CN113444904A - Preparation method of tungsten-based high-specific gravity alloy material - Google Patents
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Abstract
The invention provides a preparation method of a tungsten-based high-specific gravity alloy material, which comprises the steps of screening binary or multi-component alloy powder formed by single-component tungsten powder and other metal elements, cold isostatic pressing, sintering, forging, annealing, machining, cleaning and the like to prepare the tungsten-based high-specific gravity alloy material.
Description
Technical Field
The invention belongs to the technical field of refractory metal processing, and particularly relates to a preparation method of a tungsten-based high-specific gravity alloy material.
Background
Tungsten-based alloys, which are generally called high-specific-gravity alloys, heavy alloys or high-density alloys, have a series of excellent properties such as high strength, high hardness, good ductility, good toughness, good machinability, small thermal expansion coefficient, good corrosion resistance and oxidation resistance, good electrical and thermal conductivity, good weldability and the like, and are widely used in the field of advanced science, the national defense industry and the civil industry. For example, it is proved by a large amount of data that the tungsten-based high-specific-gravity alloy is the field with the largest tungsten amount for external use except for hard alloy, tungsten-containing steel and tungsten filament, and the like, and is used as a counterweight and a damping material on a gyro rotor and an airplane, as a armor piercing bullet and a shrapnel in the military industry, and the like, and is used as a high-specific-gravity alloy vibrator on a BB machine in the civil industry, an electric upsetting anvil block, an electrode material and the like.
At present, the tungsten-based high-specific gravity alloy industry mostly adopts complex multi-element alloying of a binding phase to improve the alloy performance. However, the process for preparing the binder phase powder by smelting, alloying and spraying is very complicated, and the addition of the multi-component powder to form the binder phase can achieve a certain strengthening effect, but along with the solid solution of tungsten and the binder phase, a series of disadvantages such as reduction of tungsten content and growth of hard phase grains are caused, which are not favorable for preparing the high-performance tungsten-based high-specific gravity alloy. Therefore, the development of a tungsten-based high-specific gravity alloy material with good mechanical property, small thermal expansion coefficient and good electric and thermal conductivity becomes the key for currently promoting the development of the military industry and the aerospace industry in China.
Disclosure of Invention
Aiming at overcoming the defect that the prior bonding phase method for preparing the high-temperature alloy can not keep the ideal strengthening effect
The invention provides a preparation method of a tungsten-based high-specific gravity alloy material, which is used for preparing a high-performance tungsten-based high-specific gravity alloy material with the actual density close to or equal to the theoretical density of the alloy, and the average grain size less than or equal to 50um, high strength, high hardness, good ductility, good toughness, good machinability, small thermal expansion coefficient, good corrosion resistance and oxidation resistance, good electric and thermal conductivity and good weldability.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a tungsten-based high specific gravity alloy material comprises the following preparation steps:
selecting multi-element alloy powder consisting of tungsten powder and other metal powder as a raw material of a tungsten-based high-specific gravity alloy material, and sieving the multi-element alloy powder for later use;
secondly, putting the alloy powder selected in the step one into a die, and preparing a powdery rod blank or a plate blank through cold isostatic pressing;
step three, putting the powdery rod blank or the plate blank into a sintering furnace, and sintering in a hydrogen or vacuum environment to obtain a sintered blank with the density of more than 98 percent for later use;
step four, heating the sintered blank at the temperature of 1000-1600 ℃ for 60-120 min, and then forging the sintered blank by matching with a corresponding die to prepare a forged blank for later use;
step five, annealing the forged blank obtained in the step four at the annealing temperature of 1000-1350 ℃ for 1-12 h, and cooling for later use;
step six, machining the blank processed in the step five to a target required size, and then carrying out defect detection and crystal scanning detection;
step seven, washing the qualified product subjected to nondestructive inspection in the step six by using clean water, drying and then carrying out vacuum packaging to obtain a finished product;
further, the grain diameter of the alloy powder screened in the first step is 160-500 meshes.
Further, other metal powders in step one include, but are not limited to, Ni, Cu, Fe, Co, Mo, and Cr.
Furthermore, the multi-element alloy powder in the first step is composed of any one of tungsten powder and other metal powder.
Further, the multi-element alloy powder in the step one is composed of any two or more of tungsten powder and other metal powder.
Further, in the first step, the mass part of the tungsten powder is 85-99%, and the mass part of the other metal powder is 1-15%.
Further, the mould in the second step is a flexible mould, the pressing pressure of cold isostatic pressing is 150-300 MPa, and the pressure maintaining time is 10-60 min.
Furthermore, in the third step, the sintering temperature is 1000-2450 ℃, and the sintering time is 4-72 hours.
Further, in the fifth step, the annealing temperature is 1000-1350 ℃, and the annealing heat preservation time is 1-12 hours.
Furthermore, in the sixth step, water immersion type ultrasonic C scanning is used, no pore defect with the average diameter larger than 0.3mm exists in the machined tube blank, the wave intensity of the bottom surface of crystal scanning is not smaller than 80%, and the average grain diameter is smaller than 35 um.
The invention has the beneficial effects that: the invention adopts a vacuum stirring and mixing process and a powder metallurgy method, and prepares the tungsten-based high-specific gravity alloy with the actual density close to or equal to the theoretical density of the alloy and the average grain size less than or equal to 50um through a hydrogen protective atmosphere sintering or vacuum sintering process, and the tungsten-based high-specific gravity alloy has the advantages of high strength, high hardness, good ductility, good toughness, good machinability, small thermal expansion coefficient, good corrosion resistance, good oxidation resistance, good electric and thermal conductivity and good weldability, overcomes a series of problems of uncontrollable tungsten content, large material brittleness and the like in the traditional process, and lays a solid practical foundation for the preparation of the high-performance tungsten-based high-specific gravity alloy and the rapid development of the military industry and the aerospace industry.
Detailed Description
The embodiments of the present invention are described in detail with reference to specific embodiments, and the embodiments and specific operations are provided in the present embodiment on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following embodiments.
A preparation method of a tungsten-based high specific gravity alloy material comprises the following preparation steps:
the method comprises the following steps of firstly, selecting raw materials prepared from a tungsten-based high-specific gravity alloy material, wherein the raw materials comprise the following two materials: a. an alloy element composed of any one of tungsten powder and metal powder; b. tungsten powder and an alloy powder composed of any two or more of the metal powders. For example, an alloy powder composed of tungsten powder and nickel powder alone, or a multi-component composition composed of tungsten powder, nickel powder and copper powderAnd (3) gold powder. Particularly, the components defined in a and b are that the tungsten powder content is 85-99% and the other metal elements content is 1-15% according to the mass fraction, namely the density of the tungsten-based high specific gravity alloy is controlled to be more than or equal to 16.5g/cm3. Meanwhile, the metal powder includes, but is not limited to, Ni, Cu, Fe, Co, Mo, Cr, and the like. When the selected powder raw materials are screened, a screen is selected to be 160-500 meshes, oversize materials are treated as waste materials, and undersize powder is reserved; before and after use, whether the screen is damaged or not is checked to ensure that sundries or large powder aggregates are screened out; firstly, primarily mixing multi-component alloy powder in a sieving and mixing mode before mixing, and then uniformly stirring the multi-component alloy powder in a vacuum stirrer;
step two, putting the powder raw material selected in the step one into a flexible die, and adjusting the pressure of cold isostatic pressing to be 150-300 MPa and the pressure maintaining time to be 10-60 min, wherein the specific execution process is adjusted within a range according to the specification of the prepared tungsten-based high-specific gravity alloy and the technical indexes of the selected powder; cold isostatic pressing is used for automatically boosting the pressure of equipment, the boosting speed is not limited, and powder alloy blanks are prepared by the cold isostatic pressing process;
step three, putting the powder blank into a sintering furnace, and sintering the powder blank in a hydrogen or vacuum environment to obtain a sintered blank with the density of more than 98%, wherein the sintering temperature is 1050-2100 ℃, and the sintering time is 6-72 hours;
and step four, heating the sintered blank in a muffle furnace at the temperature of 1000-1600 ℃, specifically selecting the sintered blank according to the designed material and the forging deformation of the product, heating for 60-120 min, selecting the specification of a die as the target size requirement, and forging and processing the sintered blank according to the designed forging die to obtain a forged blank.
Step five, annealing the forged blank at the annealing temperature of 1000-1350 ℃ for 1-12 h to optimize the metallographic structure of the forged blank, refine crystal grains, promote the processed structure to change to a recovery structure, enable the metallographic structure in the blank to tend to a stable state, further improve the comprehensive mechanical property and then cool for later use;
and step six, machining the blank subjected to heat treatment to a target required size, scanning by using water immersion type ultrasonic C, wherein no pore defect with the average diameter larger than 0.3mm exists in the machined alloy material, the intensity of the bottom surface wave of crystal scanning is not smaller than 80%, and the average grain diameter is smaller than 35 um. The water immersion type ultrasonic C scanning is divided into two times, different models are respectively selected to detect physical defects and grain structure uniformity, and the detection result is expressed by color difference of color pictures;
and seventhly, washing the machined alloy with clean water, drying and then carrying out vacuum packaging to obtain the tungsten-based high-specific gravity alloy material.
Example 1
A preparation method of a tungsten-based high specific gravity alloy material comprises the following steps:
selecting tungsten powder and nickel powder, wherein the Fisher size of the tungsten powder and the nickel powder is 3.0 mu m, the tungsten powder and the nickel powder in batches need to be sampled and analyzed, various physical and chemical performance indexes meet application requirements, screening the tungsten powder and the nickel powder by using a 500-mesh screen, treating oversize materials as waste materials, and reserving the tungsten powder and the nickel powder under the screen, wherein the mixing ratio of the tungsten powder to the nickel powder is as follows according to the mass fraction: 90 percent and 10 percent, and stirring the tungsten powder and the nickel powder by adopting a composite stirring mode of sieving stirring and vacuum stirring;
selecting a flexible rubber mold with the specification of 40 multiplied by 100 multiplied by 200mm, cleaning the interior of the flexible rubber mold, uniformly adding molybdenum-nickel alloy mixed powder, and filling the powder with the weight of 15 kg; after sealing, cold isostatic pressing is carried out, the pressing pressure is 165MPa, and the pressure maintaining time is 20 min; demolding for later use after pressing is finished;
step three, putting the powder blank into a medium-frequency induction sintering furnace, introducing hydrogen as a protective and reducing atmosphere, sintering at 1450 ℃ for 48h, cooling along with the furnace, discharging, and measuring the sintering density to be 16.73g/cm3；
Step four, placing the sintered blank in a muffle furnace with a hydrogen protective atmosphere for heating, wherein the heating temperature is 1320 ℃, the heat preservation time is 60min, and performing free forging processing on the alloy blank;
step five, carrying out recrystallization annealing at 1200 ℃ by using an annealing furnace, preserving heat for 2 hours, and naturally cooling;
sixthly, machining the tungsten-nickel alloy subjected to heat treatment to the size required by a customer drawing by using a machine, and then carrying out defect flaw detection to detect whether the inside of the alloy material has defects such as cracks, pores and the like, wherein the inside of the tungsten-nickel alloy does not have pore defects with the average diameter larger than 0.3 mm;
seventhly, washing the machined alloy with clean water, drying and then carrying out vacuum packaging to obtain the alloy with the density of 17.20g/cm3High performance tungsten-nickel high specific gravity alloys with an average grain size of 41 um.
Example 2
A preparation method of a tungsten-based high specific gravity alloy material comprises the following steps:
selecting tungsten powder and molybdenum powder, wherein the Fisher-Tropsch particle size of the tungsten powder and the molybdenum powder is 3.2 mu m, the tungsten powder and the molybdenum powder in batches need to be sampled and analyzed, various physical and chemical performance indexes meet application requirements, screening the tungsten powder and the molybdenum powder by using a 500-mesh screen, performing waste treatment on oversize products, and taking the tungsten powder and the molybdenum powder below the screen for later use, wherein the mixing ratio of the tungsten powder to the molybdenum powder is respectively as follows according to mass fractions: 85% and 15%, and stirring the tungsten powder and the molybdenum powder by adopting a composite stirring mode of sieving stirring and vacuum stirring;
selecting a flexible rubber mold with the specification of 50 multiplied by 200 multiplied by 400mm, cleaning the interior of the flexible rubber mold, uniformly adding tungsten-molybdenum alloy mixed powder, and filling the powder with the weight of 70 kg; after sealing, cold isostatic pressing is carried out, the pressing pressure is 185MPa, and the pressure maintaining time is 30 min; demolding for later use after pressing is finished;
step three, putting the powder blank into a medium-frequency induction sintering furnace, introducing hydrogen as a protective and reducing atmosphere, sintering at the temperature of 2050 ℃ for 72 hours, cooling along with the furnace, discharging, and measuring the sintering density to be 16.65g/cm3；
Fourthly, heating the sintered blank in a muffle furnace with a hydrogen protective atmosphere at 1550 ℃, keeping the temperature for 60min, and carrying out free forging processing on the alloy blank;
step five, carrying out recrystallization annealing at 1350 ℃ by using an annealing furnace, preserving heat for 2 hours, and naturally cooling;
sixthly, processing the tungsten-molybdenum alloy subjected to heat treatment to the size required by a customer drawing by using a machine, and then carrying out defect flaw detection to detect whether the inside of the alloy material has defects such as cracks, air holes and the like, wherein the inside of the tungsten-molybdenum alloy does not have air hole defects with the average diameter larger than 0.3 mm;
seventhly, washing the machined alloy with clean water, drying and then carrying out vacuum packaging to obtain the alloy with the density of 17.00g/cm3And the average grain size is 35 um.
Example 3
A preparation method of a tungsten-based high specific gravity alloy material comprises the following steps:
selecting tungsten powder, nickel powder and copper powder, wherein the Fisher particle size of the tungsten powder, the nickel powder and the copper powder is 2.8 mu m, the tungsten powder, the nickel powder and the copper powder in batches need to be sampled and analyzed, various physical and chemical performance indexes meet application requirements, screening with a 500-mesh screen, treating oversize materials as waste materials, and taking the tungsten powder and the molybdenum powder below the screen for standby, wherein the mixing ratio of the tungsten powder, the nickel powder and the copper powder is respectively as follows according to the mass fraction: 92%, 4.8% and 3.2%, and stirring the tungsten powder, the nickel powder and the copper powder by adopting a composite stirring mode of sieving stirring and vacuum stirring;
selecting a flexible rubber mold with the specification of 40 multiplied by 100 multiplied by 200mm, cleaning the interior of the flexible rubber mold, uniformly adding tungsten-molybdenum alloy mixed powder, and filling the powder with the weight of 14 kg; after sealing, cold isostatic pressing is carried out, the pressing pressure is 160MPa, and the pressure maintaining time is 30 min; demolding for later use after pressing is finished;
step three, putting the powder blank into a medium-frequency induction sintering furnace, introducing hydrogen as a protective and reducing atmosphere, sintering at 1050 ℃ for 48 hours, cooling along with the furnace, discharging, and measuring the sintering density to be 16.59g/cm3；
Fourthly, heating the sintered blank in a muffle furnace with a hydrogen protective atmosphere at 1000 ℃ for 45min, and carrying out free forging processing on the alloy blank;
step five, using an annealing furnace to carry out recrystallization annealing at 1000 ℃, preserving heat for 2 hours, and naturally cooling;
sixthly, processing the tungsten-nickel-copper alloy subjected to heat treatment to the size required by a customer drawing by using a machine, and then carrying out defect flaw detection to detect whether the inside of the alloy material has defects such as cracks, pores and the like, wherein the inside of the tungsten-nickel-copper alloy does not have pore defects with the average diameter larger than 0.3 mm;
seventhly, washing the machined alloy with clean water, drying and then carrying out vacuum packaging to obtain the alloy with the density of 17.02g/cm3And the average grain size is 35 um.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that while the invention has been described in terms of the above-mentioned embodiments, other embodiments are also possible. It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and it is intended that all such changes and modifications be covered by the appended claims and their equivalents.
Claims (10)
1. A preparation method of a tungsten-based high specific gravity alloy material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
selecting multi-element alloy powder consisting of tungsten powder and other metal powder as a raw material of a tungsten-based high-specific gravity alloy material, and sieving the multi-element alloy powder for later use;
secondly, putting the alloy powder selected in the step one into a die, and preparing a powdery rod blank or a plate blank through cold isostatic pressing;
step three, putting the powdery rod blank or the plate blank into a sintering furnace, and sintering in a hydrogen or vacuum environment to obtain a sintered blank with the density of more than 98 percent for later use;
step four, heating the sintered blank at the temperature of 1000-1600 ℃ for 60-120 min, and then forging the sintered blank by matching with a corresponding die to prepare a forged blank for later use;
step five, annealing the forged blank obtained in the step four at the annealing temperature of 1000-1350 ℃ for 1-12 h, and cooling for later use;
step six, machining the blank processed in the step five to a target required size, and then carrying out defect detection and crystal scanning detection;
and seventhly, washing the qualified product subjected to nondestructive testing in the sixth step by using clean water, drying and then carrying out vacuum packaging to obtain a finished product.
2. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: the grain size of the alloy powder screened in the first step is 160-500 meshes.
3. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: other metal powders in step one include, but are not limited to, Ni, Cu, Fe, Co, Mo, and Cr.
4. The method for preparing the tungsten-based high specific gravity alloy material according to claim 3, wherein the method comprises the following steps: the multi-element alloy powder in the first step is composed of any one of tungsten powder and other metal powder.
5. The method for preparing the tungsten-based high specific gravity alloy material according to claim 4, wherein the method comprises the following steps: the multi-element alloy powder in the step one is composed of any two or more of tungsten powder and other metal powder.
6. The method for preparing the tungsten-based high specific gravity alloy material according to claim 5, wherein the method comprises the following steps: in the first step, the mass part of the tungsten powder is 85-99%, and the mass part of other metal powder is 1-15%.
7. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: and the mould in the step two is a flexible mould, the pressing pressure of the cold isostatic pressing is 150-300 MPa, and the pressure maintaining time is 10-60 min.
8. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: in the third step, the sintering temperature is 1000-2450 ℃, and the sintering time is 4-72 h.
9. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: in the fifth step, the annealing temperature is 1000-1350 ℃, and the annealing heat preservation time is 1-12 h.
10. The method for preparing the tungsten-based high specific gravity alloy material according to claim 1, wherein the method comprises the following steps: and step six, water immersion type ultrasonic C scanning is used, no pore defect with the average diameter larger than 0.3mm exists in the machined tube blank, the wave intensity of the bottom surface of crystal scanning is not smaller than 80%, and the average grain diameter is smaller than 35 um.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114381623A (en) * | 2021-12-15 | 2022-04-22 | 有研工程技术研究院有限公司 | Preparation method of boron-containing high-specific-gravity tungsten-based alloy |
| CN114381623B (en) * | 2021-12-15 | 2022-11-11 | 有研工程技术研究院有限公司 | Preparation method of boron-containing high-specific-gravity tungsten-based alloy |
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Application publication date: 20210928 |