CN110438356A - A method of preparing nanocrystalline tungsten and tungsten alloy bulk - Google Patents
A method of preparing nanocrystalline tungsten and tungsten alloy bulk Download PDFInfo
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- CN110438356A CN110438356A CN201810412181.7A CN201810412181A CN110438356A CN 110438356 A CN110438356 A CN 110438356A CN 201810412181 A CN201810412181 A CN 201810412181A CN 110438356 A CN110438356 A CN 110438356A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Powder Metallurgy (AREA)
Abstract
The present invention relates to powder metallurgical technologies, specifically disclose a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk.This method comprises: 1, grind to pure tungsten or with the mixed powder of other compositions；2, precompressed is carried out to the powder after grinding, obtains green compact；3, green compact assembly is formed into assembly structure in ultra-high pressure sintering mold；4, assembly is sintered, tungsten required for obtaining or tungsten alloy bulk.A kind of method preparing nanocrystalline tungsten and tungsten alloy bulk of the present invention, the crystal grain of tungsten and tungsten alloy bulk can be controlled at hundreds of nanometers until 100 nanometers or less, fusionable material will be studied, especially the direction PMI has huge help, will also form powerful support to the design of China's fusion assay heap.
Description
Technical field
The invention belongs to powder metallurgical technologies, and in particular to a kind of side for preparing nanocrystalline tungsten and tungsten alloy bulk
Method.
Background technique
The material selection of fusion reactor be the key that solve that fusion is practical, wherein most complicated problem first is that plasma
(Plasma Material Interactions, PMI) is interacted with material, it is splashed including material under action of plasma
It penetrates, recycle redeposited evaporation, hydrogen helium is in the precipitation of grain boundaries, tritium fuel infiltration and delay etc..In addition there are also high heat loads, by force
Neutron irradiation etc. critical conditions.
Tungsten fusing point is high, and physical sputtering threshold value is high, and heating conduction is outstanding, more adapts to the long-term running requirement of the following fusion reactor.
Tungsten is all classified as preferred facing plasma material by fusion assay heap (DEMO) and later design.The mechanicalness of nano material
Can be more preferable, anti-neutron irradiation performance is more preferable, while may also have superiority in terms of plasma resistant irradiation and hydrogen, helium delay
Energy.Nanocrystalline tungsten and tungsten alloy get a good chance of becoming a kind of facing plasma material being applied on fusion reactor.However, before
There is no a kind of technique of maturation that can obtain uniform nanocrystalline tungsten and tungsten alloy bulk, therefore systematic research can not be carried out,
Leisure opinion application.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing nanocrystalline tungsten and tungsten alloy bulk, can prepare crystal grain ruler
It is very little in hundreds of nanometers to 100 nanometers of tungsten or tungsten alloy bulks below.
Technical scheme is as follows: a method of nanocrystalline tungsten and tungsten alloy bulk are prepared, this method comprises:
Step 1 is ground to pure tungsten or with the mixed powder of other compositions；
Step 2 carries out precompressed to the powder after grinding, obtains green compact；
Green compact assembly is formed assembly structure by step 3 in ultra-high pressure sintering mold；
Assembly is sintered by step 4, tungsten required for obtaining or tungsten alloy bulk.
The specific steps that powder is ground in the step 1 are as follows:
In glove box, powder is subjected to ball milling, apparent density of powder is improved and is uniformly mixed alloy powder.
The specific steps that precompressed obtains green compact are carried out to the powder of grinding in the step 2 are as follows:
Step 2.1, the powder being put into pre-pressing die after suitable grinding；
Step 2.2, the green compact that the powder in pre-pressing die is pressed into certain shapes, green compact consistency > 60%.
The specific steps of the step 4 are as follows:
Assembly is put into multiface upsetting machine and is sintered by step 4.1；
Mold in step 4.2, removal assembly, tungsten required for obtaining or tungsten alloy bulk.
Assembly is put into the specific steps being sintered in multiface upsetting machine in the step 4.1 are as follows:
Assembly is put into calibrated multiface upsetting machine and is sintered, wherein sintering pressure is 5~10GPa, temperature
It is 600~1200 DEG C, soaking time is 1~4h.
In the step 1, granularity is selected to be nanoscale tungsten powder individually or mix and ground with other compositions.
Hundreds of nanometers or 100 nanometers of crystallite dimension is obtained through oversintering hereinafter, consistency is closed in 90% or more tungsten or tungsten
Gold bullion material.
Remarkable result of the invention is: a kind of method preparing nanocrystalline tungsten and tungsten alloy bulk of the present invention,
The crystal grain of tungsten and tungsten alloy bulk can be controlled at hundreds of nanometers until 100 nanometers hereinafter, will study fusionable material, especially
It is that the direction PMI has huge help, powerful support will be also formed to the design of China's fusion assay heap.
Detailed description of the invention
Fig. 1 is a kind of nanocrystalline tungsten using the method acquisition of the present invention for preparing nanocrystalline tungsten and tungsten alloy bulk
Bulk fracture SEM figure；
Fig. 2 is nanocrystalline using the another kind of the method acquisition of the present invention for preparing nanocrystalline tungsten and tungsten alloy bulk
Tungsten bulk TEM figure；
Fig. 3 is nanocrystalline using the third of the method acquisition of the present invention for preparing nanocrystalline tungsten and tungsten alloy bulk
Tungsten bulk TEM figure；
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Embodiment 1
As described in Figure 1, a method of nanocrystalline tungsten and tungsten alloy bulk are prepared, this method specifically comprises the following steps:
Step 1 grinds tungsten alloy powder；
Using the tungsten powder 49.9g that granularity is 10nm, purity is 99.99%, granularity 100nm, purity are 99.99%
Yttrium powder end 0.1g is added in ball grinder in glove box together with the WC abrading-ball of 500g, and carries out ball milling with the speed of 200rpm；
Ball milling to grind the intermittent mode of 2min pause 1min, when total ball milling a length of 10h, powder is taken out in glove box after the completion of ball milling
End；
Step 2 carries out precompressed to the tungsten alloy powder after grinding, obtains green compact；
In glove box, precompressed is carried out to the tungsten alloy powder after step 1 grinding, obtains the green compact of certain shapes；
Step 2.1, the tungsten alloy powder being put into after suitable grinding in a mold；
The liner tantalum foil in tungsten carbide die, the tungsten alloy powder after being packed into 5g grinding；
Step 2.2, the green compact that the tungsten alloy powder in mold is pressed into certain shapes；
Precompressed, preload pressure 10MPa are carried out using hand-hydraulic tablet press machine；By demoulding after obtain diameter be 12 ±
It 1mm, is highly the green compact of 4 ± 0.5mm；
Green compact assembly is formed assembly structure by step 3 in ultra-high pressure sintering mold；
Assembly is sintered by step 4, tungsten alloy bulk required for obtaining；
Assembly is put into cubic hinge press and is sintered by step 4.1；
Assembly is put into calibrated 1400t cubic hinge press and is sintered, wherein sintering pressure 5GPa, temperature
Degree is 600 DEG C, soaking time 3h；
Mold in step 4.2, removal assembly, obtains required tungsten alloy bulk；
Assembly after the completion of sintering is taken out, and removes mold and residual tantalum foil, obtains 10 ± 1mm of diameter, height 3.5
The tungsten alloy bulk of ± 0.5mm.
The tungsten alloy bulk as shown in Figure 1 of preparation is detected, hardness 18.6GPa, consistency 95.5%,
Grain size about 55nm.
Embodiment 2
As described in Figure 2, a method of nanocrystalline tungsten and tungsten alloy bulk are prepared, this method specifically comprises the following steps:
Step 1 grinds tungsten powder；
Using the tungsten powder 50g that granularity is 20nm, purity is 99.99%, together with the WC abrading-ball of 500g in glove box
It is added in ball grinder, and ball milling is carried out with the speed of 200rpm；Ball milling is to grind the intermittent mode that 2min suspends 1min, total ball milling
Shi Changwei 10h, ball milling take out powder in glove box after the completion；
Step 2 carries out precompressed to the tungsten powder after grinding, obtains green compact；
In glove box, precompressed is carried out to the tungsten powder after step 1 grinding, obtain the green compact of certain shapes；
Step 2.1, the tungsten powder being put into after suitable grinding in a mold；
The liner tantalum foil in tungsten carbide die, the tungsten powder after being packed into 5g grinding；
Step 2.2, the green compact that the tungsten powder in mold is pressed into certain shapes；
Precompressed, preload pressure 6MPa are carried out using hand-hydraulic tablet press machine；By demoulding after obtain diameter be 12 ±
It 1mm, is highly the green compact of 4 ± 0.5mm；
Green compact assembly is formed assembly structure by step 3 in ultra-high pressure sintering mold；
Assembly is sintered by step 4, tungsten bulk required for obtaining；
Assembly is put into cubic hinge press and is sintered by step 4.1；
Assembly is put into calibrated 1400t cubic hinge press and is sintered, wherein sintering pressure 5GPa, temperature
Degree is 800 DEG C, soaking time 4h；
Mold in step 4.2, removal assembly, obtains required tungsten bulk；
Assembly after the completion of sintering is taken out, and removes mold and residual tantalum foil, acquisition 10 ± 1mm of diameter, height 3 ±
The tungsten bulk of 0.5mm.
The tungsten bulk as shown in Figure 2 of preparation is detected, hardness 13GPa, consistency 97.5%, average crystalline substance
Grain size about 120nm.
Embodiment 3
As described in Figure 3, a method of nanocrystalline tungsten and tungsten alloy bulk are prepared, this method specifically comprises the following steps:
Step 1 grinds tungsten powder；
Using the tungsten powder 50g that granularity is 50nm, purity is 99.99%, together with the WC abrading-ball of 500g in glove box
It is added in ball grinder, and ball milling is carried out with the speed of 200rpm；Ball milling is to grind the intermittent mode that 2min suspends 1min, total ball milling
Shi Changwei 10h, ball milling take out powder in glove box after the completion；
Step 2 carries out precompressed to the tungsten powder after grinding, obtains green compact；
In glove box, precompressed is carried out to the tungsten powder after step 1 grinding, obtain the green compact of certain shapes；
Step 2.1, the tungsten powder being put into after suitable grinding in a mold；
Tungsten powder after being packed into 5g grinding in molybdenum cup, molybdenum cup is put into tungsten carbide die；
Step 2.2, the green compact that the tungsten powder in mold is pressed into certain shapes；
Precompressed, preload pressure 10MPa are carried out using hand-hydraulic tablet press machine；By demoulding after obtain diameter be 12 ±
It 1mm, is highly the green compact of 4 ± 0.5mm；
Green compact assembly is formed assembly structure by step 3 in ultra-high pressure sintering mold；
Assembly is sintered by step 4, tungsten bulk required for obtaining；
Assembly is put into cubic hinge press and is sintered by step 4.1；
Assembly is put into calibrated 1400t cubic hinge press and is sintered, wherein sintering pressure 5GPa, temperature
Degree is 1000 DEG C, soaking time 2h；
Mold in step 4.2, removal assembly, obtains required tungsten bulk；
Assembly after the completion of sintering is taken out, and removes mold and residual molybdenum cup, acquisition 10 ± 1mm of diameter, height 2 ±
The tungsten bulk of 0.5mm.
The tungsten bulk as shown in Figure 3 of preparation is detected, hardness 19.3GPa, consistency 92.0%, it is average
Grain size about 70nm.
Claims (7)
1. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk, it is characterised in that: this method comprises:
Step 1 is ground to pure tungsten or with the mixed powder of other compositions；
Step 2 carries out precompressed to the powder after grinding, obtains green compact；
Green compact assembly is formed assembly structure by step 3 in ultra-high pressure sintering mold；
Assembly is sintered by step 4, tungsten required for obtaining or tungsten alloy bulk.
2. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 1, it is characterised in that: described
The specific steps that powder is ground in step 1 are as follows:
In glove box, powder is subjected to ball milling, apparent density of powder is improved and is uniformly mixed alloy powder.
3. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 1, it is characterised in that: described
The specific steps that precompressed obtains green compact are carried out to the powder of grinding in step 2 are as follows:
Step 2.1, the powder being put into pre-pressing die after suitable grinding；
Step 2.2, the green compact that the powder in pre-pressing die is pressed into certain shapes, green compact consistency > 60%.
4. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 1, it is characterised in that: described
The specific steps of step 4 are as follows:
Assembly is put into multiface upsetting machine and is sintered by step 4.1；
Mold in step 4.2, removal assembly, tungsten required for obtaining or tungsten alloy bulk.
5. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 4, it is characterised in that: described
Assembly is put into the specific steps being sintered in multiface upsetting machine in step 4.1 are as follows:
Assembly is put into calibrated multiface upsetting machine and is sintered, wherein sintering pressure is 5~10GPa, and temperature is
600~1200 DEG C, soaking time is 1~4h.
6. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 1 or 2, it is characterised in that: institute
In the step 1 stated, granularity is selected to be nanoscale tungsten powder individually or mix and ground with other compositions.
7. a kind of method for preparing nanocrystalline tungsten and tungsten alloy bulk according to claim 1, it is characterised in that: through burning
Knot obtains hundreds of nanometers or 100 nanometers of crystallite dimension hereinafter, the tungsten or tungsten alloy bulk of the consistency 90% or more.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113023764A (en) * | 2021-03-19 | 2021-06-25 | 襄阳汽车职业技术学院 | Preparation method of copper-based perovskite nanocrystalline film |
| CN116102353A (en) * | 2023-02-01 | 2023-05-12 | 武汉理工大学 | Superfine nanometer A 2 B 2 O 7 Structural high-entropy ceramic and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023764A (en) * | 2021-03-19 | 2021-06-25 | 襄阳汽车职业技术学院 | Preparation method of copper-based perovskite nanocrystalline film |
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| CN116102353A (en) * | 2023-02-01 | 2023-05-12 | 武汉理工大学 | Superfine nanometer A 2 B 2 O 7 Structural high-entropy ceramic and preparation method thereof |
| CN116102353B (en) * | 2023-02-01 | 2024-02-27 | 武汉理工大学 | Superfine nanometer A 2 B 2 O 7 Structural high-entropy ceramic and preparation method thereof |
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