CN115109977A - Ultra-large-specification high-performance tungsten alloy pipe and preparation method thereof - Google Patents
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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Abstract
The invention discloses an ultra-large specification high-performance tungsten alloy pipe and a preparation method thereof, wherein the tungsten alloy pipe is prepared by the following steps: mixing 89-95% of tungsten and 5-11% of heavy metal mixed material by weight percentage, and sieving to prepare tungsten alloy powder, wherein the heavy metal mixed material is more than two of nickel, cobalt, manganese and iron, the cobalt is less than or equal to 4%, and the manganese is less than or equal to 0.5%; pressing and molding the tungsten alloy powder by a cold isostatic pressing process to obtain a tubular pressed compact; removing the cold isostatic pressing forming tool, and performing surface shaping on the tubular pressed blank; placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace for sintering to obtain a tungsten alloy pre-sintered blank; and carrying out rotary sintering on the tungsten alloy pre-sintered blank to obtain a tungsten alloy pipe sintered blank. The preparation process is simpler, and is more suitable for preparing tungsten alloy thin-wall parts with ultra-large specifications, the prepared large-size tungsten alloy pipe product has good comprehensive mechanical properties, the yield of the large-size tungsten alloy pipe product is greatly improved, and the requirements of the military and civil engineering fields are met.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to an ultra-large-specification high-performance tungsten alloy pipe and a preparation method thereof.
Background
The tungsten alloy has small thermal expansion coefficient, good corrosion resistance and excellent ray shielding function, and is widely applied to the fields of national defense, civil use and advanced science. In recent years, with the development of military and civil industries, the requirements on the application range and comprehensive performance of materials in related fields are continuously expanded and improved, and especially in the fields of high-end nuclear power, large-scale assembly and military backup defense and defense, the requirements on the use of meeting different application scenes and matching various sizes and shapes (especially large-size pipe assemblies) are always the focus and difficult problems in the field of materials on the premise of ensuring the performance. The tungsten alloy is generally a two-phase alloy, and compared with single-phase metal, the tungsten alloy has the characteristics of high strength and good ductility, is more favorable for processing and deformation, and provides more possibilities for meeting multi-demand applications. However, in the current preparation process of large-size tungsten alloy products, a common problem is that the tungsten alloy pressed compact is heated unevenly due to an overlarge volume in the sintering process, and the phenomena of uneven shrinkage, deformation, cracking and the like are generated, so that the density is unqualified or finished products cannot be prepared.
Therefore, the exploration and research on the preparation of the large-size high-performance tungsten alloy pipe not only meet the current use requirement, but also provide reference for the development and application prospect of similar products in the future.
Disclosure of Invention
The invention aims to provide an oversized high-performance tungsten alloy pipe and a preparation method thereof.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows: an oversized high-performance tungsten alloy pipe comprises the following raw material components in percentage by mass: 89-95% of tungsten and 5-11% of heavy metal mixed material, wherein the heavy metal mixed material is more than any two of nickel, cobalt, manganese and iron, wherein the cobalt content is less than or equal to 4%, and the manganese content is less than or equal to 0.5%.
The invention also provides a preparation method of the ultra-large specification high-performance tungsten alloy pipe, which comprises the following steps:
s1, preparing tungsten alloy powder: the tungsten alloy powder is obtained by sieving the following mixed powder in percentage by weight: 89-95% of tungsten and 5-11% of heavy metal mixed material, wherein the heavy metal mixed material is more than any two of nickel, cobalt, manganese and iron, the cobalt content is less than or equal to 4%, and the manganese content is less than or equal to 0.5%;
s2, press forming: pressing and forming the tungsten alloy powder obtained in the step S1 through a cold isostatic pressing process to obtain a tubular pressed compact;
s3, shaping: removing the cold isostatic pressing forming tool, and performing surface shaping on the tubular pressed blank;
s4, pre-sintering: placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace for sintering to obtain a tungsten alloy pre-sintered blank;
s5, rotary sintering: carrying out rotary sintering on the tungsten alloy pre-sintered blank to obtain a tungsten alloy pipe sintered blank;
s6, vacuum heat treatment: carrying out heat treatment on the tungsten alloy pipe blank in a vacuum environment;
s7, machining: and (3) machining the tungsten alloy pipe subjected to vacuum heat treatment to obtain the tungsten alloy pipe product with the ultra-large specification meeting the size requirement.
Further, in step S1, the tungsten powder, the cobalt powder, and the manganese powder in the mixed powder are all conventional industrial powders, and the particle size of the tungsten powder is 2.0-4.0 μm, the nickel powder is electrolytic nickel powder or carbonyl nickel powder, and the iron powder is electrolytic iron powder or carbonyl iron powder.
Further, the mixed powder is mixed for 4-8 hours at a rotating speed of 100-300 r/min.
Furthermore, the screening mesh number of the mixed powder is 80-140 meshes.
Further, in step S2, the cold isostatic pressing process conditions are: the pressure is 180-250 Mpa, and the pressure maintaining time is 30-120 min.
Further, in step S3, the surface shaping includes shaping processing of thickness uniformity, surface flatness, and spatial dimension symmetry of the tubular green compact.
Further, in step S4, hydrogen is used as the atmosphere in the pre-sintering furnace, and the pre-sintering conditions are as follows: the sintering temperature is 1200-1350 ℃, and the heat preservation time is 2-4 h.
Further, in the step S5, the tungsten alloy pre-sintered blank is placed in a rotary sintering furnace for sintering, hydrogen is used as a sintering atmosphere, the rotary sintering temperature is 1300-1500 ℃, and the heat preservation time is 2-6 hours.
Further, in step S6, the tungsten alloy tube blank is sintered under the vacuum degree of 10 -1 And (3) carrying out heat treatment under a vacuum environment below Pa, wherein the heat treatment temperature is 1100-1200 ℃, and the heat treatment time is 3-6 h.
Compared with the prior art, the invention has the following beneficial effects:
1) compared with the preparation process of a large-size tungsten alloy product subjected to splicing treatment after sectional processing in the prior art, the preparation process is simpler and is more suitable for preparing the tungsten alloy thin-walled part with the ultra-large specification, and the prepared large-size tungsten alloy pipe product has good comprehensive mechanical property, so that the yield of the large-size tungsten alloy pipe product is greatly improved, and the requirements of the military and civil engineering fields are met;
2) according to the preparation method of the ultra-large high-performance tungsten alloy pipe, the second step sintering method in the used step sintering method is a rotary sintering method, so that the states of all parts of the blank in the sintering process are kept as consistent as possible and tend to be uniform, uniform shrinkage of all parts in the sintering process is facilitated, and the problems of uneven density, cracking and the like caused by nonuniform shrinkage are avoided to a certain extent.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a metallographic structure diagram of a tungsten alloy material prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples. The following examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. The experimental procedures used in the following examples are conventional procedures unless otherwise specified, and the reagents and procedures used therein are conventional in the art unless otherwise specified.
The tungsten alloy tube with the outer diameter larger than 350mm, the height larger than 500mm and the weight more than 500 kg is set as the ultra-large tungsten alloy tube, and the preparation method of the ultra-large tungsten alloy tube is explained by the specific embodiment.
Example 1
Step one, preparing tungsten alloy powder
The material design component is 90W7Ni2.5Fe0.5Co, namely the material comprises the following raw material components in percentage by mass: 90 percent of tungsten, 7 percent of nickel, 2.5 percent of iron and 0.5 percent of cobalt, specifically 500.44Kg of tungsten powder with the Fisher's particle size of 2 mu m, 38.9Kg of electrolytic nickel powder, 13.9Kg of electrolytic iron powder and 2.76Kg of cobalt powder are respectively weighed, a three-dimensional mixer is used for mixing materials at the rotating speed of 120r/min for 4 hours to obtain 556Kg of tungsten alloy powder mixed with trace cobalt element, and then the tungsten alloy powder is sieved by a 90-mesh sieve to collect undersize powder, namely the tungsten alloy powder;
step two, cold isostatic pressing forming
Filling the tungsten alloy powder into a die with a die core, compacting, placing the die filled with the tungsten alloy powder into an oil cylinder, and maintaining the pressure at 180MPa for 30min to obtain a formed pipe with the relative density of 65%, wherein the formed pipe has the outer diameter of 65%Inner diameterA tubular green compact having a length of 600 mm;
step three, shaping treatment
After cold isostatic pressing, removing tools such as a die, shaping the excircle and the two sections in the length direction of the tubular pressed blank, and ensuring that the excircle surface of the blank is round, the two ends of the blank are flat in length and uniform in thickness so as to facilitate uniform shrinkage in the subsequent sintering process;
step four, presintering treatment
Placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace, sintering at 1260 ℃ in a hydrogen atmosphere, and keeping the temperature for 2 hours to obtain a tungsten alloy pre-sintered blank;
step five, secondary rotary sintering
Placing the tungsten alloy pre-sintered blank into a rotary sintering furnace, wherein the sintering atmosphere is hydrogen, the maximum sintering temperature is 1350 ℃, the maximum temperature heat preservation time is 3 hours, and obtaining a tungsten alloy pipe sintered blank with the density of 17.02g/cm 3 Size is outer diameterInner diameterThe length is 510 mm;
step six, vacuum heat treatment
Carrying out vacuum heat treatment on the tungsten alloy pipe blank with the vacuum degree of 10 -2 Pa, the heat treatment temperature is 1100 ℃, and the heat preservation time is 3 hours;
step seven, machining
And machining the tungsten alloy pipe subjected to the vacuum heat treatment to obtain a tungsten alloy pipe product meeting the actual requirement.
Example 2
Step one, preparing tungsten alloy powder
The material design component is 95W2Ni1Fe1.5Co0.5Mn, namely the material comprises the following raw material components in percentage by mass: 95 percent of tungsten, 2 percent of nickel, 1 percent of iron, 1.5 percent of cobalt and 0.5 percent of manganese, specifically 1056.1Kg of tungsten powder with the Fisher size of 3.2 mu m, 22.23Kg of nickel carbonyl powder, 11.12Kg of iron carbonyl powder, 16.67Kg of cobalt powder and 5.56Kg of manganese powder are respectively weighed, a three-dimensional mixer is used for mixing materials at the rotating speed of 150r/min for 6h to obtain 1111.68Kg of tungsten alloy powder mixed with trace cobalt and manganese elements, and then the tungsten alloy powder passes through a 120-mesh sieve to collect undersize powder, namely the tungsten alloy powder;
step two, cold isostatic pressing forming
Filling the tungsten alloy powder into a die with a die core, compacting, placing the die filled with the tungsten alloy powder into an oil cylinder, and maintaining the pressure at 180MPa for 30min to obtain a formed pipe with the relative density of 65%, wherein the formed pipe has the outer diameter of 65%Inner diameterA tubular green compact having a length of 718 mm;
step three, shaping treatment
After cold isostatic pressing, removing tools such as a die, shaping the excircle and two sections in the length direction of the tubular pressed blank, and ensuring that the excircle surface of the blank is round, the two ends of the blank are flat in length and uniform in thickness, so that the blank can be uniformly contracted in the subsequent sintering process;
step four, presintering treatment
Placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace, sintering at 1350 ℃ in a hydrogen atmosphere, and keeping the temperature for 2 hours to obtain a tungsten alloy pre-sintered blank;
step five, secondary rotary sintering
Putting the tungsten alloy pre-sintered blank into a rotary sintering furnace, wherein the sintering atmosphere is hydrogen, the highest sintering temperature is 1485 ℃, and the highest temperature heat preservation time is 4.5h to obtain a tungsten alloy pipe sintered blank with the density of 18.02g/cm 3 Size is outer diameterInner diameterThe length is 612 mm;
step six, vacuum heat treatment
Carrying out vacuum heat treatment on the tungsten alloy pipe blank with the vacuum degree of 10 -1 Pa, the heat treatment temperature is 1200 ℃, and the heat preservation time is 3.5 hours;
step seven, machining
And machining the tungsten alloy pipe subjected to vacuum heat treatment to obtain a tungsten alloy pipe product meeting the actual requirement.
Example 3
Step one, preparing tungsten alloy powder
The material design component is 93W5Ni1.5Fe0.5Mn, namely the material comprises the following raw material components in percentage by mass: 93 percent of tungsten, 5 percent of nickel, 1.5 percent of iron and 0.5 percent of manganese, specifically 3205.2Kg of tungsten powder with Fisher's particle size of 3.0 mu m, 172.32Kg of nickel carbonyl powder, 51.7Kg of electrolytic iron powder and 17.2Kg of manganese powder are respectively weighed, a three-dimensional mixer is used for mixing materials at the rotating speed of 200r/min for 8 hours to obtain 3446.42Kg of tungsten alloy powder mixed with trace manganese element, and then the tungsten alloy powder is sieved by a 100-mesh sieve to collect undersize powder, namely the tungsten alloy powder.
Step two, cold isostatic pressing forming
Filling the tungsten alloy powder into a die with a die core, compacting, placing the die filled with the tungsten alloy powder into an oil cylinder, and pressing at 220MPaMaintaining the pressure for 60min under the action of force to obtain a molded circular ring blank with the relative density of 64 percent, wherein the molded circular ring blank has an outer diameterInner diameterA tubular compact of length 1188 mm.
Step three, shaping treatment
After cold isostatic pressing, removing tools such as a die, shaping the excircle and the two sections in the length direction of the tubular pressed blank, and ensuring that the excircle surface of the blank is round, the two ends of the blank are flat in length and uniform in thickness so as to facilitate uniform shrinkage in the subsequent sintering process;
step four, presintering treatment
Placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace, and sintering in a hydrogen atmosphere at the sintering temperature of 1300 ℃ for 3.5 hours to obtain a tungsten alloy pre-sintered blank;
step five, secondary rotary sintering
Putting the tungsten alloy and the sintered blank in the steps into a rotary sintering furnace, wherein the sintering atmosphere is hydrogen, the highest sintering temperature is 1440 ℃, the highest temperature heat preservation time is 5h, and the sintered blank of the tungsten alloy tube with the density of 17.63g/cm is obtained 3 Size is outer diameterInner diameterThe length is 1010 mm;
step six, vacuum heat treatment
Carrying out vacuum heat treatment on the tungsten alloy pipe blank with the vacuum degree of 5 multiplied by 10 -2 Pa, the heat treatment temperature is 1200 ℃, and the heat preservation time is 4 hours.
Step seven, machining
And machining the tungsten alloy pipe subjected to the vacuum heat treatment to obtain a tungsten alloy pipe product meeting the actual requirement.
Example 4
Step one, preparation of tungsten alloy powder
The material design component is 93W5Ni2Fe, namely the material comprises the following raw material components in percentage by mass: 93 percent of tungsten, 5 percent of nickel and 2 percent of iron, specifically, 4665.1Kg of tungsten powder with Fisher's particle size of 4 mu m, 250.9Kg of nickel carbonyl powder and 100.33Kg of electrolytic iron powder are respectively weighed, a three-dimensional mixer is used for mixing materials at the rotating speed of 300r/min for 8 hours to obtain 5016.33Kg of tungsten alloy powder mixed with trace manganese element, and then the tungsten alloy powder is sieved by a 140-mesh sieve to collect undersize powder, namely the tungsten alloy powder.
Step two, cold isostatic pressing forming
Filling the tungsten alloy powder into a die with a die core, compacting, placing the die filled with the tungsten alloy powder into an oil cylinder, maintaining the pressure at 235MPa for 120min to obtain a formed ring blank with the relative density of 65%, wherein the formed ring blank has the outer diameterInner diameterA tubular compact of length 1188 mm.
Step three, shaping treatment
After cold isostatic pressing, removing tools such as a die, shaping the excircle and the two sections in the length direction of the tubular pressed blank, and ensuring that the excircle surface of the blank is round, the two ends of the blank are flat in length and uniform in thickness so as to facilitate uniform shrinkage in the subsequent sintering process;
step four, presintering treatment
Placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace, and sintering at 1320 ℃ in a hydrogen atmosphere for 4 hours to obtain a tungsten alloy pre-sintered blank;
step five, secondary rotary sintering
Placing the tungsten alloy pre-sintered blank into a rotary sintering furnace, wherein the sintering atmosphere is hydrogen, the maximum sintering temperature is 1450 ℃, the maximum temperature heat preservation time is 6 hours, and obtaining a tungsten alloy pipe sintered blank, and the tungsten alloy pipe sintered blank is denseThe degree is 17.65g/cm 3 Size is outer diameterInner diameterThe length is 1010 mm;
step six, vacuum heat treatment
Carrying out vacuum heat treatment on the tungsten alloy pipe blank with the vacuum degree of 8 multiplied by 10 -3 Pa, the heat treatment temperature is 1200 ℃, and the heat preservation time is 5 hours.
Step seven, machining
And machining the tungsten alloy pipe subjected to vacuum heat treatment to obtain a tungsten alloy pipe product meeting the actual requirement.
Example 5
The difference between the present embodiment and embodiment 1 is that cobalt powder is not added in the tungsten alloy powder preparation process of step one, the vacuum heat treatment time is 5 hours, and the specific process parameters are shown in table 1;
example 6
The difference between the embodiment and the embodiment 3 is that manganese powder is not added in the tungsten alloy powder preparation process in the step one, the vacuum heat treatment time is 6 hours, and the specific process parameters are shown in table 1;
the physical sampling mechanical properties of the tungsten alloy pipe products prepared in the examples 5 and 6 are shown in the table 2;
table 1 process parameters of tungsten alloy tube articles prepared in examples 5 and 6
TABLE 2 Performance parameters of tungsten alloy tubing articles prepared in examples 1-6
As can be seen from the results in Table 2, the tungsten alloy pipe product prepared by the method of the invention has high density and excellent mechanical properties; the preparation method provided by the invention is simple in process, is suitable for industrial mass production, and can greatly improve the yield of large-size tungsten alloy pipe products.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (10)
1. The ultra-large high-performance tungsten alloy pipe is characterized by comprising the following raw materials in percentage by mass: 89-95% of tungsten and 5-11% of heavy metal mixed material, wherein the heavy metal mixed material is more than any two of nickel, cobalt, manganese and iron, wherein the cobalt content is less than or equal to 4%, and the manganese content is less than or equal to 0.5%.
2. A preparation method of an ultra-large-specification high-performance tungsten alloy pipe is characterized by comprising the following steps:
s1, preparing tungsten alloy powder: the tungsten alloy powder is obtained by sieving the following mixed powder in percentage by weight: 89-95% of tungsten and 5-11% of heavy metal mixed material, wherein the heavy metal mixed material is more than any two of nickel, cobalt, manganese and iron, the cobalt content is less than or equal to 4%, and the manganese content is less than or equal to 0.5%;
s2, press forming: pressing and molding the tungsten alloy powder obtained in the step S1 through a cold isostatic pressing process to obtain a tubular pressed compact;
s3, shaping: removing the cold isostatic pressing forming tool, and performing surface shaping on the tubular pressed blank;
s4, pre-sintering: placing the shaped tubular pressed blank into a fixed-point atmosphere pre-sintering furnace for sintering to obtain a tungsten alloy pre-sintered blank;
s5, rotary sintering: carrying out rotary sintering on the tungsten alloy pre-sintered blank to obtain a tungsten alloy pipe sintered blank;
s6, vacuum heat treatment: carrying out heat treatment on the tungsten alloy pipe blank in a vacuum environment;
s7, machining: and (3) machining the tungsten alloy pipe subjected to vacuum heat treatment to obtain the tungsten alloy pipe product with the ultra-large specification meeting the size requirement.
3. The method of claim 2, wherein: in step S1, the tungsten powder, the cobalt powder, and the manganese powder in the mixed powder are all conventional industrial powders, the particle size of the tungsten powder is 2.0 to 4.0 μm, the nickel powder is electrolytic nickel powder or carbonyl nickel powder, and the iron powder is electrolytic iron powder or carbonyl iron powder.
4. The method of claim 2, wherein: the mixed powder is mixed for 4-8 h at a rotating speed of 100-300 r/min.
5. The method of claim 2, wherein: the screening mesh number of the mixed powder is 80-140 meshes.
6. The method of claim 2, wherein: in step S2, the cold isostatic pressing process conditions are: the pressure is 180-250 Mpa, and the pressure maintaining time is 30-120 min.
7. The method of claim 2, wherein: in step S3, the surface shaping includes shaping processing of thickness uniformity, surface flatness, and spatial dimension symmetry of the tubular green compact.
8. The production method according to claim 2, characterized in that: in step S4, hydrogen is used as the atmosphere in the pre-sintering furnace, and the pre-sintering conditions are as follows: the sintering temperature is 1200-1350 ℃, and the heat preservation time is 2-4 h.
9. The method of claim 2, wherein: in the step S5, the tungsten alloy pre-sintered blank is placed in a rotary sintering furnace for sintering, hydrogen is used as a sintering atmosphere, the rotary sintering temperature is 1300-1500 ℃, and the heat preservation time is 2-6 h.
10. The method of claim 2, wherein: in step S6, the tungsten alloy tube is sintered at the vacuum degree of 10 -1 And (3) carrying out heat treatment in a vacuum environment below Pa, wherein the heat treatment temperature is 1100-1200 ℃, and the heat treatment time is 3-6 h.
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CN110129645A (en) * | 2019-05-24 | 2019-08-16 | 安泰科技股份有限公司 | A kind of multi-functional tungsten alloy functionally gradient material (FGM) and preparation method thereof |
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