CN110980748B - Superfine ytterbium silicate powder material and preparation method and application thereof - Google Patents
Superfine ytterbium silicate powder material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of superfine rare earth silicate powder materials, and particularly relates to an ytterbium silicate powder material for an environmental barrier coating, and a preparation method and application thereof. The granularity of the superfine ytterbium silicate powder material is 30-100nm; the superfine ytterbium silicate powder material is a high-temperature phase structure ytterbium silicate powder material. The preparation method comprises the following steps: preparing an ytterbium-containing cation solution; (2) preparing a urea precipitator solution; (3) heating the reaction solution in water bath, and precipitating; and (4) calcining the precursor to obtain the ytterbium silicate powder material. The method has the advantages of simple and controllable required equipment, simple and controllable process, short preparation period, low industrialization cost and high purity of the powder material, and the obtained ytterbium silicate powder material can be used as an environmental barrier coating material of an aeroengine and a gas turbine.
Description
Technical Field
The invention belongs to the field of preparation of superfine rare earth silicate powder materials, and particularly relates to an ytterbium silicate powder material for an environmental barrier coating, and a preparation method and application thereof.
Technical Field
With the continuous improvement of the thrust-weight ratio of the aero-engine, the traditional alloy material is difficult to meet the harsh use environment. The silicon carbide-based composite material gradually commissions the development direction of high-temperature thermal structural materials of high thrust-weight ratio engines by virtue of the advantages of low density, high strength, high specific modulus, high temperature resistance and the like. The Environmental Barrier Coating (EBC) is a coating protection technology developed for improving the environmental stability of the silicon carbide-based composite material, and aims to resist the corrosion damage of the gas environment of an aircraft engine to a silicon carbide-based composite material member, prevent or reduce the influence of the service environment on the performance of a high-temperature structural material and prolong the service life of a silicon carbide-based high-temperature hot end part.
The rare earth silicate has high melting point (> 1800 ℃), extremely low high temperature oxygen permeability, low thermal conductivity, low thermal expansion coefficient, low silicon activity, low modulus, low saturated vapor pressure and excellent high temperature chemical stabilityThe coating has qualitative, anti-oxyhydrogen corrosion performance and anti-CMAS corrosion performance, has lower volatilization rate in high-speed gas environment, is expected to replace BSAS to become a first choice material of a new generation EBC coating system surface layer, and is an important direction for the development of a future high-performance EBC coating. Among rare earth monosilicates, re = La, ce, pr, nd, pm, sm, eu, gd when the Re atomic radius is large, the rare earth monosilicates are liable to form a low-temperature phase structure (X) 1 -Re 2 SiO 5 ) Phase change occurs at high temperature, and high temperature stability is poor. When the Re atomic radius is small (Re = Dy, ho, er, sc, tm, yb, lu), rare earth monosilicates are liable to form a high-temperature phase structure (X) 2 -Re 2 SiO 5 ). In general, X 2 -Re 2 SiO 5 Has good high-temperature phase stability and low thermal conductivity, has a thermal expansion coefficient similar to that of a silicon-based ceramic material, and is more suitable for EBC materials. In addition, in the rare earth monosilicate having a high-temperature phase structure, most of X 2 -Re 2 SiO 5 A glassy phase is easily formed at high temperatures. Yb of 2 SiO 5 The low-melting-point glass phase is not easy to generate at high temperature, and the high-temperature glass has good high-temperature chemical structure stability. In addition, yb 2 SiO 5 Has a coefficient of thermal expansion of 3.5 to 4.5X 10 -6 ℃ -1 Yb in EBC coating 2 SiO 7 The transition layer is very similar to the Si bottom layer, and is very suitable to be used as a novel EBC coating surface layer material.
Currently, methods commonly used for preparing ytterbium silicate powder include a solid phase method, a hydrothermal method, a sol-gel method and the like. The ytterbium silicate is synthesized by a solid phase method, so that the requirements on equipment and sintering temperature are high, the energy consumption is high, the cost is high, and the impurity content is high easily due to insufficient reaction; the hydrothermal method for preparing ytterbium silicate has higher equipment requirement and harsh reaction conditions; the sol-gel method has complex preparation process, difficult control of process parameters such as aging time and the like, low powder purity and higher temperature required by later heat treatment; the method for preparing the rare earth silicate has no report, has the advantages of simple and easy required equipment, simple and controllable process, short preparation period, low industrialization cost, high purity of powder materials, low synthesis temperature and the like, and has good industrialization advantages.
Disclosure of Invention
Aiming at the defects of the existing preparation method, the invention aims to provide the preparation method of the ytterbium silicate powder material for the environmental barrier coating, which has the advantages of uniform components, high purity, small granularity, narrow particle size distribution, simple and controllable process, short period and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a superfine ytterbium silicate powder material, which has the granularity of 30-100nm. The superfine ytterbium silicate powder material is a high-temperature phase structure ytterbium silicate powder material. The ytterbium silicate is of a high-temperature phase structure and has good thermal stability.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, which comprises the following steps:
(1) Preparing Yb-containing 3+ The solution of (1); is marked as S A ；
(2) Taking silicate ester as a Si source material, dissolving the Si source material in an alcohol-water system to obtain a Si-containing solution, and marking as S B ；
(3) According to the molar ratio of Yb to Si of 20 (10-12); si is preferably in a molar ratio of 20; the solution S obtained in the steps (1) and (2) is A And S B Mixing to obtain a mixed cation solution,
(4) Weighing a proper amount of urea according to a molar ratio of Yb to urea of 1-1, preferably, a molar ratio of Yb to urea of 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating through a water bath gave a gelatinous precipitate solution, denoted as S E (ii) a The temperature of the water bath heating is more than 65 ℃;
(6) Naturally standing and aging the mixed solution containing the colloidal precipitate obtained in the step (5) to completely precipitate; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Putting the precursor colloid into a drying oven for drying, cooling and then grinding or ball-milling to obtain precursor powder; calcining the precursor powder under the condition of oxygen content to obtain an ultra-fine ytterbium silicate powder material; the temperature of the calcination is greater than 1000 ℃.
The invention relates to a method for preparing a superfine ytterbium silicate powder material, which contains Yb 3+ The solution of (a) is prepared by the following steps:
measuring hydrochloric acid or nitric acid, diluting, heating to dissolve ytterbium oxide powder, and completely dissolving the ytterbium oxide powder; adding deionized water to dilute to obtain a rare earth ion solution with a certain concentration, and recording as S A (ii) a Said S A The concentration of the medium rare earth ions is 0.1-2 mol/L; preferably 1mol/L.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, wherein a Si-containing solution in the step (2) is prepared through the following steps:
according to the volume ratio, ethyl orthosilicate: absolute ethanol: n, measuring ethyl orthosilicate, absolute ethyl alcohol and deionized water; uniformly mixing the measured tetraethoxysilane, the absolute ethyl alcohol and the deionized water; the Si-containing solution is obtained and is marked as S B (ii) a M is greater than or equal to 1 and less than or equal to 10, n is greater than or equal to 2 and less than or equal to 10; preferably, m =2 and n is equal to 4.
As a preferred scheme, the preparation method of the ultrafine ytterbium silicate powder material comprises the following steps of (4) preparing a precipitant solution according to a molar ratio of Yb to urea of 1.
According to the preparation method of the ultrafine ytterbium silicate powder material, in the step (4), the urea and the deionized water are mixed, the urea can be completely dissolved into the deionized water, and the concentration of the urea in a mixed solution is more than or equal to 1mol/L.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, wherein in the step (5), the water bath heating temperature is 70-100 ℃, and the heating time is more than 12 hours. Preferably, the water bath heating temperature is 90 ℃, and the heating time is 12h.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, wherein in the step (6), the aging time of a colloidal precipitation solution is 6-24 hours; preferably, the aging time is 12h.
In the step (6), the precipitate is washed by deionized water to ensure that no ammonium ions and chloride ions exist, and then the precipitate is washed by absolute ethyl alcohol.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, in the step (7), the temperature for drying the precipitate is 100-200 ℃, and the drying time is determined according to the actual situation; preferably, the precipitate is dried at 110 ℃ for 12h.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, in the step (7), the calcination time of a precursor is 2-20 h; preferably, the calcination time is 6-10h; the temperature of calcination is 1000-1400 deg.C, preferably 1200 deg.C.
When the preparation method of the ultrafine ytterbium silicate powder material is applied industrially, in the step (1), the hydrochloric acid or the nitric acid is analytically pure, and the diluted hydrochloric acid is preferably selected in consideration of the safety of heating of the nitric acid.
The invention relates to a preparation method of a superfine ytterbium silicate powder material, which is used in industry, in the step (1), in the process of measuring the hydrochloric acid capacity, the volatilization loss of hydrochloric acid heating is considered, so as to ensure Yb 2 O 3 Preferably, hydrochloric acid is measured with a Yb: cl molar ratio of 1.
When the preparation method of the ultrafine ytterbium silicate powder material is industrially applied, in the step (3), the uniformity is ensured by adopting a stirring mode in the preparation process of the mixed cation solution.
According to the preparation method of the superfine ytterbium silicate powder material, the prepared ytterbium silicate powder material has high purity.
Compared with a solid phase method (micron level), a sol-gel method (200-400 nm) and a coprecipitation method, the preparation method of the ultrafine ytterbium silicate powder material is provided by the invention; under otherwise identical conditions; the product obtained by the invention has smaller granularity and narrower particle size distribution.
The invention relates to an application of a superfine ytterbium silicate powder material; said applications include its use as an aircraft engine and/or gas turbine environmental barrier coating; preferably for use as an environmental barrier coating facing material.
The invention has the beneficial effects that:
the method is characterized in that a new method for preparing the ytterbium silicate powder material is invented, the ytterbium silicate powder prepared by the method is uniform in component, high in purity, small in particle size and narrow in particle size distribution, the method is low in equipment requirement, short in preparation period, low in cost, simple in process control and easy to realize industrialization, and the method is an effective method suitable for ytterbium silicate and other rare earth silicates.
Drawings
FIG. 1 is a flow chart of the preparation process of the ytterbium silicate powder material of the environmental barrier coating.
Fig. 2 is an XRD spectrum of ytterbium silicate powder prepared in example 1 of the present invention.
FIG. 3 is a transmission electron micrograph of ytterbium silicate powder prepared in example 1 of the present invention.
Fig. 4 is an XRD spectrum of ytterbium silicate powder prepared in example 2 of the present invention.
FIG. 5 is an XRD spectrum of ytterbium silicate powder prepared in example 3 of the present invention.
FIG. 6 is an XRD spectrum of ytterbium silicate powder prepared in example 4 of the present invention.
FIG. 7 is an XRD pattern of a product prepared according to comparative example 1 of the present invention.
Figure 8 is an XRD pattern of the product of comparative example 2 of the present invention.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
The first embodiment is as follows:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; diluting hydrochloric acid with deionized water, wherein the volume ratio of the hydrochloric acid to the deionized water is 1; yb of 2 O 3 The powder was gradually added to boiling hydrochloric acid solution until the powder was completely dissolved to give YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar amount of cations, weighing a proper amount of urea according to the Yb and urea molar ratio of 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in water bath at 90 deg.C for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitate solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the obtained product is shown in figure 2; fig. 2 shows that the synthesized powder is high-temperature phase ytterbium silicate, and has good crystallinity and no other impurity peak. The TEM image of the obtained powder is shown in FIG. 3; it can be seen from FIG. 3 that the synthesized powder is irregular in shape and has a particle size of 30-100nm.
Example two:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; diluting hydrochloric acid with deionized water, wherein the volume ratio of the hydrochloric acid to the deionized water is 1; yb of 2 O 3 The powder was gradually added to boiling hydrochloric acid solution until the powder was completely dissolved to give YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar weight of cations, according to the molar ratio of Yb to urea being 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in water bath at 90 deg.C for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitation solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the obtained product is shown in figure 4; fig. 4 shows that the synthesized powder is high-temperature phase ytterbium silicate, and has good crystallinity and no other impurity peak.
Example three:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; diluting hydrochloric acid with deionized water, wherein the volume ratio of the hydrochloric acid to the deionized water is 1; yb of 2 O 3 Gradually adding the powder into boiling hydrochloric acid solution until the powder is completely dissolved to obtain YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar amount of cations, according to the molar ratio of Yb to urea being 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in water bath at 90 deg.C for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitation solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the resulting product is shown in fig. 5; fig. 5 shows that the synthesized powder is high-temperature phase ytterbium silicate, and has good crystallinity and no other impurity peak.
Example four:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; adding hydrochloric acidDiluting with deionized water, wherein the volume ratio of hydrochloric acid to deionized water is 1; yb of 2 O 3 The powder was gradually added to boiling hydrochloric acid solution until the powder was completely dissolved to give YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar weight of cations, according to the molar ratio of Yb to urea being 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in water bath at 90 deg.C for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitation solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the resulting product is shown in fig. 6; fig. 6 shows that the synthesized powder is high-temperature phase ytterbium silicate, and has good crystallinity and no other impurity peak.
Comparative example one:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; diluting hydrochloric acid with deionized water, wherein the volume ratio of the hydrochloric acid to the deionized water is 1; yb of 2 O 3 The powder was gradually added to boiling hydrochloric acid solution until the powder was completely dissolved to give YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar amount of cations, according to the molar ratio of Yb to urea being 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in 60 deg.C water bath for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitation solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the resulting product is shown in fig. 7; fig. 7 shows that not only the high-temperature phase ytterbium silicate diffraction peak but also the significant ytterbium oxide diffraction peak indicate that the product purity is not high.
Comparative example two:
(1) Weighing a certain amount of Yb 2 O 3 Taking hydrochloric acid according to a Yb to Cl molar ratio of 1; diluting hydrochloric acid with deionized water, wherein the volume ratio of the hydrochloric acid to the deionized water is 1; yb of 2 O 3 The powder is gradually added to boiling hydrochloric acid solutionDissolving the powder in the solution to obtain YbCl 3 A solution; adding deionized water to adjust solution Yb after cooling 3+ The concentration is 1mol/L and is recorded as solution S A ；
(2) Accurately measuring Tetraethoxysilane (TEOS) as a Si source material according to the Yb to Si molar ratio of 20; mixing TEOS, absolute ethyl alcohol and deionized water according to the volume ratio of 1 B ；
(3) The solution S obtained in the steps (1) and (2) is A And solution S B Stirring and mixing to obtain mixed cation solution, and recording as solution S C ；
(4) According to the total molar amount of cations, according to the molar ratio of Yb to urea being 1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in 60 deg.C water bath for 12h to obtain colloidal precipitate solution, and recording as S E ；
(6) Naturally standing and aging the colloidal precipitation solution obtained in the step (5) to ensure complete precipitation; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Drying the precursor colloid in a drying oven at the drying temperature of 110 ℃ for 12h, cooling and grinding to obtain precursor powder; and calcining the precursor powder in an atmospheric environment at the calcining temperature of 1200 ℃ for 6h to obtain the ytterbium silicate powder material. The XRD of the resulting product is shown in fig. 8; fig. 8 shows that not only the high-temperature phase ytterbium silicate diffraction peak but also the significant ytterbium oxide diffraction peak indicate that the product purity is not high.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. 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 (9)
1. A preparation method of an ultra-fine ytterbium silicate powder material is characterized in that: the granularity of the superfine ytterbium silicate powder material is 30-100nm; the superfine ytterbium silicate powder material is a high-temperature phase structure ytterbium silicate powder material;
the preparation method comprises the following steps:
(1) Preparing Yb-containing 3+ The solution of (1); is marked as S A ；
(2) Taking silicate ester as a Si source material, dissolving the Si source material in an alcohol-water system to obtain a Si-containing solution, and recording the solution as S B ；
The Si-containing solution in the step (2) is prepared by the following steps:
according to the volume ratio, ethyl orthosilicate: anhydrous ethanol: n, measuring ethyl orthosilicate, absolute ethyl alcohol and deionized water; uniformly mixing the measured tetraethoxysilane, the absolute ethyl alcohol and the deionized water; the Si-containing solution is obtained and is marked as S B (ii) a M is greater than or equal to 1 and less than or equal to 10, n is greater than or equal to 2 and less than or equal to 10;
(3) According to the Yb to Si molar ratio of 20-11; the solution S obtained in the steps (1) and (2) is A And S B Mixing to obtain a mixed cation solution,
(4) Weighing a proper amount of urea according to a molar ratio of Yb to urea of 1-1 D ；
(5) Mixing the mixed cation solution and the urea precipitator solution, and uniformly stirring; heating in a water bath gave a gummy precipitate solution, denoted as S E (ii) a The water bath heating temperature is 90 ℃, and the heating time is 12h;
(6) Naturally standing and aging the mixed solution containing the colloidal precipitate obtained in the step (5) to completely precipitate; removing supernatant after aging, and washing the precipitate with deionized water and absolute ethyl alcohol to obtain precursor colloid;
(7) Putting the precursor colloid into a drying oven for drying, cooling and grinding to obtain precursor powder; calcining the precursor powder under the condition of oxygen content to obtain an ultra-fine ytterbium silicate powder material; the temperature of the calcination is 1200 ℃; the calcination time is 6-10h.
2. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps: containing Yb 3+ Is prepared by the following steps:
measuring hydrochloric acid or nitric acid, diluting, heating to dissolve ytterbium oxide powder, and completely dissolving the ytterbium oxide powder; adding deionized water to dilute to obtain a rare earth ion solution with a certain concentration, and recording as S A (ii) a Said S A The concentration of the medium rare earth ions is 0.1-2 mol/L.
3. The method for preparing an ultra-fine ytterbium silicate powder material of claim 2, wherein the method comprises the following steps: said S A The concentration of the medium rare earth ions is 1mol/L.
4. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps: in step (2), m =2 and n is equal to 4.
5. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps:
in the step (4), preparing a urea solution according to a Yb and urea molar ratio of 1-1.
6. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps:
in the step (4), the urea and the deionized water are mixed, so that the urea can be completely dissolved in the deionized water, and the concentration of the urea in the mixed solution is more than or equal to 1mol/L.
7. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps:
in the step (6), the ageing time of the colloidal precipitation solution is 6-24 h;
in the step (6), the precipitate is washed by deionized water, and after no ammonium ions and chloride ions are ensured, the precipitate is washed by absolute ethyl alcohol.
8. The method for preparing an ultra-fine ytterbium silicate powder material of claim 6, wherein the method comprises the following steps:
in the step (6), the aging time of the colloidal precipitation solution is 12h.
9. The method for preparing an ultra-fine ytterbium silicate powder material of claim 1, wherein the method comprises the following steps:
in the step (7), the drying temperature of the precipitate is 100-200 ℃.
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