CN114874008B - YTaO (YTaO) 4 /Y 3 TaO 7 Biphase ceramic and preparation method and application thereof - Google Patents
YTaO (YTaO) 4 /Y 3 TaO 7 Biphase ceramic and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of coating, in particular to an YTaO 4 /Y 3 TaO 7 Biphase ceramics, and a preparation method and application thereof. The preparation method of the biphase ceramic comprises the following steps: s1, preparing YTaO by adopting inverse microemulsion method 4 Single-phase powder and Y 3 TaO 7 Single-phase powder; s2, mixing YTAO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder is obtained to obtain mixed powder, then the mixed powder is subjected to ball milling, grinding and sieving, and then discharge plasma sintering is carried out to obtain the biphase ceramic. According to the invention, the phase change of the single-phase rare earth tantalate at high temperature is weakened or even completely counteracted by introducing the second-phase material, so that the hardness and fracture toughness of the material are effectively improved, and the thermal conductivity is reduced along with the reduction of the grain size, thereby solving the limitation of the traditional single-phase rare earth tantalate in terms of mechanical property and thermal property.
Description
Technical Field
The invention relates to the technical field of coating, in particular to an YTaO 4 /Y 3 TaO 7 Biphase ceramics, and a preparation method and application thereof.
Background
The thermal barrier coating is deposited on the surface of the object through the processes of spraying and the like by using materials such as ceramics and the like, and the coating formed by using the high-temperature resistant materials such as ceramics and the like can isolate external heat, reduce the temperature of the substrate and prevent the substrate from high-temperature oxidation, corrosion and abrasion. Thermal barrier coatings are often used as protective coatings for high temperature parts of aircraft engines and gas turbines to increase the operating temperature and efficiency of associated components, thereby extending the useful life of the associated components and reducing the emission of greenhouse gases. Studies have shown that thermal barrier coatings are effective in improving the thermal efficiency of coated objects by about 60%.
The rare earth tantalate ceramic is used as a novel elastomer ceramic thermal barrier coating material, the service temperature of the rare earth tantalate ceramic can reach 1600 ℃, and the rare earth tantalate ceramic also has the following advantages: low heat conductivity, high hardness, corrosion resistance, excellent high-temperature phase stability and mechanical property, small volume change before and after phase change and proper thermal expansion coefficient.
At present, rare earth tantalate materials are generally single-phase structures, and have limitations on mechanical and thermal properties, such as YTaO 4 The single-phase ceramic has the advantages of low heat conduction, matched thermal expansion coefficient (heat protection field), good fracture toughness and the like, but YTaO 4 The single-phase ceramic has phase change at 1400+/-20 ℃ to reduce the mechanical property.
To sum up, how to increase YTaO 4 The thermal property and mechanical property of single-phase ceramics become technical problems to be solved in the present day.
Disclosure of Invention
Accordingly, the present invention is directed to a YTaO 4 /Y3TaO 7 The biphase ceramic, the preparation method and the application thereof are used for improving the thermal property and the mechanical property of YTaO4 single-phase ceramic.
In a first aspect, the present invention provides a method for preparing a biphase ceramic, comprising the steps of:
s1, preparing YTaO by adopting inverse microemulsion method 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, mixing YTAO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder is obtained to obtain mixed powder, then the mixed powder is subjected to ball milling, grinding and sieving, and then discharge plasma sintering is carried out to obtain the biphase ceramic.
Optionally, in step S1, the YTaO is prepared by an inverse microemulsion method 4 Single-phase powder and Y 3 TaO 7 The single-phase powder comprises:
s1.1, mixing a nonionic surfactant, a cosurfactant and an oil phase, then adding yttrium nitrate solution, and stirring until the solution is colorless and transparent to obtain inverse microemulsion;
s1.2 YTaO 4 And Y 3 TaO 7 Respectively dissolving in the same oil phase as in step A to obtain YTaO 4 Oil phase solution and Y 3 TaO 7 Oil phase solution, YTAO 4 Oil phase solution and Y 3 TaO 7 Respectively dropwise adding the oil phase solution into the reverse microemulsion obtained in the step S1.1, respectively stirring, centrifuging and drying to obtain YTAO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3 YTaO obtained in step S1.2 4 Precursor and Y 3 TaO 7 Respectively calcining the precursors to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder.
Optionally, in step S1.1, the mass ratio of the nonionic surfactant, the cosurfactant, the oil phase and the yttrium nitrate solution is 5-15:5-20:20-60:5-35, preferably 10-15:10-20:30-60:15-35.
Optionally, in step S1.1, the nonionic surfactant is a fatty alcohol polyoxyethylene ether (i.e., AEO).
Optionally, in the fatty alcohol polyoxyethylene ether, the carbon number of the fatty alcohol is 12-14.
In the present invention, the polymerization degree of the fatty alcohol-polyoxyethylene ether is not limited.
Optionally, in step S1.1, the cosurfactant is ethanol.
Optionally, in step S1.1, the oil phase is petrolatum.
Optionally, in the yttrium nitrate solution in step S1.1, the mass fraction of yttrium nitrate is 5wt% to 15wt%, preferably 10wt% to 15wt%.
Optionally, in step S1.2, the YTaO 4 The mass ratio of the oil phase to the oil phase is 1:5-10, preferably 1:8-10.
Optionally, in step S1.2, the Y 3 TaO 7 The mass ratio of the oil phase to the oil phase is 1:10-20, preferably 1:15-20.
Optionally, in step S1.2, the YTaO 4 The mass ratio of the oil phase solution to the nonionic surfactant is 1:5-15, preferably 1:10-15.
Optionally, in step S1.2, the Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant is 0.2-0.25:5-15, preferably 0.22-0.25:5-15.
Optionally, in step S1.2, the stirring speed is 80-150rad/min, preferably 100-150rad/min; the stirring time is 30-40min, preferably 35-40rad/min.
Optionally, in step S1.2, the rotational speed of the centrifugation is 4000-6000rad/min, preferably 5000-6000rad/min; the centrifugation time is 4-10min, preferably 5-10min.
Optionally, in step S1.2, the drying temperature is 60-100 ℃, preferably 70-100 ℃.
Optionally, in step S1.3, the temperature of the calcination is 900-1400 ℃, preferably 1000-1400 ℃; the calcination time is 5 to 12 hours, preferably 6 to 12 hours.
Optionally, in step S2, the YTaO 4 Single-phase powder and Y 3 TaO 7 The mol ratio of the single-phase powder is x: (1-x), wherein x is more than or equal to 0.35 and less than or equal to 0.65.
Optionally, in step S2, the ball milling medium used in the ball milling process is absolute ethanol.
Optionally, in step S2, the mass ratio of the ball milling medium to the mixed powder adopted in the ball milling process is 35-45:1, preferably 40-45:1.
optionally, in the ball milling process in step S2, the ball milling is performed for 15-25min transversely at a rotational speed of 140-160rad/min, followed by performing the ball milling for 15-25min longitudinally at a rotational speed of 15-25rad/min, and performing the ball milling for 10-15h in a cycle, preferably performing the ball milling for 20-25min transversely at a rotational speed of 150-160rad/min, followed by performing the ball milling for 20-25min longitudinally at a rotational speed of 20-25rad/min, and performing the ball milling for 12-15h in a cycle.
Optionally, in step S2, a 325-400 mesh screen, preferably a 350-400 mesh screen, is passed.
Optionally, in step S2, the temperature of the spark plasma sintering is 1450-1550 ℃, preferably 1500-1550 ℃; the pressure of spark plasma sintering is 60-80MPa, preferably 70-80MPa; the spark plasma sintering time is 5-15min, preferably 6-15min.
Optionally, in step S2, the density of the biphase ceramic is greater than or equal to 98%.
In another aspect, the present invention also provides a biphase ceramic prepared by the preparation method as described above.
In a further aspect, the invention also provides the use of the biphase ceramic prepared by the preparation method in an aeroengine or gas turbine.
As described above, YTaO of the present invention 4 /Y 3 TaO 7 The biphase ceramic and the preparation method and the application thereof have the following beneficial effects:
(1) In the invention, YTaO is used 4 Introducing Y for the main phase 3 TaO 7 As a second phase, or in Y 3 TaO 7 Introduction of YTaO for the Master phase 4 As a second phase, the thermal property and mechanical property of the material are improved. For example, with YTaO 4 Introducing Y for the main phase 3 TaO 7 YTaO as the second phase 4 Is larger in grain size and Y 3 TaO 7 Is smaller by introducing Y 3 TaO 7 The grains are thinned, namely, the phase change of the single-phase rare earth tantalate at high temperature is weakened or even completely counteracted by introducing the second-phase material, so that the hardness and fracture toughness of the material are effectively improved, the thermal conductivity is reduced along with the reduction of the grain size, and the limitations of the traditional single-phase rare earth tantalate in terms of mechanical property and thermal property are solved.
(2) The biphase ceramic has the advantages of high density, high purity, fine and uniform grain size, low heat conductivity, high hardness, excellent fracture toughness and the like.
(3) In the invention, the nonionic surfactant has excellent wetting and washing functions, high stability, no ionization in aqueous solution, no influence of strong electrolyte, strong acid and strong alkali, and no influence of calcium and magnesium ions in hard water; the cosurfactant can greatly maintain the activity of the nonionic surfactant at all times; the oil phase can effectively avoid ionization of yttrium nitrate solution in water; the tantalum alkoxide is in the water core of the reverse microemulsion to generate gel through hydrolysis and polycondensation reaction, so that yttrium element is wrapped in the gel, the purity of a reactant is effectively improved, the purity of a prepared reaction product is further improved, and the tantalum alkoxide is low in cost and easy to dissolve in an oil phase.
(4) According to the invention, the oil phase can effectively reduce the loss of yttrium element and tantalum alkoxide, so that the yield is improved and the production cost is reduced.
(5) According to the invention, the colorless transparent reverse microemulsion is used as a medium to prepare the tantalate powder, the reverse microemulsion can improve the uniformity and the dispersibility of the powder, and the prepared powder has small particle size.
(6) The invention has the advantages of low cost of raw materials, high stability and no potential safety hazard in the preparation process.
Drawings
FIG. 1 is an XRD diffraction pattern of the biphasic ceramic prepared in example 1, in which the abscissa 2Theta is the diffraction angle and the ordinate Intensity is the Intensity of the diffraction peak;
FIG. 2 is an SEM image of a biphasic ceramic prepared according to example 1;
FIG. 3 is an SEM image of a biphasic ceramic prepared according to example 3;
FIG. 4 is a DSC result chart of example 3 and comparative example 1;
FIG. 5 is a graph showing the results of hardness and fracture toughness measurements for examples 1-3 and comparative examples 1-2;
FIG. 6 is a graph showing Young's modulus test results of examples 1-3 and comparative examples 1-2.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. In the present invention, unless otherwise specified, "wt%" is mass%.
The invention provides a preparation method of biphase ceramic, which comprises the following steps: .
S1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant ethanol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 5-15wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain reverse microemulsion, wherein the mass ratio of the nonionic surfactant fatty alcohol polyoxyethylene ether, the cosurfactant ethanol, the oil phase vaseline and the yttrium nitrate solution is 5-15:5-20:20-60:5-35;
s1.2 YTaO 4 The mass ratio is 1:5-10 is dissolved in oil phase vaseline to obtain YTaO 4 An oil phase solution; y is set to 3 TaO 7 The mass ratio is 1:10-20 of the mixture is dissolved in oil phase vaseline to obtain Y 3 TaO 7 An oil phase solution;
YTaO is to 4 Oil phase solution and Y 3 TaO 7 The oil phase solution is respectively added into the reverse microemulsion obtained in the step S1.1 drop by drop, stirred for 30 to 40 minutes at the rotating speed of 80 to 150rad/min, and YTaO is added 4 The mass ratio of the oil phase solution to the nonionic surfactant is 1:5-15, Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant is 0.2-0.25:5-15; centrifuging at 4000-6000rad/min for 4-10min, and drying at 60-100deg.C to obtain YTaO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3 YTaO obtained in step S1.2 4 Precursor and Y3TaO 7 Calcining the precursor at 900-1400 deg.C for 5-12 hr to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, mixing YTAO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder to obtain mixed powder, YTaO 4 Single-phase powder and Y 3 TaO 7 The mol ratio of the single-phase powder is x: (1-x), wherein x is more than or equal to 0.35 and less than or equal to 0.65; then ball milling is carried out on the mixed powder by taking absolute ethyl alcohol as a ball milling medium, and the mass ratio of the absolute ethyl alcohol of the ball milling medium to the mixed powder is 35-45:1, in the ball milling process, firstly, transversely ball milling for 15-25min at the rotating speed of 140-160rad/min, then longitudinally ball milling for 15-25min at the rotating speed of 15-25rad/min, and circularly performing the ball milling for 10-15h; followed by grindingSieving with 325-400 mesh sieve, and sintering with discharge plasma at 1450-1550 deg.C and 60-80MPa for 5-15min to obtain the final product.
The present invention will be described in detail with reference to specific exemplary examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, as many insubstantial modifications and variations are within the scope of the invention as would be apparent to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
The biphase ceramic is prepared by the following steps:
s1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether (the carbon number of fatty alcohol is 12, the polymerization degree is 5), cosurfactant absolute ethyl alcohol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 5wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain inverse microemulsion, wherein the mass percentage of nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant absolute ethyl alcohol, oil phase vaseline and yttrium nitrate solution is 10wt%:20wt%:60wt%:10wt%;
s1.2 YTaO 4 The mass ratio is 1:5 dissolving in oil phase vaseline to obtain YTaO 4 An oil phase solution; y is set to 3 TaO 7 The mass ratio is 1:10 is dissolved in oil phase vaseline to obtain Y 3 TaO 7 Oil phase solution
YTaO is to 4 Oil phase solution and Y 3 TaO 7 The oil phase solution is respectively added into the reverse microemulsion obtained in the step S1.1 drop by drop, YTaO 4 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 1:5, Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 0.2:5, a step of; then stirring at a rotation speed of 80rad/minStirring for 40min; centrifuging at 4000rad/min for 10min, and drying at 60deg.C until no liquid is present to obtain YTaO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3, the YTaO obtained in the step S1.2 is processed 4 Precursor and Y 3 TaO 7 Calcining the precursor at 1000 ℃ for 5 hours to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, according to the mole ratio of 0.6:0.4 Mixed YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder, namely mixed powder, is obtained, and then the mixed powder is placed in a ball milling tank filled with absolute ethyl alcohol serving as a ball milling medium and is uniformly mixed, wherein the mass ratio of the absolute ethyl alcohol to the mixed powder is 35:1, firstly carrying out transverse ball milling for 25min at the rotating speed of 140rad/min, then carrying out longitudinal ball milling for 25min at the rotating speed of 15rad/min, and carrying out circular ball milling for 10h in total; grinding and sieving with 400 mesh sieve, and sintering with discharge plasma at 1450 deg.C and 75MPa for 10min to obtain the biphasic ceramic.
Example 2
The biphase ceramic is prepared by the following steps:
s1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether (the carbon number of fatty alcohol is 14, the polymerization degree is 7), cosurfactant absolute ethyl alcohol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 15wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain inverse microemulsion, wherein the mass percentage of nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant absolute ethyl alcohol, oil phase vaseline and yttrium nitrate solution is 15wt%:15 wt.%: 60wt%:10wt%;
s1.2 YTaO 4 The mass ratio is 1:10 is dissolved in oil phase vaseline to obtain YTaO 4 An oil phase solution; y is set to 3 TaO 7 The mass ratio is 1:20 is dissolved in oil phase vaseline to obtain Y 3 TaO 7 Oil phase solution
YTaO is to 4 Oil phase solution and Y 3 TaO 7 The oil phase solution is respectively added into the step S1 drop by drop1 in the inverse microemulsion obtained in the step 1, YTaO 4 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 1:15, Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 0.25:15; stirring for 30min at 150rad/min; centrifuging at 6000rad/min for 4min, and drying at 100deg.C until no liquid is present to obtain YTaO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3 YTaO obtained in step S1.2 4 Precursor and Y 3 TaO 7 Calcining the precursor at 1000 ℃ for 5 hours to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, according to the mole ratio of 0.5:0.5 Mixed YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder, namely mixed powder, is obtained, and then the mixed powder is placed in a ball milling tank filled with absolute ethyl alcohol serving as a ball milling medium and is uniformly mixed, wherein the mass ratio of the absolute ethyl alcohol to the mixed powder is 45:1, firstly carrying out transverse ball milling for 15min at a rotating speed of 160rad/min, then carrying out longitudinal ball milling for 15min at a rotating speed of 25rad/min, and carrying out circular ball milling for 15h in total; grinding, sieving with 400 mesh sieve, and sintering with discharge plasma at 1500deg.C and 70MPa for 10min to obtain biphase ceramic.
Example 3
The biphase ceramic is prepared by the following steps:
s1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether (the carbon number of fatty alcohol is 13, the polymerization degree is 9), cosurfactant absolute ethyl alcohol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 12wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain inverse microemulsion, wherein the mass percentage of nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant absolute ethyl alcohol, oil phase vaseline and yttrium nitrate solution is 10wt%:20wt%:60wt%:10wt%;
s1.2 YTaO 4 The mass ratio is 1:8 dissolving in oil phase vaseline to obtain YTaO 4 An oil phase solution; y is set to 3 TaO 7 The mass ratio is 1:8 dissolving in oil phase vaseline to obtain Y 3 TaO 7 Oil phase solution
YTaO is to 4 Oil phase solution and Y 3 TaO 7 The oil phase solution is respectively added into the reverse microemulsion obtained in the step S1.1 drop by drop, YTaO 4 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 1:10, Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 0.25:10; stirring at 120rad/min for 35min; centrifuging at 5000rad/min for 6min, and drying at 80deg.C until no liquid is present to obtain YTaO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3 YTaO obtained in step 1.2 4 Precursor and Y 3 TaO 7 Calcining the precursor at 1000 ℃ for 5 hours to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, according to the mole ratio of 0.4:0.6 Mixed YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder, namely mixed powder, is obtained, and then the mixed powder is placed in a ball milling tank filled with absolute ethyl alcohol and is uniformly mixed, wherein the mass ratio of the absolute ethyl alcohol to the mixed powder is 40:1, firstly carrying out transverse ball milling for 20min at a rotating speed of 150rad/min, then carrying out longitudinal ball milling for 20min at a rotating speed of 20rad/min, and carrying out circulation to carry out total ball milling for 12h; grinding, sieving with 400 mesh sieve, and sintering with discharge plasma at 1550 deg.C and 80MPa for 10min to obtain the biphasic ceramic.
The biphase ceramic prepared in this example was subjected to electron microscope Scanning (SEM) and the results are shown in fig. 3.
Comparative example 1
The ceramic is prepared by the following steps:
s1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether (the carbon number of fatty alcohol is 12, the polymerization degree is 5), cosurfactant absolute ethyl alcohol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 5wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain inverse microemulsion, wherein the mass percentage of nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant absolute ethyl alcohol, oil phase vaseline and yttrium nitrate solution is 10wt%:20wt%:60wt%:10wt%;
s1.2 YTaO 4 The mass ratio is 1:5 dissolving in oil phase vaseline to obtain YTaO 4 An oil phase solution;
YTaO is to 4 Dropwise adding the oil phase solution into the reverse microemulsion obtained in the step S1.1, and YTaO 4 The mass ratio of the oil phase solution to the nonionic surfactant fatty alcohol-polyoxyethylene ether is 1:5, a step of; centrifuging at 4000rad/min for 10min, and drying at 60deg.C until no liquid is present to obtain YTaO 4 A precursor;
s1.3 YTaO obtained in step S1.2 4 Calcining the precursor at 1000 ℃ for 5 hours to obtain YTaO 4 Single-phase powder;
s2, YTAO 4 Grinding the single-phase powder, sieving with 400 mesh sieve, and sintering with discharge plasma at 1450 deg.C and 75MPa for 10min to obtain YTaO 4 Single phase ceramics.
Comparative example 2
This comparative example differs from example 1 in that: YTaO is prepared by adopting a common high-temperature solid-phase method 4 Single-phase powder and Y3TaO 7 The single-phase powder comprises the following specific steps:
s1.2 YTaO 4 Placing the powder in a ball milling tank, adding absolute ethyl alcohol, absolute ethyl alcohol and YTaO into the ball milling tank 4 The mass ratio of the powder is 35-45:1, ball milling and mixing uniformly, and placing the uniformly mixed materials in a drying oven at 80 ℃ for drying for 10 hours to obtain YTaO 4 A precursor;
y is set to 3 TaO 7 Placing the powder in a ball milling tank, adding absolute ethyl alcohol, absolute ethyl alcohol and YTaO into the ball milling tank 4 The mass ratio of the powder is 35:1, ball milling and mixing uniformly, and placing the uniformly mixed materials in a drying oven at 60 ℃ to dry until no liquid exists, thus obtaining Y 3 TaO 7 A precursor;
s1.3, the step S1.2 is carried outTo YTaO 4 Precursor and Y 3 TaO 7 Calcining the precursor at 1000 ℃ for 5 hours to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder.
Comparative example 3
Remove YTaO 4 Single-phase powder and Y 3 TaO 7 The mol ratio of the single-phase powder is 0.3: a biphasic ceramic was prepared in the same manner as in example 1, except for 0.7.
Comparative example 4
Remove YTaO 4 Single-phase powder and Y 3 TaO 7 The mol ratio of the single-phase powder is 0.7: 0.3A biphase ceramic was prepared in the same manner as in example 1.
Performance detection
The biphase ceramic prepared in example 1 was subjected to X-ray diffraction (XRD), the parameters of which were set as: the scanning range 2-theta is 10 DEG-60 DEG, the number of steps is 0.01 DEG, the scanning speed is 5 DEG/min, and the result is shown in figure 1.
As can be seen from FIG. 1, Y in the ceramic obtained in example 1 3 TaO 7 Phase and YTaO 4 The phases coexist, i.e. the ceramic of the invention is a biphase ceramic.
The biphasic ceramics prepared in example 1 and example 3 were each subjected to electron microscope Scanning (SEM) and the results are shown in fig. 2 to 3 (magnification 2000).
As can be seen by comparing fig. 2 and 3, the small-sized grains are significantly more than the large-sized grains in fig. 3, whereas fig. 2 is the opposite. The results indicate that Y in the ceramic 3 TaO 7 Is higher than YTaO 4 When the content is increased, the number of small-sized grains is increased.
For the biphase ceramic prepared in example 3 and TaO prepared in comparative example 1 4 The single-phase ceramics respectively perform differential thermal scanning (DSC), and the parameters of the differential thermal scanning are set as follows: the test temperature was 100-1400℃and the heating rate was 5℃per minute, and the results are shown in FIG. 4.
The density, purity, hardness, young's modulus, fracture toughness and thermal conductivity of the ceramics obtained in examples 1 to 3 and comparative examples 1 to 4 were examined, and the results are shown in Table 1 and FIGS. 5 to 6;
the method for detecting the density comprises the following steps: measuring actual density of sample by Archimedes drainage method, and weighing sample for the first time to obtain mass m 1 The method comprises the steps of carrying out a first treatment on the surface of the The sample is put into deionized water to be weighed with the mass m 2 Finally taking out the sample, wiping off the water on the surface, and weighing the mass m 3 The actual density of the sample can be calculated according to the following formula: ρ=m 1 /(m 3 -m 2 )*1g/cm 3 Actual density and theoretical density (according to Y 3 TaO 7 And YTaO 4 The specific formula is that the respective density and molar ratio are calculatedWherein ρ is 0 Is the theoretical density in g/cm 3 X and 1-X are YTaO respectively 4 And Y 3 TaO 7 In mol (1 mol in total) M 1 And M 2 YTaO respectively 4 And Y 3 TaO 7 The relative molecular mass of (C) is expressed in g/mol, ρ 1 And ρ 2 Other than YTaO 4 And Y 3 TaO 7 Is expressed in g/cm 3 ) The ratio of (2) is the density;
the purity detection method comprises the following steps: analysis of the diffraction peaks by X-ray diffraction detection for other miscellaneous peaks (miscellaneous peaks refer to the removal of Y) 3 TaO 7 And YTaO 4 The outer peak) exists, and the number percentage of the impurity peak is calculated to obtain the purity;
the hardness and fracture toughness detection method comprises the following steps: according to GB/T4340.1-2009 Vickers hardness test section 1: the test method detects the hardness of a sample, and the sample is polished before the test to obtain a smooth plane, so that the appearance of an indentation can be observed to calculate the hardness, the load used in the test process is 4.9N, and the load time is 10s; in the hardness detection process, measuring the crack length through an automatic measurement function of an instrument (HMV-G-FA, shimadzu) and reading a fracture toughness detection result;
the Young modulus detection method comprises the following steps: the sample is stably placed on an ultrasonic reflection method sound velocity tester to directly measureLongitudinal sound velocity V of sample L And transverse sound velocity V T Then according to the formulaCalculating the Young's modulus (E), wherein E is Young's modulus in GPa and ρ is the actual density of the specimen in g/cm 3 ，V L And V T The longitudinal sound velocity and the transverse sound velocity are respectively in m/s;
the detection method of the thermal conductivity comprises the following steps: the ceramics prepared in examples 1 to 3 and comparative examples 1 to 4 were polished into round sheets of phi 6X 1mm, and the thermal conductivity was measured by a laser thermal conductivity meter, and the thermal conductivity of each sample was measured at 1200 ℃.
TABLE 1 detection results
As can be seen from the data of examples 1-3 of Table 1, following Y 3 TaO 7 The content is increased, the hardness and Young's modulus of the biphase ceramic are increased, the fracture toughness is more excellent, and the thermal conductivity is lower. The results indicate that the mechanical and thermal properties of the material can be improved by introducing a second phase.
As can be seen from the data in FIG. 4 and Table 1 (examples 1-3 compared to comparative example 1), YTAO is superior to the duplex ceramic 4 The single-phase ceramics have poor properties and exhibit phase transitions at 1380 ℃. The results indicate that YTaO 4 The performance degradation of single phase ceramics may be caused by phase changes at 1380 c.
As is clear from Table 1, the YTAO obtained in examples 1 to 3 was compared with comparative example 2 4 /Y 3 TaO 7 The two-phase ceramic has higher purity and higher density, and the performances in all aspects are obviously improved.
As can be seen from table 1, the biphasic ceramics of example 1 have significantly improved properties in all respects compared to comparative examples 3 and 4. The results indicate that YTaO is controlled 4 Single-phase powder and Y 3 TaO 7 The mol ratio of the single-phase powder is x: (1-x), wherein x is 0.35.ltoreq.0.65, can be remarkableThe thermal property and the mechanical property of the material are improved.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (3)
1. A method for preparing a biphase ceramic, comprising the steps of:
s1, preparing YTaO by adopting inverse microemulsion method 4 Single-phase powder and Y 3 TaO 7 Single-phase powder:
s1.1, mixing nonionic surfactant fatty alcohol polyoxyethylene ether, cosurfactant ethanol and oil phase vaseline, then adding yttrium nitrate solution with the mass fraction of 5-15wt% of yttrium nitrate, and stirring until the solution is colorless and transparent to obtain reverse microemulsion, wherein the mass ratio of the nonionic surfactant fatty alcohol polyoxyethylene ether, the cosurfactant ethanol, the oil phase vaseline and the yttrium nitrate solution is 5-15:5-20:20-60:5-35;
s1.2 YTaO 4 The mass ratio is 1:5-10 is dissolved in oil phase vaseline to obtain YTaO 4 An oil phase solution; y is set to 3 TaO 7 The mass ratio is 1:10-20 of the mixture is dissolved in oil phase vaseline to obtain Y 3 TaO 7 An oil phase solution;
YTaO is to 4 Oil phase solution and Y 3 TaO 7 The oil phase solution is respectively added into the reverse microemulsion obtained in the step S1.1 drop by drop, stirred for 30 to 40 minutes at the rotating speed of 80 to 150rad/min, and YTaO is added 4 The mass ratio of the oil phase solution to the nonionic surfactant is 1:5-15, Y 3 TaO 7 The mass ratio of the oil phase solution to the nonionic surfactant is 0.2-0.25:5-15; centrifuging at 4000-6000rad/min for 4-10min, and drying at 60-100deg.C to obtain YTaO 4 Precursor and Y 3 TaO 7 A precursor;
s1.3 YTaO obtained in step S1.2 4 Precursor and Y 3 TaO 7 Calcining the precursor at 900-1400 deg.C for 5-12 hr to obtain YTaO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder;
s2, mixing YTAO 4 Single-phase powder and Y 3 TaO 7 Single-phase powder to obtain mixed powder, YTaO 4 Single-phase powder and Y 3 TaO 7 The mole ratio of the single-phase powder isx：(1-x) Wherein, the content of the active ingredients is less than or equal to 0.35 percentxLess than or equal to 0.65; then ball milling is carried out on the mixed powder by taking absolute ethyl alcohol as a ball milling medium, and the mass ratio of the absolute ethyl alcohol of the ball milling medium to the mixed powder is 35-45:1, in the ball milling process, firstly, transversely ball milling for 15-25min at the rotating speed of 140-160rad/min, then longitudinally ball milling for 15-25min at the rotating speed of 15-25rad/min, and circularly performing the ball milling for 10-15h; grinding and sieving with 325-400 mesh sieve, and sintering with spark plasma at 1450-1550 deg.C and 60-80MPa for 5-15min to obtain the final product.
2. The biphasic ceramic prepared by the preparation method according to claim 1.
3. Use of the biphase ceramic produced by the production method according to claim 1 in an aeroengine or a gas turbine.
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