CN114457222B - Method for improving processability of high-purity tungsten - Google Patents

Method for improving processability of high-purity tungsten Download PDF

Info

Publication number
CN114457222B
CN114457222B CN202111162011.6A CN202111162011A CN114457222B CN 114457222 B CN114457222 B CN 114457222B CN 202111162011 A CN202111162011 A CN 202111162011A CN 114457222 B CN114457222 B CN 114457222B
Authority
CN
China
Prior art keywords
tungsten
temperature
tungsten material
heat preservation
preservation time
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111162011.6A
Other languages
Chinese (zh)
Other versions
CN114457222A (en
Inventor
王亚峰
王占卫
彭立培
冀嘉梁
林坤
冯海波
孙秋丽
童莹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
718th Research Institute of CSIC
Original Assignee
718th Research Institute of CSIC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 718th Research Institute of CSIC filed Critical 718th Research Institute of CSIC
Priority to CN202111162011.6A priority Critical patent/CN114457222B/en
Publication of CN114457222A publication Critical patent/CN114457222A/en
Application granted granted Critical
Publication of CN114457222B publication Critical patent/CN114457222B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/003Selecting material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/06Heating or cooling methods or arrangements specially adapted for performing forging or pressing operations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21JFORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002Hybrid process, e.g. forging following casting
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D11/00Process control or regulation for heat treatments
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention relates to a method for improving the processing performance of high-purity tungsten, and belongs to the technical field of tungsten material processing. The method adopts the corresponding processing method according to the difference of the metallographic structures of the high-purity tungsten as follows: detecting a metallographic structure of a tungsten material with the purity of more than 99.999%, and when the metallographic structure of the tungsten material is an isometric crystal, performing the following treatment: high temperature treatment, forging, recrystallization annealing and furnace cooling, so as to improve the processing performance of the tungsten material; when the metallographic structure of the tungsten material is columnar crystal, the following treatment is carried out: high temperature treatment, forging, recrystallization annealing, furnace cooling, high temperature rolling, recrystallization treatment and furnace cooling, and the processing performance of the tungsten material can be improved. According to the method, the processing performance of the high-purity tungsten is improved by adopting a corresponding method according to different metallographic structures of the high-purity tungsten, and the defect of low processing yield such as material breakage, particle falling and cracking in the high-purity tungsten processing technology is overcome.

Description

Method for improving processability of high-purity tungsten
Technical Field
The invention relates to a method for improving the processing performance of high-purity tungsten, and belongs to the technical field of tungsten material processing.
Background
Tungsten is a metal material with high density, high melting point and high hardness, and high purity tungsten is generally tungsten material with purity of more than 99.999%, and has important application in the fields of integrated circuits, crystal smelting, medical treatment, nuclear industry, armor, aerospace and the like.
The preparation method of the high-purity tungsten mainly comprises powder metallurgy and chemical vapor deposition. The method for preparing the high-purity tungsten by powder metallurgy is to utilize tungsten powder as a raw material, press the tungsten powder into a shape by adopting isostatic pressing, then utilize multiple times of sintering to improve the compactness of the material, and finally finish the preparation of the high-purity tungsten by forging or rolling. The chemical vapor deposition is to prepare high-purity tungsten by taking hydrogen and tungsten hexafluoride as raw materials or taking hydrogen and tungsten hexachloride as raw materials and introducing the raw materials into a reactor under a certain temperature condition to react on the surface of a substrate.
Because the high-purity tungsten has the characteristics of high hardness, high wear resistance, high normal-temperature brittleness, easy corner breakage and particle falling during processing, in the field of linear cutting, polishing, rolling, turning, drilling, forging, electric spark, precision machining and other material processing of the high-purity tungsten material, the problems of material breakage, cracking, cutting wire breakage, low polishing efficiency and the like caused by internal defects or processing stress in the processing process are solved, the processing of a high-purity tungsten finished product is difficult to be completed by the traditional mechanical processing method, only relatively stable electric spark processing and diamond grinding processing can be adopted, and the processing method is single and has poor yield, so that serious resource waste is caused.
Aiming at the problems of high processing difficulty, high yield and the like of the high-purity tungsten, the prior art utilizes the thermoplasticity of the tungsten to apply external force, overcomes the resistance of the tungsten to deformation, and enables the tungsten to generate plastic deformation so as to achieve the aim of improving the tungsten performance, a specific improvement method is not specifically proposed for solving the technical problems of poor processing yield and the like of the high-purity tungsten, and a method for improving the processing performance of the high-purity tungsten is not explicitly proposed by referring to the rest prior art.
Disclosure of Invention
In order to overcome the defect of low processing yield such as material breakage, particle falling and cracking in the existing high-purity tungsten processing technology, the invention aims to provide a method for improving the processing performance of high-purity tungsten.
In order to achieve the purpose of the invention, the following technical scheme is provided.
A method for improving the processing performance of high-purity tungsten adopts a corresponding processing method according to the difference of the metallographic structures of the high-purity tungsten, and comprises the following steps:
the metallographic structure of the tungsten material with the purity of more than 99.999 percent is detected:
when the metallographic structure of the tungsten material is equiaxed crystal, the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1000-1500 ℃, and the heat preservation time is 0.5-3.0 h, so as to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), with the forging ratio of 1:1-4:1, so as to obtain the forged tungsten material.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1000-1500 ℃, and the heat preservation time is 1.0-4.0 h.
(4) And cooling along with the furnace after the annealing is finished, so that the processing performance of the tungsten material can be improved.
In step (1):
preferably, the temperature of the high-temperature treatment is 1200-1300 ℃, and the heat preservation time is 2.0-3.0 h.
In the step (2):
preferably, the forging ratio is 2:1 to 3:1.
In the step (3):
preferably, the recrystallization annealing temperature is 1100-1400 ℃, and the heat preservation time is 2.0-3.0 h.
Preferably, the step (2) is repeated for 0 to 3 times in a cyclic manner, that is, the step (2) is performed for 1 to 4 times in total, and then the step (3) is performed.
When the metallographic structure of the tungsten material is columnar crystal, the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1100-1600 ℃, and the heat preservation time is 1.0-4.0 h, so as to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), with the forging ratio of 1:1-5:1, so as to obtain the forged tungsten material.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1000-1400 ℃, and the heat preservation time is 1.0-4.0 h.
(4) And cooling along with the furnace after the annealing is finished, and obtaining the cooled tungsten material.
(5) And (3) carrying out high-temperature rolling on the cooled tungsten material prepared in the step (4), wherein the high-temperature rolling temperature is 1100-1700 ℃, the heat preservation time is 1.0-3.0 h, the rolling passes are 1-5 times, and the rolled tungsten material is obtained after the rolling is finished.
(6) Putting the rolled tungsten material prepared in the rolling step (5) into a vacuum furnace for recrystallization treatment, wherein the temperature of the recrystallization treatment is 1200-1700 ℃, and the heat preservation time is 1.0-4.0 h; and cooling along with the furnace, so that the processing performance of the high-purity tungsten can be improved.
In step (1):
preferably, the temperature of the high-temperature treatment is 1200-1400 ℃, and the heat preservation time is 1.0-3.0 h.
In the step (2):
preferably, the forging ratio is 2:1 to 4:1.
In the step (3):
preferably, the recrystallization annealing temperature is 1100-1300 ℃, and the heat preservation time is 2.0-3.0 h.
In the step (5):
the preferable high-temperature rolling temperature is 1300-1600 ℃ and the heat preservation time is 2.0-3.0 h.
In the step (6):
preferably, the temperature of the recrystallization treatment is 1300-1500 ℃, and the heat preservation time is 2.0-3.0 h.
Preferably, the step (2) is repeated 0 to 3 times, i.e., the step (2) is repeated 1 to 4 times in total, and then the step (3) is performed.
Advantageous effects
1. The invention provides a method for improving the processing performance of high-purity tungsten, which adopts a targeted processing method to improve the processing performance of the high-purity tungsten according to the difference of metallographic structure areas of the high-purity tungsten, namely tungsten materials with the purity of more than 99.999 percent; by adopting the method, on one hand, the yield of the finished product of the high-purity tungsten material in the machining process is obviously improved, the resources are effectively saved, the production cost is reduced, and on the other hand, the occurrence of coarse tissues in the high-purity tungsten product is avoided, fine and uniform equiaxed crystals are obtained, and the product quality and the service performance are improved.
2. The invention provides a method for improving the processing performance of high-purity tungsten, wherein in the method, when the metallographic structure of a tungsten material is an isometric crystal, the internal stress of the tungsten material is released in the step (1); the internal tissue structure of the tungsten material is disturbed by external force, the dislocation density in the tissue is increased, energy is stored for subsequent recrystallization treatment, and the original tissue structure is equiaxed crystal, so that the aim of disturbing the tissue structure can be completely achieved after the treatment in the step (3), and rolling treatment is not needed; in the step (3), when the deformed tungsten material is heated at a higher temperature, the elongated or flattened and crushed crystal grains are changed into new uniform and fine equiaxed crystals through re-nucleation and growth due to the increase of the atomic diffusion capacity, after the deformed tungsten material is recrystallized, the strength and hardness of the material are obviously reduced, the plasticity and toughness are greatly improved, the work hardening phenomenon is eliminated, the internal stress almost completely disappears, and the lattice type of the generated new crystal grains is consistent with the lattice type before and after deformation.
3. The invention provides a method for improving the processing performance of high-purity tungsten, wherein in the method, when the metallographic structure of a tungsten material is columnar crystal, the internal stress of the tungsten material is released in the step (1), the internal structure of the tungsten material is disturbed by external force in the step (2), and the original structure form cannot be thoroughly disturbed by single forging treatment at the moment, so that the aim of completely disturbing the columnar crystal structure is fulfilled by the treatment in the step (5) after the steps (3) and (4); in the step (6), during recrystallization annealing, broken crystal grains are changed into a new uniform and fine equiaxed crystal structure through re-nucleation and growth, the strength and hardness of the tungsten material are obviously reduced, and the plasticity and toughness are greatly improved.
Drawings
FIG. 1 is an isometric crystalline metallographic view of a tungsten material having a purity of 99.999% prior to the start of step (1) of example 1.
Fig. 2 is an isometric crystalline metallographic view of the tungsten material with improved processability obtained in step (4) of example 1.
Fig. 3 is an isometric crystalline metallographic view of a tungsten material having a purity of 99.999% prior to the start of step (1) of example 2.
Fig. 4 is an isometric crystalline metallographic view of the tungsten material with improved processability obtained in step (4) of example 2.
FIG. 5 is a columnar crystalline metallographic structure of tungsten material having a purity of 99.9999% before the start of step (1) of example 3.
Fig. 6 is an isometric crystalline metallographic view of the tungsten material with improved processability obtained in step (6) of example 3.
FIG. 7 is a diagram showing the columnar crystalline metallographic structure of tungsten material having a purity of 99.99999% before the start of step (1) in example 4.
Fig. 8 is an isometric crystalline metallographic view of the tungsten material with improved processability obtained in step (6) of example 4.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In the following examples:
sampling and detecting the metallographic structure of the material, wherein the detection method is according to the standard of GB/T13298-2015 metal microstructure detection method.
Example 1
A method for improving the processing performance of high-purity tungsten comprises the following specific steps:
the metallographic structure of the tungsten material with the purity of 99.999 percent is sampled and detected, the detection result is shown in figure 1, the scale in figure 1 is 100 mu m, the metallographic structure of the tungsten material is known to be equiaxed crystal according to the detection result, and the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1000 ℃, the heat preservation time is 3.0h, and cooling along with a furnace to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), wherein the forging ratio is 1:1, and the total forging is performed for 4 times, so that the forged tungsten material is obtained.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1000 ℃, and the heat preservation time is 1.0h.
(4) And cooling along with the furnace after the annealing is finished, so that the processing performance of the high-purity tungsten can be improved, and the tungsten material with improved processing performance is obtained.
Sampling and detecting the metallographic structure of the tungsten material with improved processing performance, which is prepared in the step (4), wherein the metallographic structure of the tungsten material is an isometric crystal according to detection results, as shown in fig. 2, the scale in fig. 2 is 100 mu m, and compared with fig. 1, the metallographic structure of the tungsten material sample is improved in grain uniformity and finer in grain size, which indicates that the metallographic structure of the tungsten material is improved.
Example 2
A method for improving the processing performance of high-purity tungsten comprises the following specific steps:
the metallographic structure of the tungsten material with the purity of 99.999 percent is sampled and detected, the detection result is shown in fig. 3, the scale in fig. 3 is 100 mu m, the metallographic structure of the tungsten material is known to be equiaxed crystal according to the detection result, and the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1500 ℃, the heat preservation time is 0.5h, and cooling along with a furnace to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), with the forging ratio of 4:1, and forging for 1 time to obtain the forged tungsten material.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1500 ℃, and the heat preservation time is 4.0h.
(4) And cooling along with the furnace after the annealing is finished, so that the processing performance of the high-purity tungsten can be improved, and the tungsten material with improved processing performance is obtained.
Sampling and detecting the metallographic structure of the tungsten material with improved processing performance, which is prepared in the step (4), wherein the metallographic structure of the tungsten material is an isometric crystal according to detection results, as shown in fig. 4, the scale in fig. 4 is 100 mu m, and compared with fig. 3, the metallographic structure of the tungsten material sample is improved in grain uniformity and finer in grain size, which indicates that the metallographic structure of the tungsten material is improved.
Example 3
A method for improving the processing performance of high-purity tungsten comprises the following specific steps:
the metallographic structure of the tungsten material with the purity of 99.9999% is sampled and detected, the detection result is shown in fig. 5, the scale in fig. 5 is 500 μm, the metallographic structure of the tungsten material is known to be columnar crystal according to the detection result, and the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1100 ℃, the heat preservation time is 4.0h, and cooling along with a furnace to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), with the forging ratio of 1:1, and forging for 1 time to obtain the forged tungsten material.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1000 ℃, and the heat preservation time is 4.0h.
(4) And cooling along with the furnace after the annealing is finished, and obtaining the cooled tungsten material.
(5) And (3) carrying out high-temperature rolling on the cooled tungsten material prepared in the step (4), wherein the high-temperature rolling temperature is 1100 ℃, the heat preservation time is 3.0h, the rolling pass is 1 time, and the rolled tungsten material is obtained after the rolling is finished.
(6) Putting the rolled tungsten material prepared in the rolling step (5) into a vacuum furnace for recrystallization treatment, wherein the temperature of the recrystallization treatment is 1200 ℃, and the heat preservation time is 4.0h; and cooling along with the furnace, so that the processing performance of the high-purity tungsten can be improved, and the tungsten material with improved processing performance is obtained.
Sampling and detecting the metallographic structure of the tungsten material with improved processability obtained in the step (6), wherein the metallographic structure of the tungsten material is an isometric crystal according to the detection result, as shown in fig. 6, the scale in fig. 6 is 500 mu m, and comparing with fig. 5, the metallographic structure of the tungsten material sample is changed from columnar crystals to isometric crystals after complete recrystallization, and the isometric crystals are small in size and uniform in distribution, so that the metallographic structure of the tungsten material is improved.
Example 4
A method for improving the processing performance of high-purity tungsten comprises the following specific steps:
sampling and detecting the metallographic structure of the tungsten material with the purity of 99.99999%, detecting according to the standard of GB/T13298-2015 metal microstructure detection method, wherein the detection result is shown in figure 7, the scale in figure 7 is 500 mu m, the metallographic structure of the tungsten material is known to be columnar crystal according to the detection result, and the following treatment is carried out:
(1) And (3) carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1600 ℃, the heat preservation time is 1.0h, and cooling along with a furnace to obtain the tungsten material after the high-temperature treatment.
(2) Forging the tungsten material subjected to the high-temperature treatment, which is obtained in the step (1), for 4 times at a forging ratio of 5:1, so as to obtain the forged tungsten material.
(3) And (3) carrying out recrystallization annealing on the forged tungsten material prepared in the step (2), wherein the recrystallization annealing temperature is 1400 ℃, and the heat preservation time is 1.0h.
(4) And cooling along with the furnace after the annealing is finished, and obtaining the cooled tungsten material.
(5) And (3) carrying out high-temperature rolling on the cooled tungsten material prepared in the step (4), wherein the high-temperature rolling temperature is 1700 ℃, the heat preservation time is 1.0h, the rolling pass is 5 times, and the rolled tungsten material is obtained after the rolling is finished.
(6) Putting the rolled tungsten material prepared in the rolling step (5) into a vacuum furnace for recrystallization treatment, wherein the temperature of the recrystallization treatment is 1700 ℃, and the heat preservation time is 1.0h; and cooling along with the furnace, so that the processing performance of the high-purity tungsten can be improved, and the tungsten material with improved processing performance can be obtained.
Sampling and detecting the metallographic structure of the tungsten material with improved processability obtained in the step (6), wherein the metallographic structure of the tungsten material is an isometric crystal according to the detection result, as shown in fig. 8, the scale in fig. 8 is 500 mu m, and comparing fig. 7, the metallographic structure of the tungsten material sample is changed from columnar crystals to isometric crystals after complete recrystallization, and the isometric crystals are finer in size and uniform in distribution, which indicates that the metallographic structure of the tungsten material is improved.
Example 5
The following tests were conducted on the tungsten material before improvement of workability and the tungsten material after improvement of workability in examples 1 to 4:
(1) Hardness test
The hardness of the samples in the examples was measured according to GB/T4340.1-2009 Vickers hardness test part 1: the test method is used for detecting according to the standard of the test method, and the detection and calibration of the sclerometer in the detection process are strictly according to the Vickers hardness test part 2 of the GB/T4340.2-2012 metal materials: the durometer test and calibration is performed in accordance with the standard.
The hardness test results are shown in tables 1 and 2, and the hardness of the tungsten materials with improved processability prepared in examples 1 to 4 is significantly reduced after being treated by the method for improving high purity tungsten processability according to the present invention. The hardness of the tungsten material directly influences the mechanical processing performance of the tungsten material, so that the internal stress of the tungsten material is completely eliminated in the recrystallization annealing process, and the strength and toughness of the tungsten material are obviously improved due to the formation of new fine grains caused by recrystallization.
Table 1 hardness of tungsten Material with equiaxed Crystal metallographic Structure
Figure BDA0003290573880000081
Table 2 hardness of tungsten Material with columnar Crystal metallographic Structure
Figure BDA0003290573880000082
(2) Yield of processing
The machining conditions of the tungsten materials with improved machining performance in examples 1 to 4 were tested, and wire cutting machining, turning, rough grinding, electric spark and fine grinding were sequentially performed, and finally the tungsten materials were machined to finished products, and each finished product was inspected and accepted according to the technical requirements of the machining drawing (mainly from the aspects of product size, finish, surface roughness, edge portion, surface chipping condition, and the like). Proved by acceptance results, the processing qualification rate of the tungsten material with improved processing performance prepared in the examples 1-4 is greatly improved.
TABLE 3 material processing yield
Figure BDA0003290573880000091
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (10)

1. A method for improving the processability of high purity tungsten, which is characterized in that: the method comprises the following steps: the metallographic structure of the tungsten material with the purity of more than 99.999 percent is detected:
when the metallographic structure of the tungsten material is equiaxed crystal, the following treatment is carried out:
(1) Carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1000-1500 ℃, and the heat preservation time is 0.5-3.0 h, so as to obtain the tungsten material after the high-temperature treatment;
(2) Forging the tungsten material subjected to high-temperature treatment, wherein the forging ratio is 1:1-4:1, and obtaining the forged tungsten material;
(3) Carrying out recrystallization annealing on the forged tungsten material, wherein the recrystallization annealing temperature is 1000-1500 ℃, and the heat preservation time is 1.0-4.0 h;
(4) Cooling along with the furnace after annealing is finished, so that the processing performance of the tungsten material can be improved;
when the metallographic structure of the tungsten material is columnar crystal, the following treatment is carried out:
(1) Carrying out high-temperature treatment on the tungsten material, wherein the temperature of the high-temperature treatment is 1100-1600 ℃ and the heat preservation time is 1.0-4.0 h, so as to obtain the tungsten material after the high-temperature treatment;
(2) Forging the tungsten material subjected to high-temperature treatment, wherein the forging ratio is 1:1-5:1, and obtaining the forged tungsten material;
(3) Carrying out recrystallization annealing on the forged tungsten material, wherein the recrystallization annealing temperature is 1000-1400 ℃, and the heat preservation time is 1.0-4.0 h;
(4) Cooling along with the furnace after annealing is completed, and obtaining a cooled tungsten material;
(5) Carrying out high-temperature rolling on the cooled tungsten material, wherein the high-temperature rolling temperature is 1100-1700 ℃, the heat preservation time is 1.0-3.0 h, the rolling passes are 1-5 times, and the rolled tungsten material is obtained after the rolling is finished;
(6) The rolled tungsten material is put into a vacuum furnace for recrystallization treatment, the temperature of the recrystallization treatment is 1200 ℃ to 1700 ℃, and the heat preservation time is 1.0h to 4.0h; and cooling along with the furnace, so that the processing performance of the high-purity tungsten can be improved.
2. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal: in the step (1), the temperature of high-temperature treatment is 1200-1300 ℃, and the heat preservation time is 2.0-3.0 h;
when the metallographic structure of the tungsten material is columnar crystal: in the step (1), the temperature of high-temperature treatment is 1200-1400 ℃, and the heat preservation time is 1.0-3.0 h.
3. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal: in the step (2), the forging ratio is 2:1-3:1;
when the metallographic structure of the tungsten material is columnar crystal: in the step (2), the forging ratio is 2:1-4:1.
4. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal: in the step (3), the recrystallization annealing temperature is 1100-1400 ℃, and the heat preservation time is 2.0-3.0 h;
when the metallographic structure of the tungsten material is columnar crystal: in the step (3), the recrystallization annealing temperature is 1100-1300 ℃, and the heat preservation time is 2.0-3.0 h.
5. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal: step (2) is carried out for 1 to 4 times, and then step (3) is carried out;
when the metallographic structure of the tungsten material is columnar crystal: step (2) is carried out for 1 to 4 times, and then step (3) is carried out.
6. A method of improving the processability of high purity tungsten according to claim 1, wherein: when the metallographic structure of the tungsten material is columnar crystal: in the step (5), the high-temperature rolling temperature is 1300-1600 ℃ and the heat preservation time is 2.0-3.0 h.
7. A method of improving the processability of high purity tungsten according to claim 1, wherein: when the metallographic structure of the tungsten material is columnar crystal: in the step (6), the temperature of recrystallization treatment is 1300-1500 ℃, and the heat preservation time is 2.0-3.0 h.
8. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal:
in the step (1), the temperature of high-temperature treatment is 1200-1300 ℃, and the heat preservation time is 2.0-3.0 h;
in the step (2), the forging ratio is 2:1-3:1;
step (2) is carried out for 1 to 4 times, and then step (3) is carried out;
in the step (3), the recrystallization annealing temperature is 1100-1400 ℃, and the heat preservation time is 2.0-3.0 h.
9. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is columnar crystal:
in the step (1), the temperature of high-temperature treatment is 1200-1400 ℃, and the heat preservation time is 1.0-3.0 h;
in the step (2), the forging ratio is 2:1-4:1;
step (2) is carried out for 1 to 4 times, and then step (3) is carried out;
in the step (3), the recrystallization annealing temperature is 1100-1300 ℃, and the heat preservation time is 2.0-3.0 h;
in the step (5), the high-temperature rolling temperature is 1300-1600 ℃ and the heat preservation time is 2.0-3.0 h;
in the step (6), the temperature of recrystallization treatment is 1300-1500 ℃, and the heat preservation time is 2.0-3.0 h.
10. A method of improving the processability of high purity tungsten according to claim 1, wherein:
when the metallographic structure of the tungsten material is equiaxed crystal:
in the step (1), the temperature of high-temperature treatment is 1200-1300 ℃, and the heat preservation time is 2.0-3.0 h;
in the step (2), the forging ratio is 2:1-3:1;
step (2) is carried out for 1 to 4 times, and then step (3) is carried out;
in the step (3), the recrystallization annealing temperature is 1100-1400 ℃, and the heat preservation time is 2.0-3.0 h;
when the metallographic structure of the tungsten material is columnar crystal:
in the step (1), the temperature of high-temperature treatment is 1200-1400 ℃, and the heat preservation time is 1.0-3.0 h;
in the step (2), the forging ratio is 2:1-4:1;
step (2) is carried out for 1 to 4 times, and then step (3) is carried out;
in the step (3), the recrystallization annealing temperature is 1100-1300 ℃, and the heat preservation time is 2.0-3.0 h;
in the step (5), the high-temperature rolling temperature is 1300-1600 ℃ and the heat preservation time is 2.0-3.0 h;
in the step (6), the temperature of recrystallization treatment is 1300-1500 ℃, and the heat preservation time is 2.0-3.0 h.
CN202111162011.6A 2021-09-30 2021-09-30 Method for improving processability of high-purity tungsten Active CN114457222B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111162011.6A CN114457222B (en) 2021-09-30 2021-09-30 Method for improving processability of high-purity tungsten

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111162011.6A CN114457222B (en) 2021-09-30 2021-09-30 Method for improving processability of high-purity tungsten

Publications (2)

Publication Number Publication Date
CN114457222A CN114457222A (en) 2022-05-10
CN114457222B true CN114457222B (en) 2023-07-14

Family

ID=81405983

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111162011.6A Active CN114457222B (en) 2021-09-30 2021-09-30 Method for improving processability of high-purity tungsten

Country Status (1)

Country Link
CN (1) CN114457222B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5722034A (en) * 1994-12-09 1998-02-24 Japan Energy Corporation Method of manufacturing high purity refractory metal or alloy
JP2001295036A (en) * 2000-04-17 2001-10-26 Toshiba Corp Tungsten sputtering target and its manufacturing method
CN101070190A (en) * 2007-06-16 2007-11-14 中国船舶重工集团公司第七一八研究所 Method for purifying tungsten hexafluoride
CN101219591A (en) * 2006-12-27 2008-07-16 山特维克知识产权股份有限公司 CVD coated cemented carbide insert for toughness demanding short hole drilling operations
CN107841648A (en) * 2017-11-22 2018-03-27 有研亿金新材料有限公司 A kind of method for improving platinum-tungsten alloys hot-working character

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5722034A (en) * 1994-12-09 1998-02-24 Japan Energy Corporation Method of manufacturing high purity refractory metal or alloy
JP2001295036A (en) * 2000-04-17 2001-10-26 Toshiba Corp Tungsten sputtering target and its manufacturing method
CN101219591A (en) * 2006-12-27 2008-07-16 山特维克知识产权股份有限公司 CVD coated cemented carbide insert for toughness demanding short hole drilling operations
CN101070190A (en) * 2007-06-16 2007-11-14 中国船舶重工集团公司第七一八研究所 Method for purifying tungsten hexafluoride
CN107841648A (en) * 2017-11-22 2018-03-27 有研亿金新材料有限公司 A kind of method for improving platinum-tungsten alloys hot-working character

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
对引进日本东芝公司钨材加工工艺的改进;罗维云,姜仁辉;上海有色金属(第03期);119-125 *

Also Published As

Publication number Publication date
CN114457222A (en) 2022-05-10

Similar Documents

Publication Publication Date Title
CN108446478B (en) Design method of multi-component high-strength titanium alloy
CN113430405B (en) High-strength and high-toughness face-centered cubic high-entropy alloy and preparation method thereof
CN111850544A (en) High-entropy alloy coating and preparation method thereof
CN113897564B (en) Non-uniform nano heterogeneous structure of high-toughness medium-entropy alloy
EP2737966A1 (en) Method for manufacturing alloy containing transition metal carbide, tungsten alloy containing transition metal carbide, and alloy manufactured by said method
CN110438350B (en) Pure molybdenum block and preparation method thereof
CN102268616B (en) Cutting steel wire modified by amorphous alloy
CN113652593A (en) MoxNbTayTiV high-entropy alloy and preparation method thereof
CN114457222B (en) Method for improving processability of high-purity tungsten
Rhys The fabrication and properties of ruthenium
Wang et al. Remarkable ductility in metastable refractory high entropy alloys via BCC-FCC/α ″martensitic transformations
CN112251684B (en) Micro-nanocrystalline maraging steel and preparation method thereof
CN115821138A (en) Potassium-doped tungsten alloy block material and preparation method and application thereof
CN112195366B (en) High-thermal-stability equiaxial nanocrystalline Ti-Zr-Ag alloy and preparation method thereof
CN112342431B (en) High-thermal-stability equiaxial nanocrystalline Ti6Al4V-Cu alloy and preparation method thereof
Fox et al. Microstructure and creep behavior of silicon nitride and SiAlONs
CN114645253A (en) Semiconductor tantalum target material and forging method thereof
CN114457319A (en) Preparation method of high-purity tungsten target material
Zhang et al. Ce Effects on Deformation‐Induced Microstructure Evolution in Cu–Ti–Ni–Mg Alloys
CN115161444B (en) Low-expansion alloy 4J36 precise foil and superfine crystal solid solution heat treatment method and application thereof
Tesi et al. Analysis of surface structures and of size and shape variations in ionitrided precipitation hardening stainless steel samples
CN112251638B (en) High-thermal-stability equiaxial nanocrystalline Ti-Cu alloy and preparation method thereof
CN113862592B (en) Heat treatment method of iron-containing metastable beta titanium alloy
Gao et al. High Hardness and High Toughness WC–Fe–Ni‐Cemented Carbides Prepared by Hot Oscillating Pressing
Xiao et al. High temperature plastic deformation behavior of non-oriented electrical steel

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant