CN111593245A - Solid solution type tungsten-based alloy and preparation method thereof - Google Patents
Solid solution type tungsten-based alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a solid solution type tungsten-based alloy, which comprises a tungsten matrix and an additive element; the additive elements comprise titanium and high-melting-point elements which can form a continuous solid solution with tungsten and have larger differences between the atomic size and the elasticity of the elements and the tungsten; the invention also discloses a preparation method of the solid solution type tungsten-based alloy, which comprises the following steps: firstly, taking tungsten powder, high-melting-point element powder and spherical titanium powder, and carrying out ball milling and mixing to obtain mixed powder; and secondly, preparing the solid solution type tungsten-based alloy by using the mixed powder as a raw material and adopting a powder bed electron beam 3D printing method. According to the invention, high-melting-point elements are added into a tungsten matrix, the crystal structure of tungsten is adjusted through solid solution, and meanwhile, titanium is added for purification and dispersion strengthening, so that the plasticity and strength of the tungsten-based alloy are improved; according to the invention, raw material powder is uniformly ground and mixed to form mixed powder with nanometer high-melting-point element powder adhered to the surfaces of spherical tungsten powder and titanium powder, and then a powder bed electron beam 3D printing method is adopted to form continuous solid solution between tungsten and the high-melting-point element, so that the purification and strengthening effects of titanium are ensured.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a solid solution type tungsten-based alloy and a preparation method thereof.
Background
Tungsten has high density, high hardness, high wear resistance and excellent radiation resistance, and is widely applied in the fields of metallurgy, machinery, military, nuclear related fields and the like. However, industrial pure tungsten is a brittle material, the ductile-brittle transition temperature is as high as 250 ℃ to 400 ℃, and the plastic property is almost not generated at room temperature, so that the use environment is limited to a certain extent. The main reasons for the brittleness and the influence on the mechanical properties of the pure tungsten material are two aspects: one is determined by the intrinsic structure of tungsten. Secondly, because the O, S, N, P and other interstitial impurity elements are distributed along the grain boundary, the solubility of the elements in tungsten is very low, most of the elements are partially gathered at the grain boundary to form an embrittlement layer film, the bonding strength of the grain boundary is reduced, and intercrystalline brittle failure is caused.
At present, the methods for improving the brittleness of tungsten in the prior art mainly include the following methods: (1) the preparation method is improved, such as the impurity content in the tungsten material is reduced from the source by methods of vacuum sintering, zone melting and the like, and the toughness of tungsten is improved; (2) by large high temperature plastic deformation, such as: the method of rotary swaging, hot rolling, twisting and the like improves the microstructure of the tungsten material and refines tungsten grains; (3) the performance of the tungsten-based material is improved through component and structure design, the most feasible alloy element for improving the plasticity of the alloy is rhenium at present, but the storage amount of rhenium is low, the material cost is greatly improved when the tungsten-rhenium alloy is prepared, and meanwhile, the rhenium can be transmuted into a high-radioactivity active element Os to cause irradiation embrittlement under a neutron irradiation environment.
Disclosure of Invention
The present invention is directed to provide a solid-solution tungsten-based alloy in order to overcome the above-mentioned shortcomings of the prior art. The alloy adds high-melting-point elements into a tungsten matrix, adjusts the crystal structure of tungsten in a solid solution mode, enhances the atomic bonding force and lattice distortion, and increases the resistance of dislocation slippage, thereby achieving the purpose of improving the plasticity of the tungsten-based alloy.
In order to solve the technical problems, the invention adopts the technical scheme that: a solid solution type tungsten-based alloy is characterized by comprising a tungsten matrix and an additive element; the additive elements comprise titanium and high-melting-point elements which can form a continuous solid solution with tungsten and have larger differences in atomic size and elasticity with tungsten.
According to the invention, high-melting-point elements which can form a continuous solid solution with tungsten and have larger differences between the atomic size and the elasticity of the elements and tungsten are added into a tungsten substrate, and the crystal structure of tungsten is adjusted in a solid solution manner, so that the atomic bonding force and lattice distortion are enhanced, the resistance of dislocation slippage is increased, and the purpose of improving the plasticity of the tungsten-based alloy is realized; simultaneously, active metal element titanium is added, and the titanium adsorbs oxygen in an alloy system to form TiO in the alloy forming process2And volatilizing to realize synchronous purification of tungsten in the preparation process of the tungsten-based alloy, further controlling the oxygen content of the tungsten-based alloy grain boundary and further improving the plasticity of the tungsten-based alloy, and a small amount of non-volatilized TiO2As dispersed particle reinforced alloy, free O impurity exists in the form of stable compound through micro-alloying, so that the embrittlement of the alloy is reduced, the formed stable compound also plays a role in strengthening, and particles of the stable compound are dispersed and distributed in a tungsten matrix and can limit the migration of crystal boundary and dislocation, thereby inhibiting the growth of crystal grains, playing a role in refining the crystal grains, and obviously improving the effect of refining the crystal grainsRoom and high temperature strength, high temperature stability, and recrystallization temperature of tungsten-based alloys.
The solid solution tungsten-based alloy is characterized in that the high melting point element is tantalum, molybdenum or niobium. The preferred high-melting-point element can form a good continuous solid solution with tungsten, and the atomic size and elasticity of the high-melting-point element are greatly different from those of tungsten, so that the solid solution strengthening effect is better realized.
The solid solution type tungsten-based alloy is characterized in that the mass content of high melting point elements in the solid solution type tungsten-based alloy is 3-20%, and the mass content of titanium elements is 1-2%. The content of the preferred high-melting-point element can be uniformly distributed on the surface of the tungsten powder on the premise of ensuring the solid solution strengthening effect, and the content of the preferred titanium element is favorable for fully adsorbing oxygen in the alloy and volatilizing completely as much as possible.
In addition, the invention also provides a preparation method of the solid solution type tungsten-based alloy, which is characterized by comprising the following steps:
step one, taking tungsten powder, high-melting-point element powder and spherical titanium powder, and carrying out ball milling and mixing to obtain mixed powder;
and step two, preparing the solid solution type tungsten-based alloy by using the mixed powder obtained in the step one as a raw material and adopting a powder bed electron beam 3D printing method.
The invention ball-milling mixes the tungsten powder, the high melting point element powder and the spherical titanium powder, improves the uniformity of the mixed powder, avoids the segregation of the elements, is prepared by adopting a powder bed electron beam 3D printing method, is beneficial to forming continuous solid solution by the tungsten and the high melting point element, and simultaneously forms TiO under the condition of low energy input by utilizing the characteristic that the powder bed electron beam 3D printing heats a single-layer powder bed quickly by the electron beam2The purification and strengthening effects of the active metal element titanium are ensured, so that the plasticity of the tungsten-based alloy is improved, and the strength of the tungsten-based alloy is improved.
The method is characterized in that in the step one, the tungsten powder is spherical tungsten powder with the particle size of 10-50 microns, the particle size of the high-melting-point element powder is smaller than 150nm, and the particle size of the spherical titanium powder is smaller than 30 microns. The high-melting-point element is added in the form of nano powder, so that the volume content of the high-melting-point element is increased, and the adoption of the optimized raw material powder is beneficial to the uniform adhesion of the high-melting-point element nano powder after ball milling to the surfaces of large-particle spherical tungsten powder and spherical tungsten powder to form composite powder, so that the segregation phenomenon of the element is avoided to the greatest extent.
The method is characterized in that the grinding ball adopted in the ball milling and mixing in the step one is Al2O3The diameter of the grinding ball is 3-5 mm, and the ball material ratio is (5-20): 1, the rotation speed of ball milling and mixing is 300 r/min-500 r/min, and the time is 10 h-30 h. The optimized ball milling process ensures the bonding strength between the high-melting-point elements and the tungsten powder and the spherical titanium powder, and simultaneously avoids the spherical tungsten powder from obviously deforming and crushing.
The method is characterized in that the high-melting-point element powder in the mixed powder in the step one is adhered to the surfaces of the tungsten powder and the titanium powder in a nano form.
The method is characterized in that the preparation of the powder bed electron beam 3D printing method in the second step specifically comprises the following steps:
step 201, establishing a three-dimensional model according to a target product and carrying out layering processing on the three-dimensional model to obtain layering information;
step 202, adding the mixed powder obtained in the step one into a powder box of powder bed electron beam 3D printing forming equipment, then flowing out and flatly paving the mixed powder on a leveled forming bottom plate through a doctor blade to form a powder layer, and then carrying out stepped heating scanning on the powder layer by adopting electron beams according to the layering information obtained in the step 201 to form a single-layer solid sheet layer on the forming bottom plate;
and 203, descending the forming bottom plate of the single-layer solid sheet layer formed in the step 202, and then sequentially repeating the powder laying process and the heating scanning process in the step 202 until the single-layer solid sheet layer is stacked layer by layer to form the solid solution type tungsten-based alloy.
The method described above, wherein the step-wise heating scan in step 202 comprises: the current of the first heating scanning is 8 mA-10 mA, and the speed is 3 m/s-5 m/s; the current of the second heating scanning is 9 mA-12 mA,the speed is 1 m/s-2 m/s; the current of the third heating scanning is 9 mA-12 mA, and the speed is 0.1 m/s-0.5 m/s. The first heating scanning process of the optimized stepped heating scanning heats the powder bed to enable titanium powder in the powder bed to form TiO after adsorbing oxygen2(ii) a The current is increased in the second heating scanning process to melt the powder bed, so that the primary solid solution of the high-melting-point element in the tungsten matrix is realized, and meanwhile, TiO formed in the first heating scanning process2Volatilizing to take away most of oxygen in the powder bed so as to achieve the aim of purifying the alloy; the third heating scanning process realizes the complete melting of the powder bed, completes the densification process and further promotes the solid solution of high-melting-point elements in the tungsten matrix.
Compared with the prior art, the invention has the following advantages:
1. the invention adds high melting point elements into the tungsten matrix, adjusts the crystal structure of tungsten by a solid solution mode, enhances the atom bonding force and lattice distortion, increases the resistance of dislocation slippage, thereby realizing the purpose of improving the plasticity of the tungsten-based alloy, simultaneously adds titanium, realizes the synchronous purification of tungsten, plays a role in dispersion strengthening, further improves the plasticity of the tungsten-based alloy, and also obviously improves the strength of the tungsten-based alloy.
2. The high-melting-point element is added in the form of nano powder, so that the volume content of the high-melting-point element is increased, the high-melting-point element nano powder is favorably and uniformly adhered to the surfaces of large-particle spherical tungsten powder and spherical tungsten powder after ball milling, and the composite powder is formed, so that the segregation phenomenon of the element is avoided.
3. The high-melting-point element nano powder has high surface activity, so that a large amount of oxygen is adsorbed on the surface, and is gathered to a crystal boundary in the melting and solidification process to influence the crystal boundary strength of the tungsten-based alloy and further influence the performance of the tungsten-based alloy, and the titanium and the oxygen adsorbed on the surface of the high-melting-point element nano powder are added into the tungsten-based alloy to generate TiO2The purification and dispersion strengthening effects of titanium are exerted, and the plasticity and strength of the tungsten-based alloy are further improved.
4. According to the invention, a three-step heating scanning mode is adopted in the 3D printing and forming process of the powder bed electron beam, and the tungsten-based alloy is promoted to form a compact body while being purified by step control, so that the solid solution of high-melting-point elements in a tungsten matrix is promoted.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The solid solution tungsten-based alloy of the embodiment comprises a tungsten matrix and additive elements of tantalum and titanium, wherein the mass content of tantalum in the solid solution tungsten-based alloy is 3%, and the mass content of titanium in the solid solution tungsten-based alloy is 1%.
The preparation method of the solid solution tungsten-based alloy of the embodiment comprises the following steps:
step one, ball-milling and mixing 9.6kg of spherical tungsten powder with the particle size of 10-50 microns, 0.3kg of tantalum powder with the particle size of less than 150nm and 0.1kg of spherical titanium powder with the particle size of less than 30 microns to obtain mixed powder with tantalum powder adhered to the surfaces of the spherical tungsten powder and the spherical titanium powder; the grinding ball adopted by ball milling is Al2O3Grinding balls with the diameter of 3mm and the ball-material ratio of 5:1, wherein the rotation speed of ball-milling mixing is 300r/min, and the time is 30 h;
step two, preparing the solid solution type tungsten-based alloy by using the mixed powder obtained in the step one as a raw material and adopting a powder bed electron beam 3D printing method; the preparation method of the powder bed electron beam 3D printing method specifically comprises the following steps:
step 201, establishing a three-dimensional model according to a target product and carrying out layering processing on the three-dimensional model to obtain layering information;
step 202, adding the mixed powder obtained in the step one into a powder box of powder bed electron beam 3D printing forming equipment, then flowing out and flatly paving the mixed powder on a leveled forming bottom plate through a doctor blade to form a powder layer, and then carrying out stepped heating scanning on the powder layer by adopting electron beams according to the layering information obtained in the step 201 to form a single-layer solid sheet layer on the forming bottom plate; the step-type heating scanning process comprises the following steps: the current of the first heating scanning is 8mA, and the speed is 3 m/s; the current of the second heating scanning is 9mA, and the speed is 1 m/s; the current of the third heating scanning is 9mA, and the speed is 0.1 m/s;
and 203, descending the forming bottom plate of the single-layer solid sheet layer formed in the step 202, and then sequentially repeating the powder laying process and the heating scanning process in the step 202 until the single-layer solid sheet layer is stacked to form the solid solution type tungsten-based alloy.
Example 2
The solid solution tungsten-based alloy of the embodiment includes a tungsten matrix and additive elements of molybdenum and titanium, wherein the mass content of molybdenum in the solid solution tungsten-based alloy is 15%, and the mass content of titanium in the solid solution tungsten-based alloy is 2%.
The preparation method of the solid solution tungsten-based alloy of the embodiment comprises the following steps:
step one, taking 8.3kg of spherical tungsten powder with the particle size of 15-45 microns, 1.5kg of molybdenum powder with the particle size of less than 150nm and 0.2kg of spherical titanium powder with the particle size of less than 25 microns for ball milling and mixing to obtain mixed powder with the molybdenum powder adhered to the surfaces of the spherical tungsten powder and the spherical titanium powder; the grinding ball adopted by ball milling is Al2O3Grinding balls with the diameter of 5mm and the ball-material ratio of 20:1, wherein the rotation speed of ball-milling mixing is 500r/min, and the time is 10 h;
step two, preparing the solid solution type tungsten-based alloy by using the mixed powder obtained in the step one as a raw material and adopting a powder bed electron beam 3D printing method; the preparation method of the powder bed electron beam 3D printing method specifically comprises the following steps:
step 201, establishing a three-dimensional model according to a target product and carrying out layering processing on the three-dimensional model to obtain layering information;
step 202, adding the mixed powder obtained in the step one into a powder box of powder bed electron beam 3D printing forming equipment, then flowing out and flatly paving the mixed powder on a leveled forming bottom plate through a doctor blade to form a powder layer, and then carrying out stepped heating scanning on the powder layer by adopting electron beams according to the layering information obtained in the step 201 to form a single-layer solid sheet layer on the forming bottom plate; the step-type heating scanning process comprises the following steps: the current of the first heating scanning is 10mA, and the speed is 5 m/s; the current of the second heating scanning is 12mA, and the speed is 2 m/s; the current of the third heating scanning is 12mA, and the speed is 0.5 m/s;
and 203, descending the forming bottom plate of the single-layer solid sheet layer formed in the step 202, and then sequentially repeating the powder laying process and the heating scanning process in the step 202 until the single-layer solid sheet layer is stacked to form the solid solution type tungsten-based alloy.
Example 3
The solid solution tungsten-based alloy of the embodiment includes a tungsten matrix and additive elements niobium and titanium, wherein the mass content of niobium in the solid solution tungsten-based alloy is 20%, and the mass content of titanium in the solid solution tungsten-based alloy is 1.5%.
The preparation method of the solid solution tungsten-based alloy of the embodiment comprises the following steps:
taking 7.85kg of spherical tungsten powder with the particle size of 10-50 microns, 2kg of niobium powder with the particle size of less than 150nm and 0.15kg of spherical titanium powder with the particle size of less than 30 microns for ball milling and mixing to obtain mixed powder with the niobium powder adhered to the surfaces of the spherical tungsten powder and the spherical titanium powder; the grinding ball adopted by ball milling is Al2O3Grinding balls with the diameter of 3-5 mm and the ball-material ratio of 10:1, wherein the rotation speed of ball-milling mixing is 400r/min, and the time is 15 h;
step two, preparing the solid solution type tungsten-based alloy by using the mixed powder obtained in the step one as a raw material and adopting a powder bed electron beam 3D printing method; the preparation method of the powder bed electron beam 3D printing method specifically comprises the following steps:
step 201, establishing a three-dimensional model according to a target product and carrying out layering processing on the three-dimensional model to obtain layering information;
step 202, adding the mixed powder obtained in the step one into a powder box of powder bed electron beam 3D printing forming equipment, then flowing out and flatly paving the mixed powder on a leveled forming bottom plate through a doctor blade to form a powder layer, and then carrying out stepped heating scanning on the powder layer by adopting electron beams according to the layering information obtained in the step 201 to form a single-layer solid sheet layer on the forming bottom plate; the step-type heating scanning process comprises the following steps: the current of the first heating scanning is 9mA, and the speed is 4 m/s; the current of the second heating scanning is 10mA, and the speed is 1.5 m/s; the current of the third heating scanning is 10mA, and the speed is 0.3 m/s;
and 203, descending the forming bottom plate of the single-layer solid sheet layer formed in the step 202, and then sequentially repeating the powder laying process and the heating scanning process in the step 202 until the single-layer solid sheet layer is stacked to form the solid solution type tungsten-based alloy.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
1. A solid solution type tungsten-based alloy is characterized by comprising a tungsten matrix and an additive element; the additive elements comprise titanium and high-melting-point elements which can form a continuous solid solution with tungsten and have larger differences in atomic size and elasticity with tungsten.
2. A solid solution tungsten-based alloy according to claim 1, wherein said high melting point element is tantalum, molybdenum or niobium.
3. The solid solution tungsten-based alloy according to claim 1, wherein the solid solution tungsten-based alloy contains 3 to 20% by mass of a high melting point element and 1 to 2% by mass of a titanium element.
4. A method for producing the solid solution tungsten-based alloy according to any one of claims 1 to 3, comprising the steps of:
step one, taking tungsten powder, high-melting-point element powder and spherical titanium powder, and carrying out ball milling and mixing to obtain mixed powder;
and step two, preparing the solid solution type tungsten-based alloy by using the mixed powder obtained in the step one as a raw material and adopting a powder bed electron beam 3D printing method.
5. The method of claim 4, wherein in the first step, the tungsten powder is spherical tungsten powder with a particle size of 10-50 μm, the high melting point element powder has a particle size of less than 150nm, and the spherical titanium powder has a particle size of less than 30 μm.
6. The method of claim 4, wherein the milling balls used in the ball milling and mixing in the first step are Al2O3The diameter of the grinding ball is 3-5 mm, and the ball material ratio is (5-20): 1, the rotation speed of ball milling and mixing is 300 r/min-500 r/min, and the time is 10 h-30 h.
7. The method according to claim 4, wherein the refractory element powder in the mixed powder in the first step is adhered to the surfaces of the tungsten powder and the titanium powder in a nano form.
8. The method according to claim 4, wherein the preparation of the powder bed electron beam 3D printing method in the second step specifically comprises the following steps:
step 201, establishing a three-dimensional model according to a target product and carrying out layering processing on the three-dimensional model to obtain layering information;
step 202, adding the mixed powder obtained in the step one into a powder box of powder bed electron beam 3D printing forming equipment, then flowing out and flatly paving the mixed powder on a leveled forming bottom plate through a doctor blade to form a powder layer, and then carrying out stepped heating scanning on the powder layer by adopting electron beams according to the layering information obtained in the step 201 to form a single-layer solid sheet layer on the forming bottom plate;
and 203, descending the forming bottom plate of the single-layer solid sheet layer formed in the step 202, and then sequentially repeating the powder laying process and the heating scanning process in the step 202 until the single-layer solid sheet layer is stacked layer by layer to form the solid solution type tungsten-based alloy.
9. The method of claim 8, wherein the step-wise heating scan in step 202 is performed by: the current of the first heating scanning is 8 mA-10 mA, and the speed is 3 m/s-5 m/s; the current of the second heating scanning is 9 mA-12 mA, and the speed is 1 m/s-2 m/s; the current of the third heating scanning is 9 mA-12 mA, and the speed is 0.1 m/s-0.5 m/s.
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| CN113134612A (en) * | 2021-04-12 | 2021-07-20 | 中南大学 | Method for preparing superfine high-purity high-solid-solubility tungsten-based alloy powder |
| CN113215462A (en) * | 2021-05-13 | 2021-08-06 | 中南大学 | Preparation of W-Ta single-phase solid solution material based on suspension induction melting |
| CN114160789A (en) * | 2021-12-09 | 2022-03-11 | 西安交通大学 | Method for enhancing performance of 3D printed metal product through surface coating of printing raw material |
| CN116334463A (en) * | 2023-04-28 | 2023-06-27 | 中南大学 | Ultra-long high-strength ultra-fine tungsten alloy wire and preparation method thereof |
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| CN114160789A (en) * | 2021-12-09 | 2022-03-11 | 西安交通大学 | Method for enhancing performance of 3D printed metal product through surface coating of printing raw material |
| CN116334463A (en) * | 2023-04-28 | 2023-06-27 | 中南大学 | Ultra-long high-strength ultra-fine tungsten alloy wire and preparation method thereof |
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