CN113416874B - Tungsten-based single-element or multi-element in-situ doped composite nano powder and preparation method thereof - Google Patents
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Abstract
The invention relates to a tungsten-based single element or multi-element in-situ doped composite superfine nano powder and a preparation method thereof. The specific process comprises the following steps: dissolving soluble tungstate and soluble salt corresponding to elements needing in-situ compounding in water, and stirring until the soluble tungstate and the soluble salt are uniformly mixed; adding acrylic acid and oxidant in turn to mix the solution evenly. Polymerizing the obtained solution at the temperature of 150 ℃ and 200 ℃ for 2-3h to obtain precursor powder. The precursor powder is firstly insulated for 3-5h in the air atmosphere at the temperature of 500-600 ℃, and then insulated for 2-3h in the hydrogen or hydrogen-nitrogen mixed atmosphere at the temperature of 600-800 ℃ to obtain the tungsten-based single-element or multi-element in-situ doped composite superfine nano powder with the granularity controllable between 5 and 50 nm. The tungsten-based single element or multi-element in-situ doped composite nano powder prepared by the method has the characteristics of uniform and superfine particle size, high purity, simple process, low cost, unlimited doped elements and the like, and is suitable for industrial production.
Description
Technical Field
The invention relates to a method for synthesizing a powder metallurgy material, in particular to tungsten-based single-element or multi-element in-situ doped nano powder and a preparation method thereof.
Background
Tungsten and its alloys are widely used in aerospace, weapons and equipments, high temperature furnaces, electronics and nuclear fusion reactors because of their high melting point (3410 ℃), high thermal conductivity (168W/(m · K)), high strength, low thermal expansion coefficient, low sputtering rate, low vapor pressure, low hydrogen solubility, low tritium retention and excellent thermal shock resistance. However, the brittleness of tungsten and its alloys, especially at low temperatures, limits their widespread use. At present, research finds that the strength, toughness, recrystallization temperature and irradiation resistance of the tungsten-based material can be obviously improved by performing dispersion doping strengthening on pure tungsten, and the ductile-brittle transition temperature of the tungsten-based material is reduced.
The existing methods for preparing the metal element second-phase doped tungsten powder include a chemical method, a hydrothermal reaction method, a sol-gel method and a mechanical alloying method, except the mechanical alloying method, a doping system needs to dissolve two or more soluble salts into water to prepare a mixed solution, then a surfactant or a chelating agent is added to react under the condition of strong acid, after the reaction is finished, an organic solvent is removed by cleaning and filtering, and then the second-phase particle doped tungsten composite powder is obtained by calcining and reducing.
Disclosure of Invention
The invention adopts a thermal polymerization-thermal reduction method to prepare the tungsten-based single element or multi-element in-situ doped composite nano powder.
Based on the purpose, the invention adopts the following technical scheme:
a tungsten-based single element or multi-element in-situ doped composite nano powder is characterized in that doping elements are dispersed in tungsten particles in situ, and the doping elements are one or more metal elements or metal oxides.
Preferably, the metal elements are cerium, aluminum, manganese, lanthanum, zirconium, thorium and yttrium, and the mass of the doping element is 1.0wt% -2.7wt% of the mass of the tungsten element.
Preferably, the nano powder is in a sphere-like shape, and the particle size of the nano powder is 5-50 nm.
A preparation method of tungsten-based single-element or multi-element in-situ doped composite nano powder comprises the following steps:
a: dissolving soluble metal tungsten salt in water to ensure that the mass concentration of tungsten element in the solution is 7.45-13.77 wt%;
b: adding soluble salt containing doping elements into the aqueous solution of the metal tungsten salt, wherein the mass of the doping elements is 1.0-2.7 wt% of that of the tungsten element;
c: sequentially adding acrylic acid and an oxidant, and uniformly mixing;
d: polymerizing the reaction system obtained in the step c at the temperature of 150-;
e: the precursor powder is firstly insulated for 3-5h in the air atmosphere at the temperature of 500-800 ℃ and then insulated for 2-3h in the hydrogen or hydrogen-nitrogen atmosphere at the temperature of 600-800 ℃ to obtain the tungsten-based single-element or multi-element in-situ doped composite nano powder with controllable granularity.
Further, the oxidant is concentrated nitric acid or hydrogen peroxide with the volume ratio of 30%, the volume ratio of the oxidant to water is 1-5%, the volume ratio of acrylic acid to water is less than 30%, and the acrylic acid is analytically pure.
Further, the soluble salt containing the doping element is nitrate or acetate, and the doping element is one or more metal elements or metal oxides.
Preferably, the soluble metal tungsten salt is a tungstate, metatungstate, or paratungstate.
Preferably, the soluble metal tungsten salt is ammonium tungstate, ammonium metatungstate, or ammonium paratungstate.
The invention has the beneficial effects that:
(1) according to the method, acrylic acid and an oxidant are selected to perform polymerization reaction under the combined action to obtain precursor powder, the existence of the oxidant enables gas to be generated in the reaction process, so that acrylic acid is enabled to generate fine foam while being polymerized, the precursor powder is fully dispersed, the synthesized powder is greatly refined, the precursor powder with high fluffiness is finally obtained, the powder granularity can reach the nanometer level, and the granularity can reach 5-50 nm.
(2) Compared with the conventional preparation method, the method for preparing the tungsten-based single element or multi-element in-situ composite nano powder by using the thermal polymerization-thermal reduction method has the advantages of simple process, good stability, fine and uniform prepared powder and capability of realizing batch preparation.
(3) The powder prepared by the method has uniform components, doping elements are not limited, and in-situ doping compounding can be realized; finally, the doping elements are dispersed in the tungsten particles, the purity of the powder is high, the particles are spherical, and the granularity is adjustable between 5 nm and 50 nm.
Drawings
FIG. 1 example 1 preparation of W-Y by thermal polymerization-thermal reduction 2 O 3 SEM topography of the in-situ composite powder;
FIG. 2 example 1 preparation of W-Y by thermal polymerization-thermal reduction 2 O 3 TEM morphology of the in-situ composite powder;
FIG. 3 example 2 preparation of W-Ce by thermal polymerization-thermal reduction 2 O 3 -ThO 2 TEM morphology of the in-situ composite powder;
FIG. 4 example 3 preparation of W-La by thermal polymerization-thermal reduction 2 O 3 -ZrO 2 -MnO 2 TEM morphology of the in-situ composite powder;
FIG. 5 example 4 preparation of W-Ce by thermal polymerization-thermal reduction 2 O 3 -Al 2 O 3 -MnO 2 TEM morphology of the in-situ composite powder;
FIG. 6 example 5 preparation of W-La by thermal polymerization-thermal reduction 2 O 3 -Ce 2 O 3 -Al 2 O 3 -ZrO 2 And (4) a TEM (transmission electron microscope) morphology image of the in-situ composite powder.
Detailed Description
Example 1:
w-1wt% Y composite nano powder doped in situ with tungsten-based single element 2 O 3 The preparation method comprises the following steps:
a. 12.623g of ammonium metatungstate is dissolved in 60mL of deionized water;
b. adding 1wt% of yttrium nitrate powder into aqueous solution of metal tungsten salt;
c. then, adding analytically pure acrylic acid and 5% concentrated nitric acid in a volume ratio of 30% and deionized water or hydrogen peroxide in a concentration of 30% in a volume ratio of 1% in sequence, and uniformly mixing;
d. heating the obtained solution to 150 ℃ for polymerization reaction for 2h to obtain precursor powder;
e. placing the powder in a tube furnace, keeping the temperature for 5h at 500 ℃ in the air atmosphere, and keeping the temperature for 2h at 800 ℃ in the hydrogen atmosphere to obtain W-1Wt%Y 2 O 3 And (3) compounding the powder in situ.
W-1wt% Y prepared by the above method 2 O 3 The SEM topography of the in-situ composite powder is shown in figure 1, the TEM topography is shown in figure 2, and the analysis result shows that the doped Y is 2 O 3 The powder is dispersed and distributed in the tungsten particles in situ, and is in a sphere-like shape, and the particle size is about 20 nm.
Example 2:
w-0.5wt% Ce of tungsten-based multi-element in-situ doped composite nano powder 2 O 3 -0.5wt%ThO 2 The preparation method comprises the following steps:
a. 14.198g of ammonium paratungstate was dissolved in 120mL of deionized water;
b. adding 0.5wt% of cerium nitrate and 0.5wt% of thorium nitrate into the aqueous solution of the metal tungsten salt;
c. then, adding analytically pure acrylic acid with the volume ratio of 25 percent to the deionized water and hydrogen peroxide with the volume ratio of 1 percent and the concentration of 30 percent in sequence, and mixing uniformly;
d. heating the obtained solution to 180 ℃ for polymerization reaction for 2h to obtain precursor powder;
e. placing the powder in a tube furnace, preserving heat for 4h at 550 ℃ in an air atmosphere, and preserving heat for 2h at 700 ℃ in a hydrogen atmosphere to obtain W-0.5wt% Ce 2 O 3 -0.5wt%ThO 2 And (3) compounding the powder in situ.
W-0.5wt% Ce prepared by the above method 2 O 3 -0.5wt%ThO 2 The TEM morphology of the in-situ composite powder is shown in FIG. 3, and the analysis result shows that the doped Ce is 2 O 3 And ThO 2 The powder is dispersed in the tungsten particles in situ, is in a sphere-like shape and has the granularity of about 20-50 nm.
Example 3:
w-2wt% La composite nano powder with W-2wt% of tungsten-based multi-element in-situ doped 2 O 3 -0.5wt%ZrO 2 -0.2wt%MnO 2 The preparation method comprises the following steps:
a. 14.198g of ammonium tungstate is dissolved in 100mL of deionized water;
b. adding 2wt% of lanthanum acetate, 0.5wt% of zirconium nitrate and 0.2wt% of manganese acetate into the aqueous solution of the metal tungsten salt;
c. sequentially adding analytically pure acrylic acid with the volume ratio of deionized water being 20% and concentrated nitric acid with the volume ratio being 3%, and uniformly mixing;
d. heating the obtained solution to 200 ℃ for polymerization reaction for 2.5h to obtain precursor powder;
e. placing the powder in a tube furnace, preserving heat for 4h at 550 ℃ in an air atmosphere, and preserving heat for 3h at 600 ℃ in a hydrogen atmosphere to obtain W-2wt% of La 2 O 3 -0.5wt%ZrO 2 -0.2wt%MnO 2 And (3) compounding the powder in situ.
W-2wt% La prepared by the above method 2 O 3 -0.5wt%ZrO 2 -0.2wt%MnO 2 The TEM morphology of the in-situ composite powder is shown in FIG. 4, and the analysis result shows that the doped La is 2 O 3 -ZrO 2 -MnO 2 The powder is dispersed in the tungsten particles in situ, and is in a sphere-like shape, and the particle size is about 10-50 nm.
Example 4:
w-1wt% Ce of tungsten-based multi-element in-situ doped composite nano powder 2 O 3 -0.5wt%Al 2 O 3 -0.5wt%MnO 2 The preparation method comprises the following steps:
a. 14.198g of ammonium tungstate dissolved oxygen is dissolved in 100mL of deionized water;
b. adding 1wt% of cerium nitrate, 0.5wt% of aluminum nitrate and 0.5wt% of manganese acetate into an aqueous solution of a metal tungsten salt;
c. sequentially adding analytically pure acrylic acid with the volume ratio of 20 percent to the deionized water and concentrated nitric acid with the volume ratio of 5 percent, and uniformly mixing;
d. heating the obtained solution to 200 ℃ for polymerization reaction for 2.5h to obtain precursor powder;
e. placing the powder in a tube furnace, preserving heat for 4h at 550 ℃ in an air atmosphere, and preserving heat for 2h at 750 ℃ in a hydrogen atmosphere to obtain W-1wt% Ce 2 O 3 -0.5wt%Al 2 O 3 -0.5wt%MnO 2 And (3) compounding the powder in situ.
W-1wt% Ce prepared by the above method 2 O 3 -0.5wt%Al 2 O 3 -0.5wt%MnO 2 TEM morphology picture of in-situ composite powder5, the analysis results show doped Ce 2 O 3 -Al 2 O 3 -MnO 2 The powder is dispersed in the tungsten particles in situ, is in a sphere-like shape and has the granularity of about 5-50 nm.
Example 5
W-0.5wt% La composite nano powder with tungsten-based multi-element in-situ doping 2 O 3 -0.2wt%Ce 2 O 3 -0.2wt%Al 2 O 3 -0.1wt%ZrO 2 The preparation method comprises the following steps:
a. 12.623g of ammonium metatungstate is dissolved in 60mL of deionized water;
b. adding 0.5wt% of lanthanum nitrate, 0.2wt% of cerium nitrate, 0.2wt% of aluminum nitrate and 0.1wt% of zirconium nitrate into the aqueous solution of the metal tungsten salt;
c. sequentially adding analytically pure acrylic acid with the volume ratio of 20 percent to the deionized water and concentrated nitric acid with the volume ratio of 3 percent, and uniformly mixing;
d. heating the obtained solution to 160 ℃ for polymerization reaction for 2.5h to obtain precursor powder;
e. placing the powder in a tube furnace, preserving heat for 3h at 600 ℃ in an air atmosphere, and preserving heat for 2h at 800 ℃ in a hydrogen-nitrogen mixed atmosphere to obtain W-0.5wt% of La 2 O 3 -0.2wt%Ce 2 O 3 -0.2wt%Al 2 O 3 -0.1wt%ZrO 2 And (3) compounding the powder in situ.
W-0.5wt% La prepared by the above method 2 O 3 -0.2wt%Ce 2 O 3 -0.2wt%Al 2 O 3 -0.1wt%ZrO 2 The TEM morphology of the in-situ composite powder is shown in FIG. 6, and the analysis result shows that the doped La is 2 O 3 -Ce 2 O 3 -Al 2 O 3 -ZrO 2 The powder is dispersed in the tungsten particles in situ, is in a sphere-like shape and has the granularity of about 5-30 nm.
Claims (5)
1. The tungsten-based single-element or multi-element in-situ doped composite nano powder is characterized in that doping elements are dispersed in tungsten particles in situ, and the doping elements are one or more metal elements or metal oxides; the nano powder is in a sphere-like shape, and the particle size of the nano powder is 5-50 nm; the metal elements are cerium, aluminum, manganese, lanthanum, zirconium, thorium and yttrium, and the metal oxide is a stable oxide corresponding to the metal elements;
the nano powder is prepared by the following method:
a: dissolving soluble metal tungsten salt in water to ensure that the mass concentration of tungsten element in the solution is 7.45-13.77 wt%;
b: adding soluble salt containing doping elements into the aqueous solution of the metal tungsten salt, wherein the mass of the doping elements is 1.0-2.7 wt% of that of the tungsten element;
c: sequentially adding acrylic acid and an oxidant, and uniformly mixing; the oxidant is concentrated nitric acid or 30% hydrogen peroxide by volume, and the volume ratio of the oxidant to the water in the step a is 1% -5%; the volume ratio of the acrylic acid to the water in step a is less than 30%;
d: polymerizing the reaction system obtained in the step c at the temperature of 150-;
e: the precursor powder is firstly insulated for 3-5h in the air atmosphere at the temperature of 500-800 ℃ and then insulated for 2-3h in the hydrogen or hydrogen-nitrogen atmosphere at the temperature of 600-800 ℃ to obtain the tungsten-based single-element or multi-element in-situ doped composite nano powder with controllable granularity.
2. A preparation method of tungsten-based single-element or multi-element in-situ doped composite nano powder is characterized by comprising the following steps:
a: dissolving soluble metal tungsten salt in water to ensure that the mass concentration of tungsten element in the solution is 7.45-13.77 wt%;
b: adding soluble salt containing doping elements into the aqueous solution of the metal tungsten salt, wherein the mass of the doping elements is 1.0-2.7 wt% of that of the tungsten element;
c: sequentially adding acrylic acid and an oxidant, and uniformly mixing; the oxidant is concentrated nitric acid or 30% hydrogen peroxide by volume, and the volume ratio of the oxidant to the water in the step a is 1% -5%; the volume ratio of the acrylic acid to the water in step a is less than 30%;
d: polymerizing the reaction system obtained in the step c at the temperature of 150-;
e: the precursor powder is firstly insulated for 3-5h in the air atmosphere at the temperature of 500-800 ℃ and then insulated for 2-3h in the hydrogen or hydrogen-nitrogen atmosphere at the temperature of 600-800 ℃ to obtain the tungsten-based single-element or multi-element in-situ doped composite nano powder with controllable granularity.
3. The method for preparing the tungsten-based single-element or multi-element in-situ doped composite nano powder as claimed in claim 2, wherein the soluble salt containing the doping element is nitrate or acetate, and the doping element is one or more metal elements or metal oxides.
4. The method for preparing the tungsten-based single-element or multi-element in-situ doped composite nano powder according to claim 3, wherein the soluble metal tungsten salt is tungstate, metatungstate or paratungstate.
5. The method for preparing the tungsten-based single-element or multi-element in-situ doped composite nanopowder according to claim 4, wherein the soluble metal tungsten salt is ammonium tungstate, ammonium metatungstate or ammonium paratungstate.
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| JP2000119766A (en) * | 1998-10-15 | 2000-04-25 | Toshiba Corp | Vibrator for vibration generator, its manufacture, and vibration generator |
| CN102350508A (en) * | 2011-10-13 | 2012-02-15 | 北京科技大学 | Method for preparing doped-tungsten-based composite powder |
| CN102626785A (en) * | 2012-04-27 | 2012-08-08 | 北京科技大学 | Preparation method for rare earth oxide doped tungsten powder |
| CN103231073A (en) * | 2013-04-27 | 2013-08-07 | 北京科技大学 | Tungsten nanowire material and manufacture method thereof |
| CN106964783A (en) * | 2017-04-21 | 2017-07-21 | 鹤山市沃得钨钼实业有限公司 | A kind of manufacture method of nano rare earth tungsten electrode |
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| JP2000119766A (en) * | 1998-10-15 | 2000-04-25 | Toshiba Corp | Vibrator for vibration generator, its manufacture, and vibration generator |
| CN102350508A (en) * | 2011-10-13 | 2012-02-15 | 北京科技大学 | Method for preparing doped-tungsten-based composite powder |
| CN102626785A (en) * | 2012-04-27 | 2012-08-08 | 北京科技大学 | Preparation method for rare earth oxide doped tungsten powder |
| CN103231073A (en) * | 2013-04-27 | 2013-08-07 | 北京科技大学 | Tungsten nanowire material and manufacture method thereof |
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