CN109518023B - Method for improving use tolerance temperature of tungsten-aluminum composite material - Google Patents
Method for improving use tolerance temperature of tungsten-aluminum composite material Download PDFInfo
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Abstract
The invention discloses a method for improving the use tolerance temperature of a tungsten-aluminum composite material, belonging to the technical field of powder metallurgy. The method comprises the following steps: (1) mechanically mixing aluminum powder and rare earth oxide to obtain pretreated aluminum powder; (2) mechanically mixing the pretreated aluminum powder obtained in the step (1) with tungsten powder to obtain composite powder; (3) and (3) carrying out vacuum degassing and hot extrusion forming on the composite powder obtained in the step (2) to obtain the tungsten-aluminum composite material. The method is simple, high in efficiency and easy for industrial production; the prepared tungsten-aluminum composite material can be applied in a higher temperature environment, and the application range of the tungsten-aluminum composite material is widened.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a method for improving the use tolerance temperature of a tungsten-aluminum composite material.
Background
The tungsten-aluminum composite material is an aluminum-based composite material which takes aluminum or aluminum alloy as a matrix and takes tungsten as a main additive phase, and the material combines excellent mechanical property and radiation-resistant shielding property, so that the tungsten-aluminum composite material has a wide application prospect.
The tungsten-aluminum composite material prepared by the powder metallurgy method is easy to react at the original tungsten/aluminum interface and generate WAl in the use in a high-temperature environment12Or WAl5An intermetallic compound. The occurrence of the interface reaction not only deteriorates the mechanical performance indexes such as strength, plasticity and the like of the composite material, but also causes physical damage to other related important devices due to the rapid expansion of the overall size of the material. In conclusion, the improvement of the use tolerance temperature of the tungsten-aluminum composite material has very important significance.
Disclosure of Invention
The invention aims to provide a method for improving the use tolerance temperature of a tungsten-aluminum composite material, which has the following specific technical scheme:
a method for improving the use endurance temperature of a tungsten-aluminum composite material is characterized by comprising the following steps:
(1) mechanically mixing aluminum powder and rare earth oxide to obtain pretreated aluminum powder;
(2) mechanically mixing the pretreated aluminum powder obtained in the step (1) with tungsten powder to obtain composite powder;
(3) and (3) carrying out vacuum degassing and hot extrusion forming on the composite powder obtained in the step (2) to obtain the tungsten-aluminum composite material.
The aluminum powder is high-purity aluminum powder and/or aluminum alloy powder; the aluminum alloy is preferably 2A12 aluminum alloy powder or 6063 aluminum alloy powder.
Preferably, the purity of the high-purity aluminum powder is more than 99%, and the particle size is 1-20 microns; the granularity of the aluminum alloy powder is less than 100 meshes.
The rare earth oxide is cerium oxide and/or cerium-based composite rare earth oxide, and the mass percentage of cerium oxide in the cerium-based composite rare earth oxide is more than or equal to 50%.
The cerium-based composite rare earth oxide is preferably CeO2-La2O3、CeO2-Nd2O3、CeO2-La2O3-Nd2O3One or more of (a).
The mass ratio of the aluminum powder to the rare earth oxide is 70: 30-95: 5.
The mechanical mixing in the step (1) comprises premixing and double-cone motion mixing; the premixing is free of grinding media, overturning mixing is adopted, the rotating speed of a turnover shaft and the horizontal direction is 45 degrees, the rotating speed of a mixing barrel is 5-30 r/min, and the premixing time is 2-10 h; the double-cone motion is mixed with grinding medium steel balls, a double-cone mixing barrel is adopted, and the ball-material ratio is 1: 1-3: 1.
The ball-material ratio in the double-cone motion mixing is adjusted according to the mass ratio of the aluminum powder to the rare earth oxide.
And (2) mixing and proportioning 30-80% of pre-treated aluminum powder and 20-70% of tungsten powder by mass.
The mechanical mixing of step (2) is preferably double-cone motion mixing: pouring the pretreated aluminum powder and tungsten powder into a biconical mixing barrel, mixing the powder for 12-48 h in the air by a grinding ball-powder weight ratio of 1:1, and obtaining the composite powder.
And (3) vacuum degassing, namely filling the composite powder obtained in the step (2) into an aluminum sheath, compacting, and then performing vacuum degassing on the aluminum sheath at the degassing temperature of 300-450 ℃ and the vacuum degree of less than 1 × 103And sealing the aluminum sheath after Pa, and degassing for not less than 6 h.
The extrusion temperature of the hot extrusion molding in the step (3) is 350-550 ℃, and the extrusion ratio is 8: 1-13: 1.
The mechanism for improving the use tolerance temperature of the tungsten-aluminum composite material is as follows: pretreating aluminum powder to form a coating layer on the surface of the aluminum powder; the existence of the coating layer at the tungsten/aluminum interface forms a barrier to the diffusion of tungsten element, thereby increasing the starting temperature of the interface reaction and enabling the tungsten-aluminum composite material to be used at higher temperature.
The invention has the beneficial effects that: based on the characteristics that cerium oxide and cerium-based composite rare earth oxide are soft and easy to bond with metal, the surface of aluminum powder is completely coated by using a mechanical mixing mode, so that the problems of needing professional equipment, high production cost and low efficiency in the prior art that a coating layer is formed on the surface of metal powder by using chemical deposition or physical sputtering and the like are solved; the method is simple, high in efficiency and easy for industrial production; compared with the tungsten-aluminum composite material which is not pretreated by aluminum powder, the tungsten-aluminum composite material prepared by the invention has the advantages that the use tolerance temperature is obviously improved, the tungsten-aluminum composite material can be applied in a higher temperature environment, and the application range of the tungsten-aluminum composite material is widened.
Drawings
FIG. 1 is a scanning electron microscope picture of an original aluminum powder without pretreatment;
FIG. 2 is a scanning electron microscope picture of pretreated aluminum powder;
FIG. 3 is a schematic diagram showing a differential scanning calorimetry analysis curve and a thermal expansion curve of a tungsten-aluminum composite material prepared by pretreating with aluminum powder and a tungsten-aluminum composite material prepared without pretreating with aluminum powder; wherein T is1The temperature is the starting temperature/dimension instability temperature of the interface reaction of the tungsten-aluminum composite material prepared by aluminum powder pretreatment; t is2The temperature is the starting temperature/dimension instability temperature of the interface reaction of the tungsten-aluminum composite material prepared without aluminum powder pretreatment.
Detailed Description
The invention provides a method for improving the use temperature resistance of a tungsten-aluminum composite material, and the invention is further described by combining the accompanying drawings and an embodiment.
Example 1
The tungsten-aluminum composite material with high temperature tolerance is prepared according to the following steps:
[a] preparing pre-treated aluminum powder
1) The mass ratio of the original aluminum powder to the rare earth oxide is 80:20, wherein the original aluminum powder is selected from high-purity aluminum powder, and the average particle size is 8 microns; the rare earth oxide is cerium-based composite rare earth oxide (80 wt% CeO)2-20wt％La2O3)。
2) And (3) introducing the two kinds of powder into a cylindrical mixing tank, and then performing turnover type medium-free premixing, wherein the turnover shaft and the horizontal direction form 45 degrees, the rotating speed of a mixing barrel is 20r/min, and the premixing time is 7 h.
3) After the premixing is finished, transferring the powder into a biconical mixing tank for grinding and mixing, wherein the grinding medium is stainless steel balls, the ball-material ratio is 1:1, mixing for 15h, discharging the powder to obtain pretreated aluminum powder, and sweepingThe SEM image is shown in FIG. 2. Comparing the scanning electron microscope images of the original aluminum powder without pretreatment shown in FIG. 1, it can be seen that the pretreated aluminum powder surface is coated with cerium-based composite rare earth oxide (80 wt% CeO)2-20wt％La2O3) And (4) completely coating.
[b] Preparing the composite powder.
And (c) mechanically mixing the pre-treated aluminum powder prepared in the step (a) with tungsten powder, wherein the mass ratio of the pre-treated aluminum powder to the tungsten powder is 50:50, and the particle size of the tungsten powder is 10 microns. Pouring the pretreated aluminum powder and tungsten powder into a biconical mixing barrel, selecting stainless steel balls as grinding media, mixing the stainless steel balls in a ball-to-material ratio of 1:1 in air for 18 hours to obtain uniformly mixed composite powder.
[c] Forming the composite material.
Step [ b ]]The prepared composite powder is put into an aluminum sheath and then is subjected to vacuum degassing treatment at the degassing temperature of 450 ℃ until the vacuum degree is lower than 1 × 103Sealing the aluminum sheath after Pa, and degassing for 10 h; then carrying out hot extrusion forming at the extrusion temperature of 500 ℃ in an extrusion ratio of 10: 1; thus obtaining the tungsten-aluminum composite material with high temperature resistance.
Comparative example 1
The same [ b ] as in example 1 was used without pretreating the original aluminum powder]And [ c)]Preparing the tungsten-aluminum composite material. The two composites obtained in example 1 and comparative example 1 were subjected to differential scanning calorimetry and thermal expansion tests, and a comparison graph shown in fig. 3 was obtained, showing that the tungsten-aluminum composite prepared by using the pretreated aluminum powder in example 1 has an interface reaction initiation temperature/dimensional instability initiation temperature (T) in a high-temperature use environment1635 ℃ C.) in comparison with the tungsten-aluminum composite material (T) obtained in comparative example 12Increased by 35 deg.c, and a significant increase in service temperature tolerance.
Example 2
The tungsten-aluminum composite material with high temperature tolerance is prepared according to the following steps:
[a] preparing pre-treated aluminum powder
1) The mass ratio of the original aluminum powder to the rare earth oxide is 94:6, wherein the original aluminum powder is 2A12 aluminum alloy powder with the particle size of 200 meshes; the rare earth oxide is cerium oxide with the purity of 99.5 percent.
2) And (3) introducing the two kinds of powder into a cylindrical mixing tank, and then performing turnover type medium-free premixing, wherein the turnover shaft and the horizontal direction form a 45-degree angle, the rotating speed of a mixing barrel is 10r/min, and the premixing time is 4 h.
3) After premixing, transferring the powder into a double-conical mixing tank for grinding and mixing, wherein a grinding medium is stainless steel balls, the ball-material ratio is 1:1, and discharging the powder after mixing for 10 hours to prepare pretreated aluminum powder; and comparing the scanning electron micrographs of the aluminum powder before and after the pretreatment, and finding that the surface of the aluminum powder after the pretreatment is completely coated by cerium oxide.
[b] Preparing the composite powder
Mechanically mixing the pre-treated aluminum powder prepared in the step (a) with tungsten powder in a certain proportion, wherein the mass ratio of the pre-treated aluminum powder to the tungsten powder is 70:30, and the particle size of the tungsten powder is 10 microns. Pouring the pretreated aluminum powder and tungsten powder into a biconical mixing barrel, selecting stainless steel balls as grinding media, mixing the stainless steel balls in a ball-to-material ratio of 1:1 in air for 18 hours to obtain uniformly mixed composite powder.
[c] Shaping of composite materials
Step [ b ]]The prepared composite powder is put into an aluminum sheath and then is subjected to vacuum degassing treatment at the degassing temperature of 400 ℃ until the vacuum degree is lower than 1 × 103And (4) sealing the aluminum sheath after Pa, and degassing for 10 h. Then hot extrusion forming is carried out, wherein the extrusion temperature is 430 ℃, and the extrusion ratio is 12: 1; thus obtaining the tungsten-aluminum composite material with high temperature resistance.
Comparative example 2
The same [ b ] as in example 2 was taken without pretreating the original aluminum powder]And [ c)]The tungsten-aluminum composite material is prepared. The results of differential scanning calorimetry and thermal expansion tests performed on the two composites obtained in example 2 and comparative example 2, plotted in a comparison graph shown in fig. 3, show that the interface reaction initiation temperature/dimensional instability initiation temperature (T) of the tungsten-aluminum composite prepared from the pre-treated aluminum powder in example 2 in a high-temperature environment1610 deg.C) as compared with the tungsten-aluminum composite material (T) prepared in comparative example 12The temperature is increased by 60 ℃ and the use tolerance temperature is obviously increased.
Example 3
The tungsten-aluminum composite material with high temperature tolerance is prepared according to the following steps:
[a] preparing pre-treated aluminum powder
1) The mass ratio of the original aluminum powder to the rare earth oxide is 90:10, wherein the original aluminum powder is 6063 aluminum alloy powder with the particle size of 150 meshes; the rare earth oxide is cerium oxide with the purity of 99.5 percent.
2) And (3) introducing the two kinds of powder into a cylindrical mixing tank, and then performing turnover type medium-free premixing, wherein the turnover shaft and the horizontal direction form a 45-degree angle, the rotating speed of a mixing barrel is 10r/min, and the premixing time is 4 h.
3) After premixing, transferring the powder into a double-conical mixing tank for grinding and mixing, wherein a grinding medium is stainless steel balls, the ball-material ratio is 1:1, and discharging the powder after mixing for 10 hours to prepare pretreated aluminum powder; and comparing the scanning electron micrographs of the aluminum powder before and after the pretreatment, and finding that the surface of the aluminum powder after the pretreatment is completely coated by cerium oxide.
[b] Preparing the composite powder
Mechanically mixing the pre-treated aluminum powder prepared in the step (a) with tungsten powder in a certain proportion, wherein the mass ratio of the pre-treated aluminum powder to the tungsten powder is 40:60, and the particle size of the tungsten powder is 10 microns. Pouring the pretreated aluminum powder and tungsten powder into a biconical mixing barrel, selecting stainless steel balls as grinding media, mixing the stainless steel balls in a ball-to-material ratio of 1:1 in air for 18 hours to obtain uniformly mixed composite powder.
[c] Shaping of composite materials
Step [ b ]]The prepared composite powder is put into an aluminum sheath and then is subjected to vacuum degassing treatment at the degassing temperature of 400 ℃ until the vacuum degree is lower than 1 × 103And (4) sealing the aluminum sheath after Pa, and degassing for 10 h. Then hot extrusion forming is carried out, the extrusion temperature is 450 ℃, and the extrusion ratio is 12: 1; thus obtaining the tungsten-aluminum composite material with high temperature resistance.
Comparative example 3
The same [ b ] as in example 3 was taken without pretreating the original aluminum powder]And [ c)]Preparing the tungsten-aluminum composite material. The two composites obtained in example 3 and comparative example 3 were subjected to differential scanning calorimetry and thermal expansion tests, and a comparative graph shown in FIG. 3 was drawn, and the results show that example 3 employs pretreated aluminumThe interface reaction starting temperature/size instability starting temperature (T) of the tungsten-aluminum composite material prepared from the powder in a high-temperature use environment1615 deg.C) as compared with the tungsten-aluminum composite material (T) prepared in comparative example 32Increased by 45 deg.c, a significant increase in service temperature.
Claims (6)
1. A method for improving the use endurance temperature of a tungsten-aluminum composite material is characterized by comprising the following steps:
(1) mechanically mixing aluminum powder and rare earth oxide to obtain pretreated aluminum powder;
(2) mechanically mixing the pretreated aluminum powder obtained in the step (1) with tungsten powder to obtain composite powder;
(3) vacuum degassing and hot extrusion molding are carried out on the composite powder obtained in the step (2) to obtain a tungsten-aluminum composite material;
the aluminum powder is high-purity aluminum powder and/or aluminum alloy powder; the rare earth oxide is cerium oxide and/or cerium-based composite rare earth oxide, and the mass percent of cerium oxide in the cerium-based composite rare earth oxide is more than or equal to 50%;
the cerium-based composite rare earth oxide is CeO2-La2O3、CeO2-Nd2O3、CeO2-La2O3-Nd2O3One or more of (a).
2. The method according to claim 1, wherein the mass ratio of the aluminum powder to the rare earth oxide is 70:30 to 95: 5.
3. The method according to claim 1, wherein the mechanical mixing in step (1) comprises premixing and double cone motion mixing; the premixing is free of grinding media, overturning mixing is adopted, the rotating speed of a turnover shaft and the horizontal direction is 45 degrees, the rotating speed of a mixing barrel is 5-30 r/min, and the premixing time is 2-10 h; the double-cone motion mixing takes steel balls as grinding media, and adopts a double-cone mixing barrel, wherein the ball-material ratio is 1: 1-3: 1.
4. The method according to claim 1, wherein the step (2) comprises the steps of mixing 30-80% of pre-treated aluminum powder and 20-70% of tungsten powder by mass; the mechanical mixing in the step (2) is double-cone motion mixing: the weight ratio of the grinding balls to the powder is 1:1, and the mixing time is 12-48 h.
5. The method according to claim 1, wherein the vacuum degassing in the step (3) is carried out by filling the composite powder obtained in the step (2) into an aluminum sheath, compacting the aluminum sheath, and then carrying out vacuum degassing on the aluminum sheath, wherein the degassing temperature is 300-450 ℃ and the vacuum degree is lower than 1 × 103And sealing the aluminum sheath after Pa, and degassing for not less than 6 h.
6. The method according to claim 1, wherein the extrusion temperature of the hot extrusion forming in the step (3) is 350-550 ℃, and the extrusion ratio is 8: 1-13: 1.
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