CN107032788B - Preparation method of submicron-grade rare earth zirconate ceramic block material - Google Patents
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Abstract
The invention relates to a preparation method of a submicron-grade rare earth zirconate ceramic block material, belonging to the technical field of inorganic non-metallic materials. Carrying out chemical coprecipitation reaction on a nitric acid solution of rare earth element oxide and an aqueous solution of zirconium oxychloride in excessive ammonia water to obtain precursor powder; and pre-calcining the obtained precursor powder, and sintering by using a spark plasma sintering technology to obtain the rare earth zirconate ceramic block material. The method provided by the invention utilizes the advantages of low sintering temperature and short heating time of the spark plasma sintering technology to inhibit the growth of crystal grains, and the density reaches more than 92%; the method has simple process and short preparation period, and can obtain the high-purity phase ceramic material without adding a sintering aid.
Description
Technical Field
The invention relates to a preparation method of a rare earth zirconate ceramic block material, in particular to a preparation method of a submicron rare earth zirconate ceramic block material, belonging to the technical field of inorganic non-metallic materials.
Background
With the development of aviation gas turbines in the direction of high flow ratio, high thrust-weight ratio and high inlet temperature, the temperature and pressure of gas in a combustion chamber are continuously increased, and the existing high-temperature alloy and cooling technology are difficult to meet the requirements. Therefore, the technology of using high-temperature structural materials alone cannot meet the urgent requirement of rapid development of advanced aeroengines.
Research shows that the addition of the thermal barrier coating with the thickness of 100-500 microns and good performance on the surface of the high-temperature alloy can reduce the surface of the high-temperature alloy by 100-200 ℃, so that the aeronautic gas turbine can be normally used at the temperature exceeding the melting point (1300 ℃) of the high-temperature alloy, thereby greatly improving the efficiency and the performance of the engine, and therefore, the thermal barrier coating is a key material of high-temperature components of aerospace engines and gas turbines. The traditional thermal barrier coating material YSZ with yttria partially stabilized widely used at present has the phenomena of aggravation of phase change, easy sintering and the like at high temperature (above 1200 ℃), and further causes that the coating fails to meet the current use requirements.
Rare earth zirconate Ln2Zr2O7The ceramic is a new thermal barrier coating candidate due to the advantages of low thermal conductivity, high service temperature, good high-temperature phase stability and the likeHowever, rare earth zirconate has the defects of high brittleness, insufficient toughness and the like, and the wide popularization and application of the rare earth zirconate are severely restricted. The nano-crystallization is one of the methods for effectively solving the brittleness problem of the rare earth zirconate ceramics at present. The research on the relationship among the grain size, the thermal conductivity, the fracture toughness and the like by adopting the rare earth zirconate ceramic block is a more efficient mode, but in the sintering and densifying process of the rare earth zirconate ceramic, the grains inevitably grow up along with the higher sintering temperature and the longer sintering time, and the denser nano ceramic block cannot be formed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a submicron-grade rare earth zirconate ceramic block material, which can maintain the submicron grain size of original powder under the condition of obtaining higher-density ceramic and avoid the severe growth of grains during high-temperature sintering; the density of the prepared rare earth zirconate ceramic reaches more than 92 percent, and the grain size is 300-800 nm, so that the grain size can be used for researching the performance of the rare earth zirconate ceramic block material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a submicron-scale rare earth zirconate ceramic block material comprises the following specific steps:
step 1, dissolving the oxide of the rare earth element in dilute nitric acid, and then adding ZrOCl2·8H2O aqueous solution to obtain mixed solution; dropwise adding the mixed solution into excessive ammonia water to perform chemical coprecipitation reaction, wherein the pH of a reaction system is 10-11 after the reaction is finished, and washing, filtering and drying precipitates generated by the reaction to obtain precursor powder;
and 3, putting the powder II into a graphite mold, putting the graphite mold into a discharge plasma sintering furnace, applying a pressure of 40-50 MPa in the axial direction of the graphite mold, heating to 1200-1400 ℃ at a heating rate of 100-150 ℃/min, maintaining the pressure and the temperature for 5-10 min, and cooling along with the furnace, wherein the solid in the graphite mold is the submicron-scale rare earth zirconate ceramic block material.
In the mixed solution in the step 1, the molar ratio of the rare earth element to the zirconium element is 1: 1; the grain size of the submicron-scale rare earth zirconate ceramic block material is 300-800 nm.
The rare earth elements in the rare earth zirconate ceramic block material are preferably Sm, Sc, Y, La, Nd, Eu, Gd, Dy, Er, Yb or Lu.
In the step 2, the ball milling is preferably carried out for 10min to 20min at the speed of 300r/min to 400 r/min.
Has the advantages that:
(1) the invention provides a high-density submicron A2Zr2O7A process for preparing the (rare-earth zirconate) ceramic block features that the SPS (spark plasma sintering) technique is used to suppress A2Zr2O7Crystal grain growth of, prepared A2Zr2O7The grain size in the ceramic material is 300 nm-800 nm, and the density reaches more than 92 percent, thereby solving the problem that A is not less than2Zr2O7The crystal grains grow violently in the sintering and compacting process of the material.
(2) The preparation method is simple, the preparation period is short, and the high-purity phase A can be obtained without adding a sintering aid2Zr2O7A ceramic material.
Drawings
FIG. 1 is Sm prepared in example 12Zr2O7Scanning Electron Microscope (SEM) image of the powder before sintering.
FIG. 2 is a submicron Sm prepared in example 12Zr2O7X-ray diffraction (XRD) pattern of the ceramic bulk material.
FIG. 3 is a submicron Sm prepared in example 12Zr2O7Cross-sectional Scanning Electron Microscope (SEM) images of the ceramic bulk material.
FIG. 4 is a submicron La prepared in example 22Zr2O7X-ray diffraction pattern of the ceramic bulk material.
FIG. 5 is a submicron La prepared in example 22Zr2O7Scanning electron microscope image of the cross section of the ceramic block material.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The reagents used in the following examples are shown in the following table:
the instruments used in the following examples are shown in the following table:
the density calculation formula is as follows: density ═ m1×DL)/((m3-m2) XD) X100%; wherein m is1Is the dry weight of the block, m2Is the floating weight of a block, m3Is a block of wet weight, DLIs the density of water and D is the theoretical density of the material.
Example 1
Submicron Sm2Zr2O7Preparing a ceramic block material:
(1) 1000g of ZrOCl2·8H2O was dissolved in 950mL of deionized water, and 540g of Sm was added2O3Dissolving in 3000mL of dilute nitric acid with the mass fraction of 30%, and then mixing the aqueous solution of zirconium oxychloride with the nitric acid solution of samarium oxide to obtain a mixed solution; then, the mixed solution is dripped into 2000mL of 17% ammonia water by mass fraction for chemical coprecipitation reaction, the pH of the reaction system is 10 after the reaction is finished, and precipitates generated by the reaction are washed, filtered and placed in an oven for drying to obtain precursor powderA body;
(2) placing the obtained precursor powder in a planetary ball mill with a ball-to-material ratio of 4:1, carrying out ball milling at 300r/min for 20min, and then screening the ball-milled powder through a test sieve to obtain powder with the particle size of 20-80 μm; then calcining the powder at 1250 ℃ for 4h to obtain Sm2Zr2O7Powder;
(3) 3g of Sm obtained in step (2)2Zr2O7Putting the powder into a graphite die with the inner diameter of phi 20.4mm and the diameter of a pressure head of phi 20mm, then putting the graphite die into a discharge plasma sintering furnace, then applying 40MPa pressure on the graphite die in the axial direction, heating to 1200 ℃ at the heating rate of 100 ℃/min, maintaining the pressure and the temperature for 5min, and cooling along with the furnace, wherein the solid in the graphite die is the submicron Sm2Zr2O7A ceramic bulk material.
To the prepared submicron Sm2Zr2O7The ceramic block material is characterized, and the results are as follows:
as can be seen from the XRD spectrum in figure 2, the prepared ceramic block material is pure Sm2Zr2O7Phase, no other impurity phase. Sm can be seen in the cross-sectional SEM image in FIG. 32Zr2O7The grain size of the ceramic block material is 400 nm-600 nm, and Sm is added before sintering2Zr2O7Compared with the particle size of the powder (as shown in figure 1), the sintered crystal grains do not grow obviously. The average density was 93.7% as measured by archimedes drainage.
Example 2
Submicron La2Zr2O7Preparing a ceramic block material:
(1) 1000g of ZrOCl2·8H2O was dissolved in 950mL of deionized water, and 505g of La was added2O3Dissolving in 3200mL of dilute nitric acid with the mass fraction of 30%, and mixing the aqueous solution of zirconium oxychloride with the nitric acid solution of lanthanum oxide to obtain a mixed solution; then the mixed solution is dripped into 2100mL ammonia water with the mass fraction of 17% for chemical coprecipitation reaction, and the pH of the reaction system is 1 after the reaction is finished0.7, washing and filtering precipitates generated by the reaction, and drying the precipitates in an oven to obtain precursor powder;
(2) placing the obtained precursor powder in a planetary ball mill with a ball-to-material ratio of 4:1, carrying out ball milling at 400r/min for 10min, and then screening the ball-milled powder through a test sieve to obtain powder with the particle size of 20-80 microns; calcining the powder at 1200 ℃ for 4h to obtain La2Zr2O7Powder;
(3) 3g of La obtained in step (2)2Zr2O7Putting the powder into a graphite die with the inner diameter of phi 20.4mm and the pressure head diameter of phi 20mm, then putting the graphite die into a discharge plasma sintering furnace, then applying pressure of 45MPa to the graphite die in the axial direction, heating to 1300 ℃ at the heating rate of 100 ℃/min, maintaining the pressure and the temperature for 10min, cooling along with the furnace, wherein the solid in the graphite die is the submicron La2Zr2O7A ceramic bulk material.
For the prepared submicron La2Zr2O7The ceramic block material is characterized, and the results are as follows:
as can be seen from the XRD spectrum in FIG. 4, the prepared ceramic bulk material is pure La2Zr2O7Phase, no other impurity phase. As can be seen from the cross-sectional SEM image in FIG. 5, La2Zr2O7The grain size of the ceramic block material is 300 nm-500 nm, and the La obtained in the step (2)2Zr2O7Compared with the particle size of the powder, the sintered crystal grains do not grow obviously. The average density was 95.7% as measured by archimedes drainage.
Example 3
Submicron Gd2Zr2O7Preparing a ceramic block material:
(1) 1000g of ZrOCl2·8H2O was dissolved in 950mL of deionized water, and 580g of Gd was added2O3Dissolving in 3400mL of dilute nitric acid with the mass fraction of 30%, and then mixing the aqueous solution of zirconium oxychloride with the nitric acid solution of gadolinium oxide to obtain a mixed solution; then the mixed solution is dripped into2400mL of ammonia water with the mass fraction of 17% to perform chemical coprecipitation reaction, the pH value of a reaction system is 10.3 after the reaction is finished, and precipitates generated by the reaction are washed, filtered and placed in an oven to be dried to obtain precursor powder;
(2) placing the obtained precursor powder in a planetary ball mill with a ball-to-material ratio of 4:1, carrying out ball milling at 300r/min for 20min, and then screening the ball-milled powder through a test sieve to obtain powder with the particle size of 20-80 μm; calcining the powder at 1150 deg.C for 3 hr to obtain Gd2Zr2O7Powder;
(3) 3g of Gd obtained in step (2)2Zr2O7Putting the powder into a graphite die with the inner diameter of phi 20.4mm and the pressure head diameter of phi 20mm, then putting the graphite die into a discharge plasma sintering furnace, then putting the graphite die into the discharge plasma sintering furnace, then applying 40MPa pressure on the graphite die in the axial direction, heating to 1400 ℃ at the heating rate of 150 ℃/min, maintaining the pressure and preserving the heat for 5min, and cooling along with the furnace, wherein the solid in the graphite die is the submicron Gd2Zr2O7A ceramic bulk material.
From Gd2Zr2O7The XRD spectrogram of the ceramic block material shows that the prepared ceramic block material is pure Gd2Zr2O7Phase, no other impurity phase. From Gd2Zr2O7In SEM image of cross section of ceramic material, Gd is shown2Zr2O7Has a crystal grain size of 500nm to 700nm, and Gd obtained in the step (2)2Zr2O7Compared with the particle size of the powder, the sintered crystal grains do not grow obviously. The average density was 98.7% as measured by archimedes drainage method.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A preparation method of a submicron-grade rare earth zirconate ceramic block material is characterized by comprising the following steps: the method comprises the following specific steps:
step 1, dissolving the oxide of the rare earth element in dilute nitric acid, and then adding ZrOCl2·8H2O aqueous solution to obtain mixed solution; dropwise adding the mixed solution into excessive ammonia water to perform chemical coprecipitation reaction, wherein the pH of a reaction system is 10-11 after the reaction is finished, and washing, filtering and drying precipitates generated by the reaction to obtain precursor powder;
step 2, ball-milling and crushing the obtained precursor powder, and screening by using a test sieve to obtain powder I with the particle size of 20-80 microns; calcining the powder I at 1100-1250 ℃ for 2-4 h to obtain powder II;
step 3, putting the powder II into a graphite mold, then putting the graphite mold into a discharge plasma sintering furnace, then applying a pressure of 40-50 MPa in the axial direction of the graphite mold, heating to 1200-1300 ℃ at a heating rate of 100-150 ℃/min, maintaining the pressure and the temperature for 5-10 min, and then cooling along with the furnace, wherein the solid in the graphite mold is the submicron-scale rare earth zirconate ceramic block material;
in the mixed solution in the step 1, the molar ratio of the rare earth element to the zirconium element is 1: 1;
the rare earth elements in the rare earth zirconate ceramic block material are Sm, Sc, Y, La, Nd, Eu, Gd, Dy, Er, Yb or Lu;
in the step 2, ball milling and crushing are carried out for 10min to 20min at the speed of 300r/min to 400 r/min.
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