CN112851340A - Ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder and preparation method thereof - Google Patents
Ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder and a preparation method thereof. The preparation method comprises the following steps: s1, preparing a mixed solution of ytterbium salt, gadolinium salt, yttrium salt and zirconium salt solution; s2, adding a precipitator into the mixed solution obtained in the step S1, standing and aging to obtain hydroxide colloid; s3, carrying out cross-flow washing separation and colloidal particle refinement on the obtained hydroxide colloid to obtain hydroxide precipitate; s4, mixing the obtained hydroxide precipitate with a dispersing agent, and then distilling and carbonizing to obtain powder; s5, grinding the powder obtained in the step S4 by a roll crusher, and then calcining at high temperature; and S6, performing jet milling on the powder to obtain nano powder. The nano powder has good high-temperature stability, low thermal conductivity and high thermal expansion coefficient, and the preparation method has the advantages of simple process, less flow, easy control of parameters and suitability for continuous large-scale production.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder and a preparation method thereof.
Background
The thermal barrier coating is a heat-insulating functional coating applied to the surfaces of hot-end components such as blades, combustion chambers and the like of aeroengines and ground gas turbines, and provides heat protection mainly through a low-heat-conductivity ceramic layer on the surface. Yttrium Stabilized Zirconia (YSZ) has high melting point (2700 ℃) and low thermal conductivity (2.1-2.2W/m)-1·K-11273K), high thermal expansion coefficient (11X 10)-6Low density (6.4 g/cm)/K3) The advantages of low elastic modulus (40GPa) and high hardness (14GPa) make the material become the most widely applied and researched thermal barrier coating material at present.
With the development of aero-engines towards higher thrust-weight ratio, lower oil consumption and the like, the design inlet temperature of an engine turbine needs to be further increased, which requires that a thermal barrier coating material can be stably used at higher temperature. However, the YSZ materials in wide use at present undergo phase transition at 1200 ℃ or higher, from metastable tetragonal (t') phase to tetragonal (t) and cubic (c) phases, and then to monoclinic (m) phase. The phase transformation process is accompanied by volume expansion of about 5-7%, and internal stress is generated. Meanwhile, the metastable tetragonal phase with higher toughness is converted into the monoclinic phase with lower toughness, so that the crack resistance of the coating is reduced, cracks are easily generated in the coating, and the peeling failure of the coating is further caused. Meanwhile, during high-temperature service, rapid sintering of the YSZ coating can occur, which can lead to the reduction of the heat insulation effect, the increase of the elastic modulus and the reduction of the thermal strain tolerance of the coating, and the continuous deterioration of the high-temperature performance of the coating. Therefore, YSZ materials have not been able to meet the design requirements (requiring inlet temperatures above 1300 ℃) of the new generation of advanced aircraft engines. It is therefore critical to further improve the high temperature phase stability of YSZ materials.
Disclosure of Invention
The invention aims to provide ytterbium, gadolinium and yttrium co-doped nano zirconia powder with better high-temperature stability, low thermal conductivity and high thermal expansion coefficient and a preparation method thereof aiming at the defects in the prior art.
The invention relates to a preparation method of ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder, which comprises the following steps:
s1, preparing ytterbium salt, gadolinium salt, yttrium salt and zirconium salt solutions, mixing the solutions according to different proportions, and continuously stirring the mixed solutions to obtain mixed solutions;
s2, adding a precipitator into the mixed solution obtained in the step S1, standing and aging to obtain hydroxide colloid;
s3, carrying out cross-flow treatment on the obtained hydroxide colloid, carrying out cross-flow washing separation and colloidal particle refinement, and repeatedly cleaning with deionized water to obtain hydroxide precipitate;
s4, mixing the obtained hydroxide precipitate with a dispersing agent, and distilling and carbonizing at a certain temperature in a vacuum environment to obtain powder;
s5, grinding the powder obtained in the step S4 by a roll crusher, and then carrying out high-temperature calcination phase formation treatment at a certain temperature;
and S6, performing jet milling on the calcined powder again to obtain the nano powder.
Further, in step S1, the zirconium salt is zirconium oxychloride, the ytterbium salt, the gadolinium salt, and the yttrium salt are all nitrates, and the mixed solution is doped with ions: the molar ratio of yttrium ions, ytterbium ions and gadolinium ions is in the range of 5: 1: 1-1: 1: 1, the molar ratio of the doping ions to the zirconium ions is 1/24-2/3.
Further, the precipitant in step S2 includes ammonia water, the concentration of the ammonia water is 20 to 50 wt.%, and the PH of the mixed solution after the ammonia water is added should be maintained at PH > 10.
Furthermore, the precipitation time after the precipitant is added in the step S2 should be 0.5-10 h, and the aging time should be more than 12 h.
Further, in the cross-flow washing process described in step S3, the precipitate is repeatedly washed until the PH of the washed supernatant is 7 and no precipitate is generated by reaction with silver nitrate.
Further, the dispersant described in step S4 includes, but is not limited to, alcohols.
Further, alcohols include, but are not limited to, n-butanol, n-propanol, ethylene glycol, isopropanol, isobutanol, or n-pentanol.
Further, the ratio of the dispersant to the hydroxide precipitate in step S4 is 1: 2-4: 1, the distillation and carbonization temperature is 100-200 ℃, and the time is 6-48 h.
Further, the high-temperature calcination phase temperature in the step S5 is 600-1300 ℃, and the calcination time is 1-20 hours.
An ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder is prepared by the preparation method.
The ytterbium, gadolinium and yttrium co-doped nano zirconia powder prepared by the preparation method can show a stable tetragonal phase or cubic phase structure according to different doping contents, has better high-temperature stability (the phase stability temperature can reach more than 1300 ℃), lower thermal conductivity and higher thermal expansion coefficient, can obtain nano powder with the particle size distribution of less than 50nm, and is beneficial to preparing a coating with a nano structure. Therefore, the co-doped nano powder can effectively improve the service temperature and the service life of the thermal barrier coating.
The preparation method of the ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder provided by the invention has the advantages of simple process, less flow, easy control of parameters and suitability for continuous large-scale production.
Drawings
FIG. 1 is a flow chart of the preparation of ytterbium, gadolinium and yttrium codoped nano zirconia ceramic powder of the invention;
FIG. 2 is a schematic diagram of X-ray powder crystal diffraction of powder obtained after sintering at 1100 ℃ for 2 hours in example 1 in a preparation method of ytterbium, gadolinium and yttrium co-doped nano-zirconia ceramic powder according to the invention;
FIG. 3 is a schematic diagram of X-ray powder diffraction of the powder after sintering at 1300 ℃ for 10 hours in example 1 in the preparation method of ytterbium, gadolinium and yttrium co-doped nano-zirconia ceramic powder of the invention;
FIG. 4 is a graph of thermal conductivity versus temperature of the powder of example 2 in the preparation method of ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder according to the invention;
FIG. 5 is a thermal expansion coefficient curve with temperature of the powder of example 2 in the preparation method of ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder according to the invention;
FIG. 6 is a schematic diagram of X-ray diffraction analysis of the nano yttrium-stabilized zirconia powder obtained in comparative example 1;
FIG. 7 is a schematic diagram of X-ray powder diffraction of the nano-yttrium-stabilized zirconia powder obtained in comparative example 1 after being treated at 1300 ℃ for 10 h;
FIG. 8 is a graph showing the thermal conductivity of the nano zirconia powder of comparative example 1 as a function of temperature.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
Example 1:
dissolving yttrium nitrate, ytterbium nitrate and gadolinium nitrate in deionized water to prepare a nitrate solution with the concentration of 0.2 mol/L. Zirconium oxychloride is dissolved in deionized water to prepare a solution with the concentration of 0.5 mol/L. Mixing the four solutions according to a proportion to prepare yttrium ions: ytterbium ion: gadolinium ions: zirconium ion ═ 1: 1: 1: 31.8, and after continuously stirring for 6 hours, adding ammonia water with the concentration of 30 wt.% into the mixed solution dropwise until the pH value of the mixed solution is more than 10. The precipitate was subjected to repeated cross-flow washing with deionized water through the ceramic membrane until the filtrate had a PH of 7 and was free of chloride ions. And (3) mixing the washed hydroxide precipitate and n-butanol according to the mass ratio of 2: 1, mixing and stirring uniformly, and then placing in a drying and distilling device at 150 ℃ for dehydration and distillation treatment. The powder is crushed once by a double-roller machine and then is placed in a high-temperature furnace at 1100 ℃ for calcination for 2 hours. And finally, carrying out secondary treatment on the powder by an airflow mill to obtain ternary co-doped nano zirconia powder particles with the average particle size of 30 nm.
The ternary co-doped nano zirconia powder prepared in example 1 was subjected to X-ray diffraction (XRD) analysis, and the obtained pattern result is shown in fig. 1, and the analysis of the result shows that the sample is tetragonal. The XRD pattern after high-temperature treatment at 1300 ℃ for 10h is shown in figure 2, and no monoclinic phase appears, which indicates that the powder has good high-temperature stability at 1300 ℃.
Example 2:
mixing yttrium nitrate, ytterbium nitrate and gadolinium nitrate solution with the concentration of 0.2mol/L and zirconium oxychloride solution with the concentration of 0.7mol/L in proportion to obtain yttrium ions with the molar ratio: ytterbium ion: gadolinium ions: zirconium ion ═ 19: 11: 11: 79.5, and dropwise adding the mixed solution into sufficient 30% ammonia water by volume concentration, wherein the pH value of the solution is kept between 9 and 10. After titration, standing the solution for precipitation and aging for 12h to obtain hydroxide colloid; and (3) carrying out cross-flow washing on the obtained colloid by adopting an inorganic ceramic membrane technology, wherein a cleaning medium is deionized water. The washing process was repeated until the solution had a pH of 7 and no chloride ions in the solution (no precipitate was formed by adding silver nitrate). And (3) mixing the obtained hydroxide with isopropanol according to the mass ratio of 2: 5, mixing, and placing in a drying and distilling device at 120 ℃ for dehydration treatment. The powder is subjected to primary crushing treatment by a double-roller machine, then is put into a high-temperature furnace at 1000 ℃ for calcining for 2 hours, and is subjected to secondary crushing treatment by an airflow mill, so that the ytterbium, gadolinium and yttrium co-doped nano-zirconia powder with good dispersibility is finally obtained.
The ternary co-doped nano zirconia powder prepared in example 2 was subjected to thermal conductivity and thermal expansion tests. FIG. 4 is a graph showing the thermal conductivity of the ytterbium, gadolinium and yttrium co-doped nano zirconia powder obtained in example 2, which varies with temperature, and the thermal conductivity is 1.35W/mK (room temperature 1450 ℃). FIG. 5 is the thermal expansion coefficient of the ytterbium, gadolinium and yttrium codoped nano zirconia powder obtained in example 2, which varies with temperature, and the thermal expansion is 11X 10-6/K(1400℃)。
As can be seen from the figures 2 to 5, the ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder prepared by the method has good high-temperature stability (the phase stability temperature can reach more than 1300 ℃), low thermal conductivity and high thermal expansion coefficient.
Comparative example 1
Yttrium nitrate with the concentration of 0.2mol/L and zirconium oxychloride solution with the concentration of 0.7mol/L are mixed according to the proportion of 8: 92, mixing to obtain a mixed solution, and dropwise adding the mixed solution into sufficient ammonia water with the volume concentration of 30%, wherein the pH value of the solution is kept between 9 and 10. After titration, standing the solution for precipitation and aging for 12h to obtain hydroxide colloid; and (3) carrying out cross-flow washing on the obtained colloid by adopting an inorganic ceramic membrane technology, wherein a cleaning medium is deionized water. The washing process was repeated until the solution had a pH of 7 and no chloride ions in the solution (no precipitate was formed by adding silver nitrate). And (3) mixing the obtained hydroxide with isopropanol according to the mass ratio of 2: 5, mixing, and placing in a drying and distilling device at 120 ℃ for dehydration treatment. The powder is subjected to primary crushing treatment by a double-roller machine, then is put into a high-temperature furnace at 1000 ℃ for calcining for 2 hours, and is subjected to secondary crushing treatment by an air flow mill, so that the nano yttrium-stabilized zirconia powder is finally obtained.
XRD (X-ray diffraction) test is carried out on the nano yttrium-stabilized zirconia powder obtained in the comparative example 1, X-ray diffraction (XRD) analysis is carried out on the powder, the obtained spectrum result is shown in figure 6, and the result analysis shows that the sample is in a tetragonal phase. The XRD pattern after high temperature treatment at 1300 ℃ for 10h is shown in figure 7, which shows that cubic phase appears, which indicates that the powder has phase change and poor stability. FIG. 8 is a graph showing the thermal conductivity of the nano-zirconia powder of comparative example 1, which varies with temperature, and has a thermal conductivity of 2.69W/mK (room temperature 1000 ℃ C.).
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing ytterbium salt, gadolinium salt, yttrium salt and zirconium salt solutions, mixing the solutions according to different proportions, and continuously stirring the mixed solutions to obtain mixed solutions;
s2, adding a precipitator into the mixed solution obtained in the step S1, standing and aging to obtain hydroxide colloid;
s3, carrying out cross-flow treatment on the obtained hydroxide colloid, carrying out cross-flow washing separation and colloidal particle refinement, and repeatedly cleaning with deionized water to obtain hydroxide precipitate;
s4, mixing the obtained hydroxide precipitate with a dispersing agent, and distilling and carbonizing at a certain temperature in a vacuum environment to obtain powder;
s5, grinding the powder obtained in the step S4 by a roll crusher, and then carrying out high-temperature calcination phase formation treatment at a certain temperature;
and S6, performing jet milling on the calcined powder again to obtain the nano powder.
2. The method according to claim 1, wherein the zirconium salt in step S1 is zirconium oxychloride, the ytterbium salt, the gadolinium salt, and the yttrium salt are nitrates, and the mixed solution is doped with ions: the molar ratio of yttrium ions, ytterbium ions and gadolinium ions is in the range of 5: 1: 1-1: 1: 1, the molar ratio of the doping ions to the zirconium ions is 1/24-2/3.
3. The method according to claim 1, wherein the precipitant in step S2 comprises ammonia water, the concentration of ammonia water is 20-50 wt.%, and the PH of the mixed solution after the ammonia water is added is maintained at PH > 10.
4. The method for preparing ytterbium, gadolinium and yttrium co-doped nano-zirconia ceramic powder according to claim 3, wherein the precipitation time after the precipitant is added in the step S2 is 0.5-10 hours, and the aging time is more than 12 hours.
5. The method for preparing ytterbium, gadolinium and yttrium co-doped nano-zirconia ceramic powder according to claim 4, wherein in the cross-flow washing process of step S3, the precipitate is repeatedly washed until the pH value of the washed supernatant is 7 and no precipitate is generated by reaction with silver nitrate.
6. The method according to claim 5, wherein the dispersant in step S4 includes, but is not limited to, alcohols.
7. The method of claim 6, wherein the alcohol includes but is not limited to n-butanol, n-propanol, ethylene glycol, isopropanol, isobutanol, or n-pentanol.
8. The method for preparing ytterbium, gadolinium and yttrium codoped nano zirconia ceramic powder according to claim 7, wherein the ratio of the dispersing agent to the hydroxide precipitate in step S4 is 1: 2-4: 1, the distillation and carbonization temperature is 100-200 ℃, and the time is 6-48 h.
9. The method for preparing ytterbium, gadolinium and yttrium codoped nano zirconia ceramic powder according to claim 8, wherein the high temperature calcination phase temperature in step S5 is 600-1300 ℃, and the calcination time is 1-20 hours.
10. An ytterbium, gadolinium and yttrium three-element co-doped nano zirconia ceramic powder is characterized in that: prepared by the preparation method as described in any one of claims 1 to 9.
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