is 50% of bulk ceramic material.
Example 2 Al 2 O 3 Mass fraction of 60% and NiTa 2 O 6 Preparation of compact block with mass fraction of 55%
The method comprises the steps of preparing nickel tantalate powder according to the method in the embodiment 1, weighing aluminum oxide and the nickel tantalate powder, placing the aluminum oxide and the nickel tantalate powder into a grinding machine, grinding and mixing, wherein a grinding medium is absolute ethyl alcohol, the rotating speed is set to 2000 rpm, and the grinding time is 12 hours, so that nanoscale powder is obtained and dried. Weighing 1.2g of powder, placing the powder into a tabletting mold with the diameter of 15mm, maintaining the pressure for 5 minutes under 200MPa to obtain a preliminarily formed block with the diameter of 15mm and the thickness of 1.2mm, placing the block into a high-temperature furnace for heat preservation and sintering, wherein the sintering temperature parameter is that the heating rate is 5 ℃ per minute between room temperature and 500 ℃, the heating rate is 3 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1600 ℃, and finally, cooling the block to room temperature for 10 hours after heat preservation at 1600 ℃ and taking the block out to obtain the ceramic block material with the density of more than 99%.
Example 3 NiO mass fraction 30% and NiTa 2 O 6 Preparation of compact block with mass fraction of 70%
Weighing 2g of nickel oxide and 11.8302g of tantalum oxide according to the stoichiometric ratio, adding the nickel oxide and the tantalum oxide into a nylon ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, zirconia balls are used as milling balls, the volume of the materials is less than 2/3 of the volume of the ball milling tank, sealing the ball milling tank, and placing the ball milling tank into a planetary ball mill for ball milling and mixing, wherein the rotating speed is 300 revolutions per minute, and the ball milling time is 12 hours. Then putting the solution in the ball mill into a rotary evaporator to evaporate alcohol, setting the rotation speed at 60 rpm and the temperature at 55 ℃, setting the required time at 45 minutes, putting the dried powder into a high-temperature furnace to carry out heat preservation sintering, wherein the sintering temperature parameters are that the heating rate is 3 ℃ per minute between room temperature and 500 ℃, the heating rate is 2 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1500 ℃,finally, the mixture is kept at 1300 ℃ for 5 hours, cooled to room temperature and taken out to obtain pure nickel tantalate (NiTa) 2 O 6 ) And (3) powder. 5.9272g of nickel oxide powder is weighed, and the two powders are put into a grinding machine for grinding and mixing, wherein the grinding medium is absolute ethyl alcohol, the rotating speed is set to 3000r/min, and the grinding time is 24 hours, so that nanoscale powder is obtained. Weighing 2g of powder after drying, preparing compact ceramic through spark plasma sintering, wherein the sintering process comprises the steps of heating up at 100 ℃ per minute between room temperature and 600 ℃, heating up at 50 ℃ per minute between 600 ℃ and 1050 ℃, keeping the temperature at 1050 ℃ for 20 minutes, and then cooling along with a furnace to obtain compact NiO with the mass fraction of 30% and NiTa 2 O 6 70 percent of bulk ceramic material.
As shown in fig. 1-4.
The comparison of the X-ray diffraction pattern of the sample with the standard PDF card is shown in FIG. 1, and the result shows that the phases in the dense block are NiO and NiTa 2 O 6 No other impurity phase or precipitated phase exists; the scanning electron microscope image (figure 2) of the sample shows that no pores or cracks exist on the surface of the sample, the result is consistent with the compactness test result (the compactness is more than 98 percent, and the porosity is less than 2 percent), the dark crystal grains in the image are nickel oxide, the light crystal grains are nickel tantalate, and the nickel oxide crystal grains are smaller, so that the pores among the nickel tantalate crystal grains can be effectively filled, and the compactness of the material is improved. FIG. 3 shows that the thermal conductivity of the material is 1.0-2.5W/m/K in the temperature range of 25-900 ℃, and the thermal conductivity at high temperature (1.0W/m/K, 900 ℃) is far lower than 2.5W/m/K of YSZ and 1.5W/m/K of rare earth zirconate, thus proving that the bulk ceramic material prepared in example 3 has excellent thermal insulation and protection performance and can be used as a thermal insulation and protection coating material. At the same time, the thermal conductivity of the coating material is much lower than that of its dense bulk material, which is typically 1/2 to 1/3 of that of the dense bulk material, and thus it can be seen that the thermal conductivity of the corresponding coating is about 0.5 to 1W/m/K in the corresponding temperature range.
Example 4 NiO mass fraction 30% and NiTa 2 O 6 Preparation of coating with mass fraction of 70%
The dense NiO prepared in example 3 has a mass fraction of 30% and NiTa 2 O 6 The preparation method comprises the steps of grinding and sieving (500 meshes) a ceramic block with the mass fraction of 70% to obtain a powder material with uniform particle size, preparing spherical powder with the particle size of 20-80 micrometers through spray granulation and drying treatment to enable the powder material to have good fluidity, and preparing a ceramic coating with the thickness of about 100 micrometers on silicon carbide fiber reinforced silicon carbide ceramic through electron beam physical vapor deposition, wherein the coating structure is shown in figure 5. The scanning electron microscope test result shows that the coating is in a columnar crystal structure, the compactness of the coating is more than 99 percent and the porosity is less than 1 percent through the Archimedes drainage method test, and the transmission of air and water vapor can be effectively blocked, so that the silicon carbide composite ceramic matrix is protected.
Example 5 SiO 2 Mass fraction of 20% and NiTa 2 O 6 Preparation of coating material with mass fraction of 80%
Weighing 20g of nickel oxide and 118.302g of tantalum oxide according to the stoichiometric ratio, adding the nickel oxide and the tantalum oxide into a nylon ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, zirconia balls are used as milling balls, the volume of the materials is less than 2/3 of the volume of the ball milling tank, sealing the ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling and mixing, wherein the rotating speed is 300 revolutions per minute, and the ball milling time is 12 hours. Then putting the solution in the ball mill into a rotary evaporator to evaporate alcohol, setting the rotation speed at 60 revolutions per minute and the temperature at 55 ℃, setting the required time at 45 minutes, putting the dried powder into a high-temperature furnace to carry out heat preservation sintering, wherein the sintering temperature parameters are that the heating rate is 3 ℃ per minute between room temperature and 500 ℃, the heating rate is 2 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1500 ℃, finally, preserving the heat at 1300 ℃ for 5 hours, cooling to room temperature, taking out the cooled solution to obtain pure nickel tantalate (NiTa) 2 O 6 ) And (3) powder. 34.5755g of silica powder was weighed, and the two powders were put into a grinder for grinding and mixing, the grinding medium was absolute alcohol, the rotation speed was set at 3000 rpm, and the grinding time was 24 hours, thereby obtaining nanoscale powder. Grinding and sieving the powder (500 mesh) to obtain powder material with uniform particle size, spray granulating and drying to obtain spherical powder with particle size of 30-70 μm to make it have good fluidityA ceramic coating having a thickness of about 100 microns was prepared on a silicon carbide fiber reinforced silicon carbide ceramic by electron beam physical vapor deposition, the coating structure being shown in fig. 6. The scanning electron microscope test result shows that the coating is in a columnar crystal structure, the compactness of the coating is 98.2% and the porosity is 1.8% through the Archimedes drainage method test, the transmission of air and water vapor can be effectively blocked, so that the silicon carbide composite ceramic matrix is protected, and the microstructure of the coating is shown in figure 6, so that the coating is compact in structure, the columnar crystals are well combined, the inward transmission of the air and the water vapor is effectively blocked, and the matrix material is protected.
Example 6 MgO mass fraction of 30% and NiTa 2 O 6 Preparation of powder with mass fraction of 50%
Weighing 20g of nickel oxide and 118.302g of tantalum oxide according to a stoichiometric ratio, adding the nickel oxide and the tantalum oxide into a nylon ball milling tank, wherein a ball milling medium is absolute ethyl alcohol, zirconia balls are used as milling balls, the volume of the materials is less than 2/3 of the volume of the ball milling tank, sealing the ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling and mixing, wherein the rotating speed is 300 r/m, and the ball milling time is 12 hours. Then putting the solution in the ball mill into a rotary evaporator to evaporate alcohol, setting the rotation speed at 60 r/min and the temperature at 55 ℃, setting the required time at 45 minutes, putting the dried powder into a high-temperature furnace to carry out heat preservation sintering, wherein the sintering temperature parameters are that the heating rate is 3 ℃ per minute between room temperature and 500 ℃, the heating rate is 2 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1500 ℃, finally, preserving the heat at 1300 ℃ for 5 hours, cooling to room temperature, and taking out the nickel tantalate to obtain pure nickel tantalate (NiTa) 2 O 6 ) And (3) powder. 138.302g of magnesium oxide powder was weighed, and the two powders were put into a mill for milling and mixing with anhydrous alcohol at a rotation speed of 3000 rpm for 24 hours to obtain nanoscale powder. The powder is prepared into spherical powder with the particle size of 10-100 microns through spray granulation and drying treatment, so that the powder has good fluidity, as shown in figure 7, the whole uniformity of the powder material is excellent, and the sphericity of the powder is high and is spherical under an electron microscope; while the particle diameter is 10-100 micronsThe method is suitable for preparing coating materials.
Example 7 Al 2 O 3 45% by mass and NiTa 2 O 6 Preparation of 55% mass fraction block
Weighing 2g of nickel oxide and 11.8302g of tantalum oxide according to the stoichiometric ratio, adding the nickel oxide and the tantalum oxide into a nylon ball milling tank, wherein the ball milling medium is absolute ethyl alcohol, zirconia balls are used as milling balls, the volume of the materials is less than 2/3 of the volume of the ball milling tank, sealing the ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling and mixing, wherein the rotating speed is 300 r/m, and the ball milling time is 12 hours. Then putting the solution in the ball mill into a rotary evaporator to evaporate alcohol, setting the rotation speed at 60 revolutions per minute and the temperature at 55 ℃, setting the required time at 45 minutes, putting the dried powder into a high-temperature furnace to carry out heat preservation sintering, wherein the sintering temperature parameters are that the heating rate is 3 ℃ per minute between room temperature and 500 ℃, the heating rate is 2 ℃ per minute between 500 ℃ and 1200 ℃, the heating rate is 1 ℃ per minute between 1200 ℃ and 1500 ℃, finally, preserving the heat at 1300 ℃ for 5 hours, cooling to room temperature, taking out the cooled solution to obtain pure nickel tantalate (NiTa) 2 O 6 ) And (3) powder. 11.3156g of alumina powder was weighed, and the two powders were put into a grinder for grinding and mixing, the grinding medium was absolute alcohol, the rotation speed was set to 2400 revolutions per minute, and the grinding time was 20 hours, thereby obtaining nanoscale powder. After drying, weighing 2.2g of powder, preparing compact ceramic by spark plasma sintering, wherein the sintering process comprises the steps of heating up to 100 ℃ per minute at the temperature ranging from room temperature to 600 ℃, heating up to 50 ℃ per minute at the temperature ranging from 600 ℃ to 1050 ℃, keeping the temperature at 1150 ℃ for 10 minutes, and cooling along with a furnace to obtain compact Al 2 O 3 45 percent of NiTa 2 O 6 The mass fraction is 55% of bulk ceramic material. See fig. 8.
The results of the thermal physical properties of the materials of examples 1 to 7, such as thermal conductivity, thermal expansion coefficient, hardness, young's modulus, and fracture toughness, are shown in Table 1. It can be seen that the control of the thermal conductivity, the thermal expansion coefficient, the hardness, the Young's modulus, the fracture toughness and other properties of the material is realized along with the difference of the types and the mass ratio of the added oxide powder, wherein the thermal expansion coefficients in different ranges enable the material to be applied to the surfaces of different types of substrates, the matching of the thermal expansion coefficients of the coating and the substrates is realized, so that the service life is prolonged, the generation of thermal stress is reduced, and the fracture toughness is greatly improved, thereby being beneficial to the prolonging of the service life of the coating and the block material.
TABLE 1 thermophysical properties of nickel tantalate ceramic materials prepared in examples 1-7
Figure DEST_PATH_IMAGE002
Test examples 1 to 4
Ceramic blocks containing different mass fractions (10%, 20%,40%, 50%) of nickel oxide were prepared according to the method of example 3, and the mechanical properties of nickel tantalate ceramic blocks with different mass fractions of nickel oxide are shown in table 2.
TABLE 2 Nickel tantalate ceramic bulk mechanical properties for different mass fractions of nickel oxide
Figure DEST_PATH_IMAGE004
As a result: table 2 shows that the mechanical properties of nickel tantalate with increasing mass fraction of nickel oxide particles are significantly changed, and the hardness and Young's modulus of nickel oxide are low, so that both of these two indexes are reduced with increasing nickel oxide content, but the fracture toughness reaches a maximum of 3.2MPa. M. 1/2 Therefore, the material realizes excellent comprehensive mechanical properties of high fracture toughness and low modulus, and meets the performance requirements of being used as a high-temperature heat-insulation protective material.

Claims (3)

1. The oxide particle optimized nickel tantalate ceramic material is characterized by consisting of nickel tantalate powder and metal oxide powder/particles and having a chemical general formula (NiTa) 2 O 6 ） 1-y （R a O b ） y Wherein R is a O b NiO and Al 2 O 3 MgO or SiO 2 Y tableR is shown a O b The mass percentage of the NiTa ceramic material is more than or equal to 0.1 and less than or equal to 0.5 2 O 6 The weight percentage of the nickel tantalate ceramic material is 1-y; the nickel tantalate ceramic material is a nickel tantalate ceramic block with the density of more than 98% and the thermal conductivity of 1-6W/(m.K) at the temperature range of 25-900 ℃ or nickel tantalate ceramic powder with the particle size of 0.1-50 mu m;
the nickel tantalate ceramic block is prepared by the following process steps:
a. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, wherein the grinding medium is absolute ethyl alcohol, the grinding speed is 2000-3000r/min, the grinding time is 12-24h, and drying to obtain mixture powder;
b. performing high-temperature pressureless solid-phase sintering or spark plasma sintering on the mixture powder to obtain a target nickel tantalate ceramic block; wherein:
the high-temperature pressureless solid-phase sintering is to place the mixture powder in a tabletting mold, maintain the pressure for 3-7 minutes under 150-300MPa, sinter in a high-temperature furnace, firstly heat up to 400-600 ℃ at the speed of 4-6 ℃/min, then heat up to 1100-1300 ℃ at the speed of 2-4 ℃/min, finally heat up to 1500-1600 ℃ at the speed of 0.5-1.5 ℃/min, preserve heat for 8-12 hours, and cool to obtain the nickel tantalate ceramic block;
when in spark plasma sintering, firstly heating to 500-700 ℃ at the speed of 80-120 ℃/min, then heating to 1000-1100 ℃ at the speed of 40-60 ℃/min, preserving heat for 10-30min, and then cooling along with the furnace;
the nickel tantalate ceramic powder is prepared by the following process steps:
A. putting the nickel tantalate powder and the metal oxide powder/particles into a grinding machine for grinding, wherein the grinding medium is absolute ethyl alcohol, the rotating speed is set to be 2000-3000r/min, and the grinding time is 12-24h, so as to obtain nano-grade powder;
B. and (3) preparing the nanoscale powder into spherical powder through spray granulation and drying treatment.
2. The oxide particle optimized nickel tantalate ceramic material according to claim 1, wherein the nickel tantalate powder is prepared by a method comprising: ball-milling nickel oxide powder and tantalum oxide powder in a ball mill at a rotation speed of 320r/min for 12h according to a molar ratio of 1.
3. The use of a nickel tantalate ceramic material as claimed in claim 1 or 2 in the preparation of a nickel tantalate ceramic coating, wherein the nickel tantalate ceramic coating has a porosity of between 0 and 30% and a coating thermal conductivity of between 0.5 and 1.0W/(m-K) in the temperature range of 25 to 900 ℃, and wherein the nickel tantalate ceramic coating is prepared by the following process steps:
1) Grinding the nickel tantalate ceramic block/powder and sieving the powder by a 500-mesh sieve to obtain a powder material with uniform particle size, and performing spray granulation and drying to obtain spherical powder with the particle size of 20-80 microns;
2) And (3) carrying out electron beam physical vapor deposition or atmospheric plasma spraying or sonic flame spraying or plasma spraying-physical vapor deposition on the surface of the high-temperature metal or ceramic matrix composite material part to obtain the nickel tantalate ceramic coating with the thickness of 50-500 mu m.
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