CN110205573A - The quick annealing process of regulation deformation tungsten material microstructure under a kind of low temperature - Google Patents
The quick annealing process of regulation deformation tungsten material microstructure under a kind of low temperature Download PDFInfo
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- CN110205573A CN110205573A CN201910547049.1A CN201910547049A CN110205573A CN 110205573 A CN110205573 A CN 110205573A CN 201910547049 A CN201910547049 A CN 201910547049A CN 110205573 A CN110205573 A CN 110205573A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/38—Heating by cathodic discharges
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing 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
- C22F1/18—High-melting or refractory metals or alloys based thereon
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Abstract
The invention discloses quickly regulation deforms the annealing process of tungsten (W) material microstructure under a kind of low temperature, sample is heated using discharge plasma sintering (SPS) technology, and the DC pulse current on sample is acted on using it, accelerate the Microstructures Evolvement of deformation W material.The microscopic structure of W material is regulated and controled by changing SPS technological parameter.The present invention realizes that efficient, energy conservation makes annealing treatment to W material using SPS technology, regulates and controls its microscopic structure.The annealing temperature of selection is lower than 1000 DEG C, and the entire annealing process duration is less than 60min, shows apparent advantage compared to deformation W anneal of material (recrystallization annealing needs to keep the temperature a few hours at 1350 DEG C) under normal vacuum.
Description
Technical field
The present invention relates to the annealing process for quickly regulating and controlling deformation tungsten material microstructure under a kind of low temperature, belong to metal material
Technical field of heat treatment technology.
Background technique
Tungsten (W) has high-melting-point (3422 DEG C), high heat conductance (room temperature 173W/mK), high sputtering threshold value, good high temperature power
The advantages that learning performance, is widely used in the engineering fields such as nuclear energy, electronic device, military affairs, space flight.In order to meet different field
Using, the microscopic structure of W material can be regulated and controled with it is expected obtain different performance W material.And annealing is regulation deformation states W material
One of effective means of microscopic structure.In annealing process, Recovery and recrystallization can occur for deformation W material, to realize to change
Shape W material microstructure is regulated and controled.
Annealing of metal materials heat treatment is usually to carry out in traditional heat-treatment furnace, passes through conduction, convection current and radiation etc.
Comprehensive method makes material (general > 0.3T at relatively high temperaturesm) the continuous heating long period.The energy consumed during this in addition to
Outside being heat-treated to material, more energy consumptions are in furnace body heating and radiation loss.Conventional anneal is heat-treated not
But a large amount of energy is consumed, and low efficiency.For W pure for rolling deformation state, conventional anneal heat treatment is needed 1350
A few hours are kept the temperature at DEG C, are just able to achieve perfect recrystallization.In addition, when carrying out annealing heat-treatment using traditional approach, for a long time
High temperature will lead to the coarse grains of material, tissue odds.
Annealing heat-treatment is directly carried out by metal material using DC pulse current, can be used as conventional anneal heat treatment
Alternative.When electric current passes through metal material, Joule heat caused by its own internal resistance (fuel factor) will directly to material into
Row heating；Meanwhile high-density current carries high-throughput electronics, can promote atomic migration (non-thermal effect), accelerates metal material
Expect Microstructures Evolvement.Heat and non-thermal effect synergistic effect, promote the migration of dislocation, accelerate deformable metal material and occur back
Multiple, recrystallization, grain growth and phase transition process, to obtain microscopic structure after uniform heat treatment.SPS technology can provide directly
Stream pulse current directly heats sample and assists applying mechanical pressure.Therefore, it is expected to using SPS technology real under cryogenic
Now deformation W material microstructure is quickly regulated and controled, with the microscopic structure of even tissue after being annealed.
Summary of the invention
The present invention is intended to provide quickly regulation deforms the annealing process of W material microstructure under a kind of low temperature, SPS skill is utilized
While art is heated directly to sample, using the DC pulse current for being passed through sample, the microscopic structure of deformation states W material is accelerated to drill
Become.By regulating and controlling SPS parameter and annealing, to realize to deformation W materials microstructure regulation.In addition, using by sample
Portion generates uniform current field, can obtain the W material of even tissue, solve prior heat treatment deformation W material grains it is coarse,
The problem of the uniform poor efficiency of tissue odds.
The present invention quickly regulates and controls the annealing process of deformation W material microstructure at low temperature, is by SPS technology come real
It is existing, the W material of different microstructures is obtained by regulation parameter and annealing.Specifically comprise the following steps:
Step 1: preparing the deformation W material sample that can be used for SPS annealing.Prepared using wire cutting and mechanical grinding technology
The smooth and parallel deformation states of upper and lower surfaces (present invention is using rolling than being 90%) W plate.Ready sample is placed in
Boiling is boiled 2~10min and is cleaned in 10wt.%NaOH aqueous solution, and dry 8~20h, is obtained in 50~100 DEG C of vacuum ovens
Obtain the deformation W material that can be made annealing treatment.
Step 2: under the conditions of SPS, deforming the annealing of W material.Deformation W material sample is mounted on SPS equipment
In graphite electrode pressure head, then anneal under the conditions of vacuum, DC pulse current.By changing heating when SPS annealing
Rate, annealing temperature and soaking time regulate and control W material microstructure to realize.
In step 2, in order to avoid deformation W material aoxidizes in annealing process, the vacuum degree of SPS equipment furnace chamber is less than
10Pa；In order to guarantee SPS graphite electrode and deformation W material have good contact, in annealing process plus load be 5~
100MPa。
In step 2, by heating rate, annealing temperature and the soaking time when changing SPS annealing to obtain acting on sample
Different current densities and action time on product.SPS annealing technological parameter adjustable range: heating rate be 10~300 DEG C/
Min, annealing temperature are 200~1000 DEG C, and soaking time is 0~10min.When annealing under corresponding condition, electric current tends to stablize
When by the current density range of sample be 300~1000A/cm2。
Step 3: after completing SPS heating and heat preservation, deformation W material sample is cooled down with furnace.
The total time of annealing process of the present invention≤60min.
The present invention is regulated and controled using microscopic structure of the SPS technology to deformation W material, is become with the deformation ratio of W material, processing
Shape mode is unrelated.This feature of SPS DC pulse current is mainly utilized, is on the one hand brought rapidly up using its Joule heat generated
Annealing temperature；On the other hand atom diffusion is promoted to fast implement Microstructures Evolvement using pulse current, to be expected to lower
At a temperature of realize to deformation W material microscopic structure carry out Effective Regulation.When heating rate is 100/min, pass through sample
Current density is 300~600Acm-2, when the time of the function of current is when within 2min, sample is replied；It is electric when extending
When the time of stream effect is to 6min, deformation W material is locally recrystallized；When further extending the function of current time to 8min,
Perfect recrystallization has occurred in sample；Meanwhile under identical sintering temperature, increases heating rate, can be improved and act on sample
Current density, and then accelerate the diffusion of atom, to accelerate sample recovery and recrystallization process.In addition, the DC pulse of SPS technology
Electric current uniformly acts in sample, thus can obtain uniform microscopic structure.Therefore, present invention can be implemented in right under low temperature
The microscopic structure of deformation W material is quickly regulated and controled.
Detailed description of the invention
Fig. 1 (a) is the metallographic microstructure of the pure W of rolling deformation state；Figure (b) is to be moved back using traditional approach in 1350 DEG C of isothermals
Metallographic microstructure after fiery 4h.It can be found that the crystal grain of deformation states W material is become by threadiness after traditional approach is annealed
Etc. shaft-like.
(a) when the pure W of Fig. 2 rolling deformation state heating rate under the conditions of SPS is 100 DEG C/min, annealing temperature is 200 DEG C
Microstructure after current density-time graph and (b) annealing.Compared with Fig. 1 (a), it can be found that 200 DEG C under the conditions of SPS
When annealing, there is no significantly changing for the microscopic structure of deformation W material.
(a) when the pure W of Fig. 3 rolling deformation state heating rate under the conditions of SPS is 100 DEG C/min, annealing temperature is 600 DEG C
Microstructure after current density-time graph and (b) annealing.It can be found that under the conditions of SPS 600 DEG C just have part deform W
Crystal grain recrystallizes.
(a) when the pure W of Fig. 4 rolling deformation state heating rate under the conditions of SPS is 200 DEG C/min, annealing temperature is 600 DEG C
Microstructure after current density-time graph and (b) annealing.Compared with Fig. 3, it can be found that at the identical temperature of SPS (600 DEG C)
Current density can be increased by improving heating rate, and the recrystal grain quantity that deformation W material occurs increases and to there is recrystallization abnormal long
Big phenomenon.
(a) when the pure W of Fig. 5 rolling deformation state heating rate under the conditions of SPS is 100 DEG C/min, annealing temperature is 800 DEG C
Microstructure and (b) XRD spectrum.It can be found that perfect recrystallization has occurred in deformation W material under the conditions of SPS at 800 DEG C, and
Even tissue.Compared with conventional anneal mode, as shown in Fig. 1 (b), annealing temperature is significantly reduced under the conditions of SPS, and the W obtained
The grain structure of material is relatively tiny and uniform.
Specific embodiment
Embodiment 1:
Using line cutting technology from rolling deformation is 13mm than cutting diameter on the deformation W plate for 90%, with a thickness of 2.8mm
Wafer sample.It is dry in 80 DEG C of vacuum ovens after 5min removal surface and oil contaminant is boiled in boiling in 10wt.%NaOH aqueous solution
12h obtains the W sample that can carry out SPS annealing.Sample after cleaning is mounted in the graphite electrode pressure head of SPS equipment,
Then it anneals under the conditions of vacuum, pulse current.When SPS anneals, vacuum degree is less than 10Pa, plus load 30MPa, rises
Warm rate is 100 DEG C/min, annealing temperature is 200 DEG C, soaking time 0min.Under corresponding condition, by the electric current of sample
300~600Acm of density-2(shown in such as Fig. 2 (a)), after annealing shown in its microscopic structure such as Fig. 2 (b).As can be seen that deformation W
Material at 200 DEG C SPS annealing conditions undertissue there is no significantly changing, illustrate within the short function of current time and
The diffusion for facilitating atom at lower temperature can promote the progress that deformation W material is replied.It can be found that sample adds from room temperature
Heat is to 200 DEG C, and in 300~600Acm-2Current density acted on 2min after, there is no significantly becoming for the tissue of sample
Change.
Embodiment 2:
Using line cutting technology from rolling deformation is 13mm than cutting diameter on the deformation W plate for 90%, with a thickness of 2.8mm
Wafer sample.It is dry in 80 DEG C of vacuum ovens after 5min removal surface and oil contaminant is boiled in boiling in 10wt.%NaOH aqueous solution
12h obtains the W sample that can carry out SPS annealing.Sample after cleaning is mounted in the graphite electrode pressure head of SPS equipment,
Then it anneals under the conditions of vacuum, pulse current.When SPS anneals, vacuum degree is less than 10Pa, plus load 30MPa, rises
Warm rate is 100 DEG C/min, annealing temperature is 600 DEG C, soaking time 0min.Under corresponding condition, by the electric current of sample
300~600Acm of density-2(shown in such as Fig. 3 (a)), after annealing shown in its microscopic structure such as Fig. 3 (b).It can be found that SPS item
Recrystallization takes place in deformation W material after the lower 600 DEG C of annealing of part.Compared to Fig. 2 it is believed that making in higher temperatures, high current density
Under, the Recrystallization nucleation of deformation W material is promoted.However, short function of current time and lower temperature are unfavorable for W crystal grain
Uniformly grow up, it will be seen that annealing the phenomenon that there are nonuniform organizations under the conditions of the SPS.In addition, 300~
600A·cm-2Current density under, when acting on that current time increases to 6min from 2min on sample, the highest that makes sample anneal
Temperature rises to 600 DEG C from 200 DEG C, and partial recrystallisation takes place in deformation W material.
Embodiment 3:
Using line cutting technology from rolling deformation is 13mm than cutting diameter on the deformation W plate for 90%, with a thickness of 2.8mm
Wafer sample.It is dry in 80 DEG C of vacuum ovens after 5min removal surface and oil contaminant is boiled in boiling in 10wt.%NaOH aqueous solution
12h obtains the W sample that can carry out SPS annealing.Sample after cleaning is mounted in the graphite electrode pressure head of SPS equipment,
Then it anneals under the conditions of vacuum, pulse current.When SPS anneals, vacuum degree is less than 10Pa, plus load 30MPa, rises
Warm rate is 200 DEG C/min, annealing temperature is 600 DEG C, soaking time 0min.Under corresponding condition, by the electric current of sample
300~1000Acm of density-2(shown in such as Fig. 4 (a)), after annealing shown in its microscopic structure such as Fig. 4 (b).Compared with Example 2,
Sample is heated to 600 DEG C with different heating rates, under the heating rate of 200 DEG C/min, improves the electric current by sample
Density shortens the function of current time (halving), deformation W material recrystal grain quantity increases and there are abnormal grain growths
Phenomenon.
Embodiment 4:
Using line cutting technology from rolling deformation is 13mm than cutting diameter on the deformation W plate for 90%, with a thickness of 2.8mm
Wafer sample.It is dry in 80 DEG C of vacuum ovens after 5min removal surface and oil contaminant is boiled in boiling in 10wt.%NaOH aqueous solution
12h obtains the W sample that can carry out SPS annealing.Sample after cleaning is mounted in the graphite electrode pressure head of SPS equipment,
Then it anneals under the conditions of vacuum, pulse current.When SPS anneals, vacuum degree is less than 10Pa, plus load 30MPa, rises
Warm rate is 100 DEG C/min, annealing temperature is 800 DEG C, soaking time 0min.Under corresponding condition, by the electric current of sample
300~600Acm of density-2, after annealing shown in its microscopic structure such as Fig. 5 (a).It can be found that under the conditions of SPS after 800 DEG C of annealing
It deforms the even grain size of W material, be about 20 μm.It finds in addition, being characterized by xrd, anneals under the conditions of 800 DEG C of SPS
Afterwards, texture orientation, which has occurred and that, substantially change (shown in such as Fig. 5 (b)), is changed into perfect recrystallization state by (211) of rolling state
(110).Compared with Example 2, sample is in 300~600Acm-2Current density under, act on the time of electric current on sample
Increase to 8min from 6min, the maximum temperature for making sample anneal rises to 800 DEG C from 200 DEG C, and perfect recrystallization occurs for sample.
Claims (8)
1. quickly regulation deforms the annealing process of tungsten material microstructure under a kind of low temperature, it is characterised in that:
Deformation W is heated using SPS technology, and the DC pulse current using effect on it, it is aobvious to accelerate deformation W material
Micro-assembly robot develops, and by changing SPS technological parameter, obtains the W material of different microstructures.
2. annealing process according to claim 1, it is characterised in that include the following steps:
The W plate for rolling state is cut by disk using wire cutting, keeps disk lower planes parallel by mechanical grinding, then by sample
It is placed in 10wt.%NaOH solution, 2~10min, cleaning sample are boiled in boiling；It is subsequently placed in 50~100 DEG C of vacuum ovens dry
8~20h；Sample is fitted into the SPS equipment using graphite as electrode, quickly heats up to lower temperature heat preservation under vacuum conditions
Furnace cooling after a period of time.
3. technique according to claim 2, it is characterised in that:
In annealing process, vacuum degree is less than 10Pa in SPS equipment furnace.
4. technique according to claim 2, it is characterised in that:
In annealing process, 5~100MPa of plus load.
5. technique according to claim 2, it is characterised in that:
Heating rate is 10~300 DEG C/min.
6. technique according to claim 2, it is characterised in that:
Annealing temperature is 200~1000 DEG C, and soaking time is 0~10min.
7. technique according to claim 2, it is characterised in that:
Anneal total time≤60min.
8. technique according to claim 2, it is characterised in that:
Under corresponding condition in annealing process, when electric current tends to stablize, the current density by sample is 300~1000A/
cm2。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114717496A (en) * | 2022-03-24 | 2022-07-08 | 太原理工大学 | Boeing hot rolling combined pulse current annealing method for titanium alloy plate |
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| CN102605307A (en) * | 2012-03-22 | 2012-07-25 | 西安理工大学 | Preparation method for tungsten copper alloy sheet |
| CN105296903A (en) * | 2015-10-29 | 2016-02-03 | 燕山大学 | High-pressure twisting-electric field assistant thermal treatment fine grain method for ZrTiAlV alloy |
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2019
- 2019-06-24 CN CN201910547049.1A patent/CN110205573A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605307A (en) * | 2012-03-22 | 2012-07-25 | 西安理工大学 | Preparation method for tungsten copper alloy sheet |
| CN105296903A (en) * | 2015-10-29 | 2016-02-03 | 燕山大学 | High-pressure twisting-electric field assistant thermal treatment fine grain method for ZrTiAlV alloy |
Non-Patent Citations (2)
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| XIAOQIANG LI ET AL.: "93W-5.6Ni-1.4Fe heavy alloys with enhanced permormance prepared by cyclic spark plasma sintering", 《MATERIALS SCIENCE AND ENGINEERING A》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114717496A (en) * | 2022-03-24 | 2022-07-08 | 太原理工大学 | Boeing hot rolling combined pulse current annealing method for titanium alloy plate |
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Application publication date: 20190906 |
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