CN110983087B - Method for improving oxide distribution in yttrium oxide dispersion strengthening tungsten alloy - Google Patents
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Abstract
The invention relates to a preparation method for improving oxide distribution in yttrium oxide dispersion strengthening tungsten alloy, which comprises the steps of dissolving polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate in deionized water, adjusting the solution to be alkaline by ammonia water after the polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate are fully dissolved, and then mechanically stirring the solution to fully react; pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction; filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, drying the obtained precipitate in a drying oven to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining in argon gas flow to obtain composite oxide powder; then pure hydrogen is used for two-step reduction to obtain W-Y2O3Compounding precursor powder; pressing the obtained composite precursor powder into a compact, and obtaining W-Y with obviously improved distribution of yttrium oxide in a tungsten matrix in a hydrogen atmosphere2O3And (3) alloying.
Description
Technical Field
The invention provides a method for improving distribution of yttrium oxide in tungsten alloy by utilizing an alkaline hydrothermal method and subsequent sintering, belonging to the technical field of powder metallurgy engineering.
Background
Due to unique mechanical and physical properties such as low sputtering rate, high thermal conductivity, low hydrogen retention, low swelling, no chemical sputtering and the like, the metal tungsten is widely applied to the fields of aerospace, nuclear fusion and military affairs. However, the inherent brittleness of metallic tungsten, including low temperature brittleness, recrystallization brittleness, and irradiation brittleness, greatly limits its widespread use, particularly as a structural material. Therefore, improving the brittleness and thus the ductility of the tungsten material is an important development direction of the tungsten material.
The presence of the impurity elements C, O, etc. is an important cause of brittleness of the tungsten material, and due to their low solubility in tungsten, these impurity elements easily form corresponding compounds at grain boundaries, thereby reducing the bonding strength of the grain boundaries of the tungsten material. Therefore, improving the enrichment state of impurities at grain boundaries is an effective way to improve the brittleness of tungsten materials. In addition, the working temperature of the tungsten material is usually higher than the recrystallization temperature thereof, which often results in coarsening of the material structure, and further results in enrichment of impurity elements, and finally deteriorates the low-temperature brittleness of the tungsten material, so that improving the structure stability of the tungsten material at high temperature is another effective way to improve the low-temperature brittleness of the tungsten material. According to the previous research, the rare earth oxide is added into the tungsten matrix, so that the structure coarsening of tungsten crystal grains under the conditions of sintering and service can be obviously inhibited, and the recrystallization temperature of the material is improved.
Currently, the main methods for preparing ODS-W alloy precursor powders are mechanical alloying and wet chemical methods, however, these methods produce composite powders in which the oxide second phase is generally large in size and very prone to segregation at grain boundaries. During subsequent sintering, the second phases of the oxide tend to coalesce and coarsen at the grain boundaries and have larger sizes due to the agglomeration effect of the phases. Due to the incongruity of the deformation, these large-sized oxides at the grain boundaries are likely to become the starting points of crack initiation, and thus the effect of improving the properties of the tungsten alloy by the second-phase oxides is greatly impaired.
Aiming at the current research situation, the invention develops an emerging hydrothermal method for preparing W-Y2O3The distribution of the yttrium oxide in the W matrix is obviously improved after the composite powder precursor is sintered by hydrogen. The method adopts a hydrothermal method in an alkaline environment, and polyvinylpyrrolidone (P) is added into a hydrothermal solutionVP) to prepare high-quality composite precursor powder with uniformly distributed yttrium oxide and uniformly fine tungsten grains, wherein the yttrium oxide at the grain boundary is obviously refined after hydrogen sintering, and the volume fraction of the yttrium oxide distributed in the grains is obviously improved.
Disclosure of Invention
The invention develops an emerging hydrothermal method for preparing W-Y2O3The distribution of the yttrium oxide in the W matrix of the composite powder precursor after hydrogen sintering is obviously improved. The method adopts a hydrothermal method in an alkaline environment, and adds polyvinylpyrrolidone (PVP) into a hydrothermal solution, so as to prepare high-quality composite precursor powder with uniformly distributed yttrium oxide and uniformly fine tungsten grains, wherein the yttrium oxide at the grain boundary is obviously refined after hydrogen sintering, and the volume fraction of the yttrium oxide distributed in the grains is obviously improved.
The specific technical scheme is as follows:
a preparation method for improving oxide distribution in a yttrium oxide dispersion strengthening tungsten alloy comprises the following steps:
(1) dissolving polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate in deionized water, adjusting the pH value of the solution to 9-11 by using ammonia water after the polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate are fully dissolved, and then mechanically stirring the solution to fully react;
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 170-200 ℃ for 12-24 h;
(3) filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, drying the obtained precipitate in a drying oven to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 1-2 hours in argon gas flow at 450-500 ℃ to obtain composite oxide powder;
(4) placing the composite oxide powder in a tubular furnace, and carrying out two-step reduction by using pure hydrogen, wherein the first-step reduction temperature is 580-650 ℃, and the time is 2-4 hours; then raising the temperature to 700-800 ℃ for the second step of reduction for 2-4 h to obtain W-Y2O3Composite precursor of (2)Powder;
(5) the obtained composite precursor powder is pressed into a block and sintered for 4-6h at the temperature of 1600 plus 1800 ℃ in the hydrogen atmosphere to obtain W-Y with obviously improved distribution of yttrium oxide in the tungsten matrix2O3And (3) alloying.
In the step (1), the concentration of ammonium metatungstate in the solution is as follows: 0.15-0.2 g/mL;
in the step (1), the mass of the yttrium nitrate hexahydrate is 0.013-0.026 times that of the ammonium metatungstate;
the concentration of the polyvinylpyrrolidone in the step (1) in the solution is 0.0025-0.005 g/mL.
The invention has the following advantages:
1. and preparation of W-Y2O3Compared with the traditional mechanical alloying method, the wet chemical method and the sol-gel method of the composite precursor powder, the composite precursor powder obtained by the preparation method can obviously refine the size of yttrium oxide at a W grain boundary (the average size is refined from 420nm to 105 nm); as shown in fig. 1b, the yttria (white arrow mark) at the grain boundary of the W alloy is significantly refined;
2. compared with W-Y prepared under traditional acidic condition2O3Compared with the composite precursor powder, the composite precursor powder prepared by the alkaline hydrothermal method has good dispersibility, and the volume fraction of the yttrium oxide distributed in the crystal after sintering is obviously improved (increased from 6.7% to 35.5%); as shown in fig. 2b, the amount of yttrium oxide (marked by white arrows) dispersed in the W alloy crystal is increased;
3. the W-Y with obviously improved distribution of yttrium oxide in tungsten matrix can be obtained by sintering the composite powder precursor prepared by the method2O3The W grain size in the alloy is obviously refined (the average size is refined from 580nm to 410 nm). As shown in fig. 3b, the grain size in the W alloy produced by the invention is significantly refined.
Drawings
FIG. 1 a: W-Y prepared under acidic hydrothermal conditions2O3TEM pictures of yttria distribution at grain boundaries in the alloy (white arrow marks);
FIG. 1 b: EXAMPLE 1 preparation ofPrepared W-Y2O3TEM pictures of yttria distribution at grain boundaries in the alloy (white arrow marks);
FIG. 2 a: W-Y prepared under acidic hydrothermal conditions2O3TEM pictures of the intragranular yttria distribution in the alloy (white arrow marks);
FIG. 2 b: example 2 preparation of W-Y2O3TEM pictures of the intragranular yttria distribution in the alloy (white arrow marks); FIG. 3 a: W-Y prepared under acidic hydrothermal conditions2O3SEM pictures of alloy fractures;
FIG. 3 b: example 3 preparation of W-Y2O3SEM pictures of fractures in the alloy.
Detailed Description
The features of the present invention are further described below by way of examples, but the present invention is not limited to the following examples.
Example 1
(1) 6g of ammonium metatungstate, 0.1g of PVP and 0.08g of yttrium nitrate hexahydrate are dissolved in 40mL of deionized water, and after the ammonium metatungstate, the pH of the solution is adjusted to 9 by using ammonia water (the concentration of ammonium metatungstate in the solution is 0.15g/mL, the mass of yttrium nitrate hexahydrate is 0.013 times of that of ammonium metatungstate, and the concentration of polyvinylpyrrolidone in the solution is 0.0025 g/mL);
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 180 ℃ for 24 hours;
(3) after the temperature of the reaction kettle is reduced to room temperature, filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, placing the obtained precipitate in a drying oven to be dried to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 1h in argon gas flow at 450 ℃ to obtain composite oxide powder;
(4) carrying out two-step reduction on the composite oxide powder in hydrogen gas flow, wherein the first-step reduction temperature is 600 ℃, the reduction time is 2h, then raising the temperature to 750 ℃ for carrying out the second-step reduction, the reduction time is 4h, and then cooling to room temperature in hydrogen atmosphere to obtain W-Y2O3The precursor powder is compounded, the heating rate is 5 ℃/min, and the air flow is 100 mL/min.
(5) Pressing the obtained composite precursor powder into a compact, and sintering the compact at 1600 ℃ for 6h under hydrogen flow to obtain W-Y with obviously improved distribution of yttrium oxide in a tungsten matrix2O3And (3) alloying. From the TEM image of FIG. 1b, it can be seen that W-Y was prepared under acidic hydrothermal conditions2O3Compared with the alloy (FIG. 1a), the W alloy prepared by the invention has obviously refined yttrium oxide at grain boundaries (the average size is refined from 420nm to 105 nm).
Example 2
(1) Dissolving 8g of ammonium metatungstate, 0.1g of PVP and 0.16g of yttrium nitrate hexahydrate in 40mL of deionized water, and after completely dissolving the ammonium metatungstate, adjusting the pH of the solution to 10 by using ammonia water (the concentration of ammonium metatungstate in the solution is 0.2g/mL, the mass of yttrium nitrate hexahydrate is 0.02 times of that of ammonium metatungstate, and the concentration of polyvinylpyrrolidone in the solution is 0.0025 g/mL);
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 170 ℃ for 24 hours;
(3) after the temperature of the reaction kettle is reduced to room temperature, filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, placing the obtained precipitate in a drying oven to be dried to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 1h in argon gas flow at 500 ℃ to obtain composite oxide powder;
(4) the composite oxide powder is reduced in two steps in hydrogen gas flow, the first step reduction temperature is 580 ℃, the reduction time is 3 hours, then the temperature is raised to 800 ℃ for the second step reduction, the reduction time is 2 hours, and then the W-Y is obtained after the temperature is cooled to the room temperature in the hydrogen atmosphere2O3The precursor powder is compounded, the heating rate is 5 ℃/min, and the air flow is 100 mL/min.
(5) Pressing the obtained composite precursor powder into a compact, and sintering the compact at 1800 ℃ for 4h under hydrogen flow to obtain W-Y with obviously improved distribution of yttrium oxide in a tungsten matrix2O3And (3) alloying. From the TEM image of FIG. 2bIt is shown that the W-Y prepared under acidic hydrothermal conditions2O3Compared with the alloy (fig. 2a), the volume fraction of the yttrium oxide distributed in the crystal grains in the W alloy prepared by the invention is obviously improved (from 6.7 percent to 35.5 percent).
Example 3
(1) 6g of ammonium metatungstate, 0.2g of PVP and 0.16g of yttrium nitrate hexahydrate are dissolved in 40mL of deionized water, and after the ammonium metatungstate, the pH value of the solution is adjusted to 11 by using ammonia water (the concentration of ammonium metatungstate in the solution is 0.15g/mL, the mass of yttrium nitrate hexahydrate is 0.026 times that of ammonium metatungstate, and the concentration of polyvinylpyrrolidone in the solution is 0.005 g/mL);
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 200 ℃ for 12 hours;
(3) after the temperature of the reaction kettle is reduced to room temperature, filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, placing the obtained precipitate in a drying box for drying to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 2 hours in argon gas flow at 480 ℃ to obtain composite oxide powder;
(4) the composite oxide powder is reduced in two steps in hydrogen gas flow, the first step reduction temperature is 650 ℃, the reduction time is 2 hours, then the temperature is raised to 700 ℃ for the second step reduction, the reduction time is 4 hours, and then the W-Y is obtained after the temperature is cooled to the room temperature in the hydrogen atmosphere2O3The precursor powder is compounded, the heating rate is 5 ℃/min, and the air flow is 100 mL/min.
(5) Pressing the obtained composite precursor powder into a compact, and sintering the compact at 1700 ℃ for 4h under the flow of hydrogen to obtain W-Y with obviously improved distribution of yttrium oxide in the tungsten matrix2O3And (3) alloying. From the TEM image of FIG. 3b, it can be seen that W-Y was prepared under acidic hydrothermal conditions2O3Compared with the alloy (FIG. 3a), the grain structure of the W alloy prepared by the invention is obviously refined (the average size is refined from 580nm to 410 nm).
Example 4
(1) Dissolving 7g of ammonium metatungstate, 0.15g of PVP and 0.12g of yttrium nitrate hexahydrate in 40mL of deionized water, and after completely dissolving the ammonium metatungstate, adjusting the pH value of the solution to 10 by using ammonia water (the concentration of ammonium metatungstate in the solution is 0.175g/mL, the mass of yttrium nitrate hexahydrate is 0.017 times of that of ammonium metatungstate, and the concentration of polyvinylpyrrolidone in the solution is 0.004 g/mL);
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 180 ℃ for 16 hours;
(3) after the temperature of the reaction kettle is reduced to room temperature, filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, placing the obtained precipitate in a drying box for drying to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 1.5 hours in argon gas flow at 450 ℃ to obtain composite oxide powder;
(4) the composite oxide powder is reduced in two steps in hydrogen gas flow, the first step reduction temperature is 580 ℃, the reduction time is 4 hours, then the temperature is raised to 750 ℃ for the second step reduction, the reduction time is 3 hours, and then the W-Y is obtained after the temperature is cooled to room temperature in the hydrogen atmosphere2O3The precursor powder is compounded, the heating rate is 5 ℃/min, and the air flow is 100 mL/min.
(5) Pressing the obtained composite precursor powder into a compact, and sintering the compact for 5 hours at 1600 ℃ under hydrogen airflow to obtain W-Y with obviously improved distribution of yttrium oxide in a tungsten matrix2O3And (3) alloying.
While the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the art that the methods and techniques described herein can be modified or re-combined to achieve the desired end result without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (4)
1. A preparation method for improving oxide distribution in a yttrium oxide dispersion strengthening tungsten alloy is characterized by comprising the following steps:
(1) dissolving polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate in deionized water, adjusting the pH value of the solution to 9-11 by using ammonia water after the polyvinylpyrrolidone, ammonium metatungstate and yttrium nitrate hexahydrate are fully dissolved, and then mechanically stirring the solution to fully react;
(2) pouring the suspension obtained by the reaction into a hydrothermal reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at the temperature of 170-200 ℃ for 12-24 h;
(3) filtering the suspension liquid after the hydrothermal reaction, washing the obtained precipitate with absolute ethyl alcohol, drying the obtained precipitate in a drying oven to obtain composite powder, then placing the composite powder in a tubular furnace, and calcining for 1-2 hours in argon gas flow at 450-500 ℃ to obtain composite oxide powder;
(4) carrying out two-step reduction on the obtained composite oxide powder in a tubular furnace by using pure hydrogen, wherein the temperature of the first-step reduction is 580-650 ℃, and the reduction time is 2-4 h; then raising the temperature to 700-800 ℃ for the second step of reduction for 2-4 h to obtain W-Y2O3The composite precursor powder of (1);
(5) the obtained composite precursor powder is pressed into a block and sintered for 4-6h at the temperature of 1600 plus 1800 ℃ in the hydrogen atmosphere to obtain W-Y with obviously improved distribution of yttrium oxide in the tungsten matrix2O3And (3) alloying.
2. The method according to claim 1, wherein the concentration of ammonium metatungstate in the solution in step (1) is: 0.15-0.2 g/mL.
3. The method according to claim 1, wherein the mass of yttrium nitrate hexahydrate in step (1) is 0.013 to 0.026 times the mass of ammonium metatungstate.
4. The method according to claim 1, wherein the concentration of polyvinylpyrrolidone in the solution in step (1) is 0.0025 to 0.005 g/mL.
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| KR20160133046A (en) * | 2015-05-11 | 2016-11-22 | 주식회사 마프로 | Method for manufacturing doped thermochromic nano particle and method for manufacturing thermochromic film |
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