CN110129645B - Multifunctional tungsten alloy gradient material and preparation method thereof - Google Patents
Multifunctional tungsten alloy gradient material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multifunctional tungsten alloy gradient material and a preparation method thereof. The multifunctional tungsten alloy gradient material comprises two material sections according to the direction from one end of the material to the other end, wherein the material of the front section consists of tungsten and a metal additive, and the weight percentage range of the tungsten is 93-98%; the rear section material consists of tungsten and a metal additive, wherein the weight percentage range of the tungsten is 88-93%, and the tungsten content of the front section material is greater than that of the rear section material. According to the application requirements, the front section is required to have higher strength, and the rear section is required to have higher toughness. The preparation method of the multifunctional tungsten alloy gradient material comprises the following steps: the preparation method comprises the steps of preparing tungsten alloy powder, pressing and forming, sintering and heat treatment. The tungsten alloy gradient material prepared by the invention has good comprehensive mechanical properties.
Description
Technical Field
The invention relates to the field of metal materials, in particular to a multifunctional tungsten alloy gradient material and a preparation method thereof.
Background
The tungsten alloy is a metal alloy which takes tungsten as a matrix and is added with other elements. Tungsten has the characteristics of high melting point and large specific gravity, and other elements are added through reasonable component design, so that the characteristic of large brittleness of tungsten can be improved, and the alloy has higher practicability and flexibility. After the efforts of scholars at home and abroad, tungsten and tungsten alloy have obtained a series of excellent properties: high strength, good ductility, good processability, small thermal expansion coefficient, large thermal conductivity, excellent ray shielding effect, good oxidation resistance and corrosion resistance, and the like. Because of the above advantages, tungsten and tungsten alloys are widely used in the fields of medical treatment, electronic information, aerospace, military industry, and the like. However, with the increasing strengthening of military and civil engineering, the material performance is required to be higher and higher: not only has good comprehensive mechanical property, but also realizes the multifunction of the material as much as possible. In order to match with the demand direction of modern science and technology for new metal materials, the research works of improving the performance of tungsten alloy, improving the adaptability of the tungsten alloy in multiple environments, expanding the application range of the tungsten alloy and the like are urgent.
Disclosure of Invention
In view of the limitations of the prior art, it is an object of the present invention to provide a multifunctional tungsten alloy gradient material.
The second purpose of the present invention is to provide a method for preparing a multifunctional tungsten alloy gradient material.
A multifunctional tungsten alloy gradient material comprises two material sections according to the direction from one end of the material to the other end, wherein the material of the front section consists of tungsten and a metal additive, wherein the weight percentage range of the tungsten is 93-98%; the rear section material consists of tungsten and a metal additive, wherein the weight percentage range of the tungsten is 88-93%, and the tungsten content of the front section material is greater than that of the rear section material. According to the application requirements, the front section is required to have higher strength, and the rear section is required to have higher toughness.
The multifunctional tungsten alloy gradient material is integrally formed and comprises two material sections with different component distribution ratios, a combination part is arranged between the front section material and the rear section material, and the use directions of the front section material and the rear section material are determined according to the application environment in the use process.
In the above multifunctional tungsten alloy gradient material, as a preferred embodiment, in the front-stage material and the back-stage material, the metal additive comprises: nickel and iron, more preferably the metal additive further comprises cobalt and/or manganese, further preferably the metal additive further comprises molybdenum; further preferably, in the front-stage material, the content of the metal additive is as follows in percentage by weight: 1-5% of nickel, 1-3% of iron, 0-4% of cobalt and 0-0.5% of manganese; further preferably, 0.5-3% cobalt and 0.02-0.5% manganese; in the back-end material, the content of the metal additive is as follows in percentage by weight: 1-8% of nickel, 1-3% of iron, 0-4% of cobalt and 0-0.5% of manganese; further preferably, the cobalt is 0.5-3% and the manganese is 0.02-0.5%.
In the above multifunctional tungsten alloy gradient material, as a preferred embodiment, the front-stage material is composed of the following components in percentage by weight: 93% of W, 5% of Ni, 1% of Fe and 1% of Co; the rear section material comprises the following components: 90% of W, 7% of Ni, 2.5% of Fe and 0.5% of Co; alternatively, the front-end material is composed of the following components: 95% of W, 2% of Ni, 1% of Fe, 1.5% of Co and 0.5% of Mn; the rear section material comprises the following components: 93% of W, 5% of Ni, 1% of Fe and 1% of Co; alternatively, the front-end material is composed of the following components: 97% of W, 1% of Ni, 0.5% of Fe, 1% of Co and 0.5% of Mn; the rear section material comprises the following components: 95% of W, 2% of Ni, 1.5% of Fe and 1.5% of Co.
A preparation method of a multifunctional tungsten alloy gradient material comprises the following steps:
the preparation method of the tungsten alloy powder comprises the following steps: weighing the components and the weight ratio of the front-section material and the rear-section material in the multifunctional tungsten alloy gradient material according to any one of claims 1 to 4, respectively mixing the raw materials of the front-section material and the rear-section material, performing ball milling, and sieving to obtain tungsten alloy powder of the front-section material and tungsten alloy powder of the rear-section material;
a step of press forming: according to the design sequence of the front section material and the rear section material, sequentially filling the tungsten alloy powder of the front section material and the tungsten alloy powder of the rear section material into a die, and then performing compression molding to obtain a pressed blank;
sintering: sintering the pressed blank to obtain a tungsten alloy sintered blank;
a heat treatment step: and carrying out heat treatment on the tungsten alloy sintered blank to obtain the tungsten alloy material.
In the above preparation method, as a preferred embodiment, the preparation method further comprises a machining step of: machining the tungsten alloy material to obtain a tungsten alloy final product;
in the above preparation method, as a preferred embodiment, in the ball milling step, the fisher particle size of the tungsten powder is 2.0 to 4.0 μm (for example, 2.2 μm, 2.5 μm, 3 μm, 3.5 μm, 3.8 μm), the nickel powder is electrolytic nickel powder or nickel carbonyl powder, the iron powder is electrolytic iron powder or iron carbonyl powder, and the cobalt powder and manganese powder are conventional industrial powders.
In the above preparation method, as a preferred embodiment, in the ball milling step, the ball milling time is 2 to 8 hours (e.g., 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours), the rotation speed of the ball milling is 100 to 500r/min (e.g., 120r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min), and the ball-to-material ratio is 2:1 to 3: 1; preferably, the sieving is 80-140 mesh sieving (such as 80 mesh, 100 mesh, 120 mesh and 140 mesh).
In the above production method, as a preferred embodiment, in the press forming step, the press forming is cold isostatic pressing, the pressure of the cold isostatic pressing is 180 to 250MPa (such as 185MPa, 200MPa, 220MPa, 235MPa, 245MPa), and the dwell time is 5 to 15min (such as 6min, 8min, 10min, 13min, 14 min).
In the above production method, as a preferred embodiment, in the sintering step, the sintering is performed in a hydrogen atmosphere, and preferably, the sintering temperature is 1300 to 1550 ℃ (such as 1340 ℃, 1360 ℃, 1380 ℃, 1405 ℃, 1450 ℃, 1485 ℃, 1500 ℃, 1520 ℃, 1540 ℃, 1545 ℃), and the sintering time is 0.5 to 4h (such as 1h, 1.5h, 2h, 2.5h, 3h, 3.5 h).
In the above preparation method, as a preferred embodiment, in the heat treatment step, the heat treatment is performed under vacuum, the temperature of the heat treatment is 905 to 1200 ℃ (such as 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃), and the time of the heat treatment is 1 to 8 hours (such as 1.5 hours, 2 hours, 2.5 hours, 3 hours, 4.5 hours, 5 hours, 6 hours, 7 hours, 7.5 hours).
Through research and experiments, the invention fully utilizes the performance characteristics of the existing tungsten alloy with different components, finds out an integral component which is prepared by reasonably arranging and designing the tungsten alloy materials with different components and performances, and can greatly provide the functional adaptability of the tungsten alloy. For example, in the aspect of national defense industry, the penetration and blasting damage effects of the blasting combat part are effectively improved.
Compared with the prior art, the invention has the following beneficial effects:
the tungsten alloy provided by the invention is based on respective performance characteristics of tungsten alloys with different components, effectively integrates materials with different components on the basis of reasonable design, and aims to provide an all-in-one use scheme for actual needs of military and civil engineering. The prepared tungsten alloy material has good comprehensive mechanical property;
the preparation method of the invention uses a high-energy ball milling method to activate and mix the tungsten alloy raw material powder so as to refine the granularity of the powder and increase the specific surface area of the particles, so that the densification is easier in the sintering process, the sintering activity of the material is enhanced, the sintering performance of the material is improved, and in the sintering process, the diffusion among different components is more effectively ensured and the joint surface is strengthened.
Thirdly, the raw materials of the invention are loaded by product structure design and special mode to prepare a whole blank with multiple sections and different component proportions; then the processing technology comprises the steps of firing, vacuum heat treatment, deformation strengthening processing, aging treatment and the like. Through reasonable component proportion, structural design and preparation methods, the multifunctional tungsten alloy gradient material disclosed by the invention has excellent and stable comprehensive mechanical properties, and provides a reference for the design and development of a new-function armor-piercing projectile.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a metallographic structure photograph of a tungsten alloy material prepared by the preparation method of example 1 of the present invention.
Detailed Description
In order that the present invention may be more readily and clearly understood, there now follows a more particular description of the invention, reference being had to the accompanying drawings. The specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
The preparation process of the multifunctional tungsten alloy gradient material is shown in figure 1.
Example 1
Step one, preparation of tungsten alloy powder
A first component 93W5Ni1Fe1Co (corresponding numbers are the mass percent of each component in the alloy): 930g of tungsten powder with the Fisher size of 3.5 mu m, 50g of carbonyl nickel powder, 10g of electrolytic iron powder and 10g of cobalt powder are respectively weighed, mixed and then put into a high-energy ball mill, 2Kg of hard alloy balls are added, ball milling is carried out for 4 hours under the condition that the rotating speed is 120r/min, 1000g of alloy powder mixed with trace cobalt elements is obtained, then the alloy powder is sieved by a 120-mesh sieve, and undersize powder is used as a first group of powder.
And a second component 90W7Ni2.5Fe0.5Co (corresponding figures are the mass percent of each component in the alloy), namely 900g of tungsten powder with the Fisher size of 3.5 mu m, 70g of carbonyl nickel powder, 25g of electrolytic iron powder and 5g of cobalt powder are respectively weighed, mixed and then put into a high-energy ball mill, 2Kg of hard alloy balls are added, ball milling is carried out for 4h under the condition that the rotating speed is 120r/min, 1000g of tungsten alloy powder mixed with trace cobalt elements is obtained, and then the tungsten alloy powder is sieved by a 90-mesh sieve, and undersize powder is used as the second group of powder.
Step two, cold isostatic pressing forming
And (3) completely filling the first group of powder into a mould, compacting, filling the second group of powder into the mould, then placing the mould filled with the raw materials into an oil cylinder, and maintaining the pressure for 10min under the pressure of 180MPa to obtain a molded compact with the relative density of 65%, wherein the size of the molded compact is phi 26 x 353 mm.
Step three, sintering treatment
And (3) putting the molded compact obtained in the second step into a hydrogen sintering furnace for sintering treatment, wherein the highest sintering temperature is 1485 ℃, and the highest temperature is kept for 1h to obtain a sintered compact with the density of 17.62g/cm3 and the size of phi 23 x 301 mm.
Step four, heat treatment after sintering
And (4) putting the sintered blank obtained in the third step into a vacuum sintering furnace for vacuum heat treatment at the temperature of 1100 ℃, and preserving heat for 3 hours to obtain the tungsten alloy bar.
Step five, machining
And machining the tungsten alloy bar in the fourth step to obtain a tungsten alloy final product meeting the actual requirement.
The resulting tungsten alloy final parts were tested according to GB/T228.1-2010 with the performance results shown in Table 1 below (wherein the middle section is the combined front and rear sections); according to application requirements, the front section adopts 93W5Ni1Fe1Co material with higher tensile strength to ensure sufficient strength but relatively low elongation, the rear section adopts 90W7Ni2.5Fe0.5Co, the material has better ductility and higher elongation, the strength of the front section is reduced, the combination part positioned in the middle also has very ideal performance, and the material can effectively improve the penetrating and blasting damage effects of the blasting combat part.
Table 1 example 1 properties of tungsten alloy articles in various sections
Example 2
Step one, preparation of tungsten alloy powder
The first component 95W2Ni1Fe1.5Co0.5Mn (corresponding figures are the mass percent of each component in the alloy), namely 950g of tungsten powder with the Fisher size of 3.5 mu m, 20g of carbonyl nickel powder, 10g of electrolytic iron powder, 15g of cobalt powder and 5g of manganese powder are respectively weighed, mixed and then put into a high-energy ball mill, 2Kg of hard alloy balls are added, ball milling is carried out for 4 hours under the condition that the rotating speed is 120r/min, 1000g of tungsten alloy powder mixed with trace cobalt and manganese elements is obtained, then the tungsten alloy powder is sieved by a 100-mesh sieve, and undersize powder is used as the first group of powder.
A second component 93W5Ni1Fe1Co (corresponding numbers are the mass percent of each component in the alloy): 930g of tungsten powder with the Fisher size of 3.2 mu m, 50g of electrolytic nickel powder, 10g of carbonyl iron powder and 10g of cobalt powder are respectively weighed, mixed and then put into a high-energy ball mill, 2Kg of hard alloy balls are added, ball milling is carried out for 4 hours under the condition that the rotating speed is 120r/min, 1000g of alloy powder mixed with trace cobalt elements is obtained, then the alloy powder is sieved by a 100-mesh sieve, and undersize powder is used as a second group of powder.
Step two, cold isostatic pressing forming
And filling the first group of powder into a mold, compacting, filling the second group of powder into the mold, then placing the mold filled with the raw materials into an oil cylinder, and maintaining the pressure at 180MPa for 10min to obtain a molded compact with the relative density of 63%, wherein the size of the molded compact is phi 25 x 351 mm.
Step three, sintering treatment
And (3) putting the molded compact obtained in the second step into a hydrogen sintering furnace for sintering treatment, wherein the highest sintering temperature is 1485 ℃, the highest temperature heat preservation time is 1h, and the sintered compact is obtained, the density is 17.62g/cm3, and the size is phi 23 x 301.
Step four, heat treatment after sintering
And (4) putting the sintered blank obtained in the third step into a vacuum sintering furnace for vacuum heat treatment at the temperature of 1100 ℃, and preserving heat for 3 hours to obtain the tungsten alloy bar.
Step five, machining
And machining the tungsten alloy bar in the fourth step to obtain a tungsten alloy final product meeting the actual requirement.
The resulting tungsten alloy final parts were tested according to GB/T228.1-2010 with the performance results shown in Table 2 below (wherein the middle section is the combined front and rear sections); according to application requirements, the front section adopts a 95W2Ni1Fe1.5Co0.5Mn material with higher tensile strength to ensure sufficient strength, the elongation rate is lower, and the brittleness is higher, the rear section adopts 93W5Ni1Fe1Co, compared with the 95W2Ni1Fe1.5Co0.5Mn material, 93W5Ni1Fe1Co has better toughness, the strength of the front section is reduced in higher elongation, the combination part positioned in the middle also has very ideal performance, and the material can effectively improve the penetration and blasting damage effects of blasting fighting parts.
Table 2 example 2 properties of tungsten alloy articles in various sections
Example 3
Step one, preparation of tungsten alloy powder
The first component 97W1Ni0.5Fe1Co0.5Mn (corresponding figures are the mass percentage content of each component in the alloy) 970g of tungsten powder with Fisher size of 3.0 mu m, 10g of carbonyl nickel powder, 5g of electrolytic iron powder, 10g of cobalt powder and 5g of manganese powder are respectively weighed, mixed and then put into a high-energy ball mill, 2Kg of hard alloy ball is added, ball milling is carried out for 2h under the condition that the rotating speed is 150r/min, 1000g of tungsten alloy powder mixed with trace cobalt and manganese elements is obtained, and then the powder is sieved by a 140-mesh sieve, so as to obtain the first group of powder.
The second component 95W2Ni1.5Fe1.5Co (the corresponding number is the mass percentage content of each component in the alloy): respectively weighing 950g of tungsten powder with the Fisher particle size of 3.0 mu m, 20g of carbonyl nickel powder, 15g of electrolytic iron powder and 15g of cobalt powder, mixing, putting into a high-energy ball mill, adding 2Kg of hard alloy balls, ball-milling for 2 hours at the rotating speed of 150r/min to obtain 1000g of alloy powder mixed with trace cobalt elements, then sieving by a 120-mesh sieve, and taking undersize products to obtain a second group of powder.
Step two, cold isostatic pressing forming
And filling the first group of powder into a mold, compacting, filling the second group of powder into the mold, then placing the mold filled with the raw materials into an oil cylinder, and maintaining the pressure at 180MPa for 10min to obtain a molded compact with the relative density of 64%, wherein the size of the molded compact is phi 26 multiplied by 354 mm.
Step three, sintering treatment
And (3) putting the molded compact obtained in the second step into a hydrogen sintering furnace for sintering treatment, wherein the sintering highest temperature is 1550 ℃, and the highest temperature heat preservation time is 1h, so that a sintered compact is obtained, the density is 18.23g/cm3, and the size is phi 22 x 298.
Step four, heat treatment after sintering
And (4) putting the sintered blank obtained in the third step into a vacuum sintering furnace for vacuum heat treatment at the temperature of 1150 ℃ for 4 hours to obtain the tungsten alloy material.
Step five, machining
And machining the tungsten alloy material in the fourth step to obtain a tungsten alloy final product meeting the actual requirement.
The resulting tungsten alloy final parts were tested according to GB/T228.1-2010 with the performance results shown in Table 3 below (wherein the middle section is the combined front and rear sections); the front section is made of 97W1Ni0.5Fe1Co0.5Mn which has higher tensile strength but lower elongation rate, belongs to a brittle material, meets the use requirement of actual use on the brittleness of the front section of the material, and the rear section is made of 95W2Ni1.5Fe1.5Co, meets the requirement of better toughness of the rear section. The middle joint part also has ideal performance, and the material can effectively improve the penetration and blasting damage effects of the blasting combat part.
Table 3 example 3 properties of tungsten alloy articles in various sections
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (14)
1. A multifunctional tungsten alloy gradient material is characterized by comprising two material sections according to the direction from one end of the material to the other end, wherein the front section material consists of tungsten and a metal additive, wherein the weight percentage range of the tungsten is 93-98%; the rear section material consists of tungsten and a metal additive, wherein the weight percentage range of the tungsten is 88-93%, and the tungsten content of the front section material is greater than that of the rear section material; in the front-stage material and the back-stage material, the metal additive includes: nickel and iron; the metal additive further comprises cobalt and/or manganese;
in the front-stage material, the content of the metal additive is as follows in percentage by weight: 1-5% of nickel, 1-3% of iron, 0-4% of cobalt and 0-0.5% of manganese;
in the back-end material, the content of the metal additive is as follows in percentage by weight: 1-8% of nickel, 1-3% of iron, 0-4% of cobalt and 0-0.5% of manganese.
2. The multi-functional tungsten alloy gradient material of claim 1, wherein the metal additive further comprises molybdenum.
3. The multi-functional tungsten alloy gradient material of claim 1, wherein in the front-stage material, by weight, cobalt is 0.5-3% and manganese is 0.02-0.5%.
4. The multi-functional tungsten alloy gradient material of claim 1, wherein in the back-end material, by weight, cobalt is 0.5-3%, and manganese is 0.02-0.5%.
5. The multi-functional tungsten alloy gradient material of claim 1,
the front section material comprises the following components in percentage by weight: the rear-section material comprises the following components of W93%, Ni 5%, Fe 1% and Co 1%: 90% of W, 7% of Ni, 2.5% of Fe and 0.5% of Co; alternatively, the front-end material is composed of the following components: the rear section material comprises 95% of W, 2% of Ni, 1% of Fe, 1.5% of Co and 0.5% of Mn, and comprises the following components: 93% of W, 5% of Ni, 1% of Fe and 1% of Co; alternatively, the front-end material is composed of the following components: the rear section material comprises 97% of W, 1% of Ni, 0.5% of Fe, 1% of Co and 0.5% of Mn, and comprises the following components: 95% of W, 2% of Ni, 1.5% of Fe and 1.5% of Co.
6. The preparation method of the multifunctional tungsten alloy gradient material is characterized by comprising the following steps of:
the preparation method of the tungsten alloy powder comprises the following steps: weighing the components and the weight ratio of the front-section material and the rear-section material in the multifunctional tungsten alloy gradient material according to any one of claims 1 to 5, respectively mixing the raw materials of the front-section material and the rear-section material, performing ball milling, and sieving to obtain tungsten alloy powder of the front-section material and tungsten alloy powder of the rear-section material;
a step of press forming: according to the design sequence of the front section material and the rear section material, sequentially filling the tungsten alloy powder of the front section material and the tungsten alloy powder of the rear section material into a die, and then performing compression molding to obtain a pressed blank;
sintering: sintering the pressed blank to obtain a tungsten alloy sintered blank;
a heat treatment step: and carrying out heat treatment on the tungsten alloy sintered blank to obtain the tungsten alloy material.
7. The method for preparing the multifunctional tungsten alloy gradient material according to claim 6, further comprising a machining step, wherein the machining step is as follows: and machining the tungsten alloy material to obtain a tungsten alloy final product.
8. The method for preparing a multifunctional tungsten alloy gradient material according to claim 6, wherein in the step of preparing the tungsten alloy powder, the Fisher size of the tungsten powder in the raw material is 2.0-4.0 μm, the nickel powder in the raw material is electrolytic nickel powder or carbonyl nickel powder, and the iron powder in the raw material is electrolytic iron powder or carbonyl iron powder.
9. The preparation method of the multifunctional tungsten alloy gradient material as claimed in claim 6, wherein the ball milling time is 2-8 hours, the rotation speed of the ball milling is 100-500 r/min, and the ball-to-material ratio of the ball milling is 2:1-3: 1.
10. The preparation method of the multifunctional tungsten alloy gradient material as claimed in claim 6, wherein the sieving is 80-140 mesh sieving.
11. The method for preparing the multifunctional tungsten alloy gradient material according to claim 6, wherein in the step of compression molding, the compression molding is cold isostatic pressing, the pressure of the cold isostatic pressing is 180-250 MPa, and the dwell time is 5-15 min.
12. The method for preparing the multifunctional tungsten alloy gradient material according to claim 6, wherein in the sintering step, the sintering is performed in a hydrogen atmosphere.
13. The method for preparing the multifunctional tungsten alloy gradient material according to claim 6, wherein in the sintering step, the sintering temperature is 1300-1550 ℃, and the sintering time is 0.5-4 h.
14. The method for preparing the multifunctional tungsten alloy gradient material according to claim 6, wherein in the heat treatment step, the heat treatment is performed under vacuum, the temperature of the heat treatment is 905-1200 ℃, and the time of the heat treatment is 1-8 h.
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