CN116119719B - Superfine platy tungsten oxide and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of material preparation, in particular to superfine platy tungsten oxide and a preparation method thereof, wherein the prepared tungsten oxide is of a platy structure, and single tungsten oxide is thinner; the superfine platy tungsten oxide has the Fisher particle size of 0.5-1.5 mu m, is obviously smaller than the traditional tungsten oxide, and has the specific surface area of 3.0-5.0 m 2 And/g, which is obviously higher than the traditional tungsten oxide, is favorable for preparing high-performance fine particle products, and can promote the application of tungsten materials in the fields of aviation, aerospace, military and atomic energy.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to superfine platy tungsten oxide and a preparation method thereof.
Background
The metal tungsten has a series of excellent properties such as high melting point, high hardness, high density, low thermal expansion coefficient and the like, is a main raw material for producing various functional materials and structural materials, and is widely applied to the fields of aviation, aerospace, military, atomic energy and the like. Because tungsten has a high melting point, tungsten alloy products are often prepared by taking tungsten powder as a raw material and adopting a powder metallurgy method. The adoption of the fine powder can obviously reduce the sintering temperature, and can prepare the fine-grain alloy with high density at a lower sintering temperature, so that the performances of the alloy, such as strength, hardness, wear resistance and the like, can be obviously improved. Therefore, the production of fine-grained refractory metal powder and fine-grained alloy has become a hot spot of recent research and attention.
The key point of the preparation of the fine particle powder is the control of the raw materials and the control of the volatilization-deposition in the hydrogen reduction process, thereby effectively inhibiting the growth of particles and obtaining superfine powder. At present, the needle-shaped structure, loose and porous blue tungsten with the Fisher particle size smaller than 12 mu m and large specific surface area are better applied in the preparation process of fine particle and superfine particle tungsten powder. The yellow tungsten trioxide has larger defects in the process of preparing the fine particle powder due to the characteristics of large Fisher particle size (more than 14 mu m), low specific surface area and the like, and the high-performance fine particle product meeting the requirements is difficult to prepare. Therefore, the development of the superfine tungsten oxide with small Fisher particle size and large specific surface area has better practical significance.
Disclosure of Invention
In order to solve the problems in the prior art, the main purpose of the invention is to provide an ultrafine platy tungsten oxide and a preparation method thereof.
In order to solve the technical problems, according to one aspect of the present invention, the following technical solutions are provided:
an ultrafine platy tungsten oxide having a platy structure, having a Fisher particle size of 0.5-1.5 [ mu ] m and a specific surface area of 3.0-5.0 m 2 /g。
In order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the preparation method of the superfine platy tungsten oxide comprises the following steps:
s1, taking an ammonium tungstate solution for standby;
s2, taking hydrochloric acid for standby, wherein the preparation amount of the hydrochloric acid is 1.1-1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into standby hydrochloric acid in a dropwise adding mode, and stirring while dropwise adding;
s4, filtering after stirring is completed, and drying the filtered tungstic acid at the temperature of 110-120 ℃;
s5, calcining the dried tungstic acid at the temperature of 500-600 ℃ for 1.0-2.0 h, and sieving to obtain the superfine platy tungsten oxide.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: in the step S1, the concentration of the ammonium tungstate solution is 200-250 g/L.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: in the step S2, the concentration of the hydrochloric acid is 16-20wt%.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: the step S3 is carried out at normal temperature.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: in the step S3, the stirring speed is 50-100 r/min.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: in the step S3, the dropping speed is 100-200 mL/min.
As a preferable scheme of the preparation method of the superfine platy tungsten oxide, the invention comprises the following steps: in the step S3, continuously stirring for 0.5-1.0 h after the dripping is completed;
in order to solve the above technical problems, according to another aspect of the present invention, the following technical solutions are provided:
the superfine platy tungsten oxide is applied to the fields of aviation, aerospace, military and atomic energy.
The beneficial effects of the invention are as follows:
the invention provides superfine platy tungsten oxide and a preparation method thereof, wherein the prepared tungsten oxide is of platy structure, and single tungsten oxide is thinner, and the structure is favorable for promoting the hydrogen reduction reaction and facilitating the preparation of fine particle powder; the superfine platy tungsten oxide has the Fisher particle size of 0.5-1.5 mu m, is obviously smaller than the traditional tungsten oxide, and has the specific surface area of 3.0-5.0 m 2 And/g, which is obviously higher than the traditional tungsten oxide, is favorable for preparing high-performance fine particle products, and can promote the application of tungsten materials in the fields of aviation, aerospace, military and atomic energy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of ultrafine platy tungsten oxide prepared according to example 1 of the present invention;
FIG. 2 is an SEM image of ultrafine platy tungsten oxide prepared according to example 2 of the present invention;
FIG. 3 is an SEM image of ultrafine platy tungsten oxide prepared according to example 3 of the present invention;
FIG. 4 is an SEM image of ultrafine platy tungsten oxide prepared according to example 4 of the present invention;
FIG. 5 is an SEM image of ultrafine platy tungsten oxide prepared according to example 5 of the present invention;
FIG. 6 is an SEM image of ultrafine platy tungsten oxide prepared according to example 6 of the present invention;
FIG. 7 is an SEM image of tungsten oxide prepared in comparative example 2 of the present invention;
fig. 8 is an SEM image of tungsten oxide prepared in comparative example 3 of the present invention.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides superfine platy tungsten oxide and a preparation method thereof, wherein the prepared tungsten oxide is of platy structure, and single tungsten oxide is thinner, and the structure is favorable for promoting the hydrogen reduction reaction and facilitating the preparation of fine particle powder; the superfine platy oxidationThe Fisher particle size of tungsten is 0.5-1.5 mu m, which is significantly smaller than that of the traditional tungsten oxide, and the specific surface area is 3.0-5.0 m 2 And/g, significantly higher than conventional tungsten oxide.
An ultrafine platy tungsten oxide having a platy structure, having a Fisher particle size of 0.5-1.5 [ mu ] m and a specific surface area of 3.0-5.0 m 2 And/g. In particular, the fermi particle size of the ultrafine platy tungsten oxide may be, for example, but not limited to, any one or a range between any two of 0.5 μm, 0.8 μm, 1.0 μm, 1.2 μm, 1.5 μm; the specific surface area of the ultrafine platy tungsten oxide can be, for example, but not limited to, 3.0m 2 /g、3.5m 2 /g、4.0m 2 /g、4.5m 2 /g、5.0m 2 A range between any one or any two of/g;
according to another aspect of the invention, the invention provides the following technical scheme:
the preparation method of the superfine platy tungsten oxide comprises the following steps:
s1, taking an ammonium tungstate solution for standby;
s2, taking hydrochloric acid for standby, wherein the preparation amount of the hydrochloric acid is 1.1-1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into standby hydrochloric acid in a dropwise adding mode, and stirring while dropwise adding;
s4, filtering after stirring is completed, and drying the filtered tungstic acid at the temperature of 110-120 ℃;
s5, calcining the dried tungstic acid at the temperature of 500-600 ℃ for 1.0-2.0 h, and sieving to obtain the superfine platy tungsten oxide.
Preferably, in the step S1, the concentration of the ammonium tungstate solution is 200-250 g/L. If the concentration of ammonium tungstate is too low, the yield is too low; if the concentration is too high, the requirements on the preparation process of ammonium tungstate are high, and APT is easy to separate out, so that the preparation of tungsten oxide is not facilitated. In particular, the concentration of the ammonium tungstate solution may be, for example, but not limited to, any one of 200g/L, 210g/L, 220g/L, 230g/L, 240g/L, 250g/L, or a range between any two thereof;
preferably, in the step S2, the concentration of the hydrochloric acid is 16-20wt%, and the preparation amount of the hydrochloric acid is 1.1-1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid; the acid concentration is too high, so that the ammonium tungstate is excessively nucleated instantaneously after being added, the tungstic acid deposition growth effect is not obvious, and the control of the platy structure is not facilitated. Too low acid concentration can result in low reaction efficiency, large amount of acid needed, large volume of reaction mother liquor, high requirements on reaction equipment and filtering equipment and low production efficiency. In particular, the concentration of hydrochloric acid may be, for example, but not limited to, any one of 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, or a range between any two; if the acid consumption is too low, the acid amount required by the reaction is insufficient, and tungstic acid is difficult to form; and the excessive acid consumption is not easy to form a plate-shaped structure and causes acid waste. In particular, the amount of hydrochloric acid may be in a range between any one or any two of 1.1 times, 1.15 times, 1.2 times, 1.25 times, 1.3 times, for example, but not limited to, the theoretical amount of hydrochloric acid required to produce tungstic acid;
preferably, the step S3 is performed at normal temperature, and the stirring speed is 50-100 r/min; the dropping speed is 100-200 mL/min; continuously stirring for 0.5-1.0 h after the dripping is completed; the stirring speed is too slow, which is unfavorable for the rapid dispersion of ammonium tungstate into hydrochloric acid, and reduces the nucleation speed of the tungstic acid. The stirring speed is too high, more tungstic acid is nucleated, the deposition growth effect is not obvious, and the plate-shaped structure is not beneficial to formation. Specifically, the stirring speed may be, for example, but not limited to, any one of 50r/min, 60r/min, 70r/min, 80r/min, 90r/min, 100r/min or a range between any two thereof; too slow a drop velocity results in a longer overall reaction time. If the dropping speed is too high, the quantity of tungstic acid nucleation is large, the effect of deposition growth is not obvious, and the plate-shaped structure is not beneficial to formation. Specifically, the drop rate may be, for example, but not limited to, any one or a range between any two of 100mL/min, 110mL/min, 120mL/min, 130mL/min, 140mL/min, 150mL/min, 160mL/min, 170mL/min, 180mL/min, 190mL/min, 200mL/min; too short stirring time is easy to react incompletely, so that the concentration of tungsten in the filtrate is high; too long stirring time results in too low reaction efficiency. Specifically, the continuous stirring time after the completion of the dropwise addition may be, for example, but not limited to, any one or a range between any two of 0.5h, 0.75h, and 1.0h;
preferably, in the step S4, since the acid is used in an excessive amount, the acid residue is still remained in the mother solution after the tungstic acid is prepared, and the water is removed and the residual dilute acid is removed during the drying process. The boiling point of the dilute hydrochloric acid is 108 ℃, so that the temperature is generally above 110 ℃ in order to remove the residual acid more thoroughly, but the temperature is too high, the requirement on equipment is higher, and the energy consumption is high. Specifically, the drying temperature may be, for example, but not limited to, any one or a range between any two of 110 ℃, 111 ℃, 112 ℃, 113 ℃, 114 ℃, 115 ℃, 116 ℃, 117 ℃, 118 ℃, 119 ℃, 120 ℃;
preferably, in the step S5, the calcination temperature is low, and the time required for completely converting the tungstic acid into tungsten oxide needs to be increased, which is unfavorable for improving the production efficiency and saving the production cost. And if the temperature is too high, the material is easy to sinter and grow, and the specific surface area of tungsten oxide is reduced. Specifically, the calcination temperature may be, for example, but not limited to, any one or a range between any two of 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, 560 ℃, 570 ℃, 580 ℃, 600 ℃; the calcination time may be, for example, but is not limited to, any one or a range between any two of 1.0h, 1.25h, 1.5h, 1.75h, 2.0 h; after calcination, the mixture is sieved to remove coarse particles and mechanical inclusions, and the sieve may be selected according to the need, for example, 80 mesh sieve, 100 mesh sieve, etc.
According to another aspect of the invention, the invention provides the following technical scheme:
the superfine platy tungsten oxide is applied to the fields of aviation, aerospace, military and atomic energy.
The technical scheme of the invention is further described below by combining specific embodiments.
Example 1
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 200g/L for later use;
s2, taking hydrochloric acid with the concentration of 16wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.1 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 100r/min, the dripping speed is 100mL/min, and continuing stirring for 0.5h after the dropwise adding is completed;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid at 500 ℃ for 2.0h, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 1.0 mu m and the specific surface area of 4.1m as shown in figure 1 2 /g。
Example 2
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 18 weight percent for standby, wherein the preparation amount of the hydrochloric acid is 1.2 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 80r/min, the dripping speed is 180mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid for 1.5 hours at 550 ℃, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 1.3 mu m and the specific surface area of 3.3m as shown in figure 2 2 /g。
Example 3
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 250g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 50r/min, the dripping speed is 200mL/min, and continuing stirring for 1.0h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at 120 ℃;
s5, calcining the dried tungstic acid at 600 ℃ for 1.0h, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 1.5 mu m and the specific surface area of 3.0m as shown in figure 3 2 /g。
Example 4
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 50r/min, the dripping speed is 180mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid for 1.0h at 550 ℃, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 1.1 mu m and the specific surface area of 3.6m as shown in figure 4 2 /g。
Example 5
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.1 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 50r/min, the dripping speed is 180mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid at 550 ℃ for 1.0h, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 0.8 mu m and the specific surface area of 4.4m as shown in figure 5 2 /g。
Example 6
The preparation process of superfine platy tungsten oxide includes the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.1 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 100r/min, the dripping speed is 140mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid at 550 ℃ for 1.0h, and sieving to obtain superfine platy tungsten oxide, wherein the superfine platy tungsten oxide prepared by the embodiment has the Fisher size of 0.5 mu m and the specific surface area of 5.0m as shown in figure 6 2 /g。
Comparative example 1
A method for preparing tungsten oxide, comprising the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.1 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 100r/min, the dripping speed is 140mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid for 1.0h at 650 ℃, and sieving to obtain tungsten oxide which has a platy structure, a Fisher particle size of 2.0 mu m and a specific surface area of 2.5m 2 /g。
Comparative example 2
A method for preparing tungsten oxide, comprising the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.4 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 100r/min, the dripping speed is 140mL/min, and continuing stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid for 1.0h at 550 ℃, and sieving to obtain tungsten oxide, wherein the tungsten oxide is shown in a figure 7, has an agglomerated state and no platy structure, has a Ferrareearth particle size of 0.46 mu m and a specific surface area of 6.2m 2 And/g, tungsten oxide is seriously agglomerated, which is not beneficial to the control of the thickness of a material layer and seriously affects the uniformity of the particle size distribution of a product.
Comparative example 3
A method for preparing tungsten oxide, comprising the following steps:
s1, taking 500mL of ammonium tungstate solution with the concentration of 230g/L for later use;
s2, taking hydrochloric acid with the concentration of 20wt% for standby, wherein the preparation amount of the hydrochloric acid is 1.1 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid;
s3, adding the standby ammonium tungstate solution into the standby hydrochloric acid in a dropwise adding mode at normal temperature, stirring while dropwise adding, wherein the stirring speed is 200r/min, the dripping speed is 300mL/min, and continuously stirring for 0.8h after the dropwise adding is finished;
s4, filtering after stirring, and drying the filtered tungstic acid at the temperature of 110 ℃;
s5, calcining the dried tungstic acid for 1.0h at 550 ℃, and sieving to obtain oxygenAs shown in FIG. 8, the tungsten carbide is in an agglomerated state and has no plate-like structure, the Fisher size is 1.3 μm, and the specific surface area is 5.2m 2 And/g, tungsten oxide is seriously agglomerated, which is not beneficial to the control of the thickness of a material layer and seriously affects the uniformity of the particle size distribution of a product.
As can be seen from the above examples, the ultrafine platy tungsten oxide has a Fisher particle size of 0.5-1.5 μm, significantly smaller than conventional tungsten oxide, and a specific surface area of 3.0-5.0 m 2 And/g, which is obviously higher than that of the traditional tungsten oxide, the superfine platy tungsten oxide is favorable for preparing high-performance fine particle products, and can promote the application of tungsten materials in the fields of aviation, aerospace, military and atomic energy.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (3)
1. A preparation method of superfine platy tungsten oxide is characterized in that the superfine platy tungsten oxide has a platy structure, the Fisher particle size is 0.5-1.5 mu m, and the specific surface area is 3.0-5.0 m 2 /g; the method comprises the following steps:
s1, taking an ammonium tungstate solution for standby; the concentration of the ammonium tungstate solution is 200-250 g/L;
s2, taking hydrochloric acid for standby, wherein the preparation amount of the hydrochloric acid is 1.1-1.3 times of the theoretical amount of the hydrochloric acid required for preparing the tungstic acid; the concentration of the hydrochloric acid is 16-20wt%;
s3, adding the standby ammonium tungstate solution into standby hydrochloric acid in a dropwise adding mode, and stirring while dropwise adding; the dropping speed is 100-200 mL/min, and the step S3 is carried out at normal temperature;
s4, filtering after stirring is completed, and drying the filtered tungstic acid at the temperature of 110-120 ℃;
s5, calcining the dried tungstic acid at the temperature of 500-600 ℃ for 1.0-2.0 h, and sieving to obtain the superfine platy tungsten oxide.
2. The method for preparing ultrafine platy tungsten oxide according to claim 1, wherein in the step S3, the stirring speed is 50-100 r/min.
3. The method for preparing ultrafine platy tungsten oxide according to claim 1, wherein in the step S3, stirring is continued for 0.5-1.0 h after the completion of dripping.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0356607A (en) * | 1989-07-21 | 1991-03-12 | Catalysts & Chem Ind Co Ltd | Manufacture of tangsten ultra fine particles |
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| US20170225234A1 (en) * | 2014-10-20 | 2017-08-10 | Central South University | A preparation method of rare earth oxide dispersion strengthened fine grain tungsten materials |
| CN114180630A (en) * | 2021-12-27 | 2022-03-15 | 南京理工大学 | Multilayer nano plate-shaped WO3 and preparation method and application thereof |
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