CN106799500B - The preparation method of ultrafine tungsten powder - Google Patents
The preparation method of ultrafine tungsten powder Download PDFInfo
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- CN106799500B CN106799500B CN201710008006.7A CN201710008006A CN106799500B CN 106799500 B CN106799500 B CN 106799500B CN 201710008006 A CN201710008006 A CN 201710008006A CN 106799500 B CN106799500 B CN 106799500B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of preparation methods of ultrafine tungsten powder, and surfactant is dissolved in deionized water or distilled water obtained solution, ammonium paratungstate is added in solution；By HNO3Progress chemical precipitation reaction in above-mentioned solution is added under mechanical stirring and ultrasound condition, forms suspension；By dehydrated alcohol be added suspension in the reaction was continued, mechanical stirring and ultrasonic treatment are in working condition in entire reaction process and its revolving speed and power remain unchanged, and the suspension after reaction is filtered and uses washes of absolute alcohol sediment obtained；Kept the temperature at a lower temperature in tube furnace with pure hydrogen and carry out first step reduction, be then warming up to higher temperature and keep the temperature carry out second step restore to obtain ultrafine tungsten powder.The invention enables to the average grain size of tungsten powder reach 10~45nm, and grain size distribution has good uniformity.The high-densit tungsten-bast alloy of acquisition fine grain is sintered for postorder to lay a good foundation.
Description
Technical field
The invention proposes one kind apply in wet chemistry method surfactant and ultrasonic treatment come prepare it is ultra-fine (≤
50nm) the technology of tungsten powder belongs to powder preparation engineering technical field.
Background technique
Tungsten is widely used due to its higher fusing point (3410 DEG C) and excellent physical and chemical performance: as too
The part of empty airship and aeroengine, jet-vane control assembly, the precentrum of rocket, contact plunger, cooling fin etc..And by passing
It is difficult sintering densification when the tungsten powder of system powder metallurgy process sintering micron-scale, it usually needs very high sintering temperature and very long
Sintering time.And the activated sintering developed in recent years is then to improve the effective way of consistency, including addition activated metal is first
Plain (such as Fe, Ni, Cu) and use ultrafine tungsten powder.But it frequently can lead to the tight of alloy density by adding activated metal element
Decline again, which greatly limits the wide applications of such material.Therefore in order to obtain the tungsten of high-compactness at a lower temperature
Alloy, the method for unique feasible are exactly using ultra-fine tungsten powder.
The conventional method for preparing ultrafine tungsten powder specifically includes that (1) high-energy ball milling method (2) tungsten oxide hydrogen reduction method (3) colloidal sol-
Gel method (4) freeze-drying (5) cyclic oxidation reduction method (6) liquid chemical method.Although high-energy ball milling method is due to its low cost
With high yield by favor, but the technique cannot control the size, shape and distribution of powder well.Meanwhile ball-milling method
It also results in and introduces a large amount of defects in powder face structure, crystal structure occurs to destroy, introduce impurity element etc..And it is other
Method compares high-energy ball milling method, and the purity of the powder of preparation, partial size make moderate progress, and the shape of tungsten grain has also obtained well
Control.But the powder diameter of synthesis is still submicron-scale, and grain size distribution homogeneity is poor, still into
One step improves.
Surfactant is added in traditional liquid chemical method can make nucleus generate repulsion work with identical charges
With, it can be prevented further to reunite and grown up, play the role of refine crystal grain.In addition, the steric effect of surfactant makes
Originally affine nano grain surface separates, and prevents mutual reunion, provides to prepare evenly dispersed, fine grain precursor powder
It may.Meanwhile the use of surfactant can be such that the surface of crystal grain is modified, and can effectively control its surface topography.And surpass
The high temperature and high pressure environment that acoustic cavitation effect generates provides when energy goes that molecule is overcome to be formed for system from interface energy
Nucleation energy barrier surface potential barrier, so that nucleus generating rate improves several orders of magnitude；Meanwhile cavitation is generated in solid particles surface
A large amount of micro-bubbles can interfere the ordered arrangement of configurational ion, and nucleus is hindered further to grow up.In addition, the height that ultrasonic cavitation generates
The mechanical effects such as crushing, emulsification, the stirring that pressure shock wave and microjet play, can effectively prevent the life of nucleus within a certain period of time
Long and reunion, makes molecule be more evenly distributed.
For the above present Research, the invention proposes apply ultrasonic treatment and table on the basis of original liquid chemical method
Face activating agent prepares ultrafine tungsten powder.
Summary of the invention
The present invention prepares ultrafine tungsten powder by applying surfactant and ultrasonic treatment in wet-chemical reaction process.It should
The average grain size for the tungsten powder that technology enables to reaches 10~45nm, and grain size distribution has good uniformity.For
Postorder sintering obtains the high-densit tungsten-bast alloy of fine grain and lays a good foundation.
Specific technical solution is as follows:
A kind of preparation method of ultrafine tungsten powder, comprising the following steps:
(1) surfactant is dissolved in deionized water or distilled water, disperses it with mechanical stirring and ultrasonic treatment, is molten
Ammonium paratungstate (APT) is then added in the solution of preparation by solution, obtained solution；
It (2) is 65%~68%HNO by concentration3It is added under mechanical stirring and ultrasound condition in above-mentioned solution and carries out chemistry
Precipitation reaction forms suspension；
(3) dehydrated alcohol is added in suspension to the reaction was continued, mechanical stirring and ultrasonic treatment are equal in entire reaction process
In running order and its revolving speed and power remain unchanged, and the suspension after reaction is filtered and uses washes of absolute alcohol institute
The sediment of acquisition；
(4) obtained sediment is placed in drying in drying box to be placed in tube furnace, is forged in nitrogen or argon stream
Burning obtains tungsten oxide powder；
(5) in tube furnace with pure hydrogen at 580~650 DEG C, first step reductase 12~5h；Again at 700~800 DEG C,
Second step reductase 12~6h；Obtain ultrafine tungsten powder.
Surfactant selects one of the following: polyvinylpyrrolidone (PVP), dodecyl in the step (1)
Sodium sulphate (SDS).
The concentration of ammonium paratungstate in the solution in the step (1) are as follows: 0.08~0.33g/mL；The quality of surfactant
It is the 5%~15% of ammonium paratungstate quality.
Dense HNO in the step (2)3Volume be 0.25~1.17 times of deionized water or distilled water volume.
The time of chemical precipitation reaction in the step (2) are as follows: 20~60min.
The volume of addition dehydrated alcohol in the step (3) is 0.5~3 times of suspension total volume.
The time that the reaction was continued after addition dehydrated alcohol in the step (3) is 2~5h.
Churned mechanically revolving speed is 1000~5000rpm in the step, and the power of ultrasonic treatment is 100~400W.
450~500 DEG C of calcination temperature in the step (4)；Calcination time is 1~3h.
Advantages of the present invention:
1, compared with traditional wet chemistry method, sol-gel method, the tungsten prepared after surfactant and ultrasonic treatment is added
The size of the crystal grain of powder further refines, dimensional homogeneity is further optimized, shape also realizes accurate regulation.
2, the disadvantages of this method avoid high-energy ball milling methods to be easily introduced impurity, energy consumption is high, so that the purity of the tungsten powder of preparation
It is increased dramatically, good prospect is possessed in the preparation of superfine nano tungsten powder.
3, uniform, Ultra-fine Grained tungsten powder is prepared into using this method, obtains the high-densit tungsten base of fine grain for postorder sintering and closes
Gold is laid a good foundation.
Detailed description of the invention
Fig. 1: the SEM picture of the tungsten powder of preparation；
Fig. 2: the SEM picture of the tungsten powder of preparation；
Fig. 3: the TEM picture of the tungsten powder of preparation.
Specific embodiment
Feature of the invention is further described below by example, but the invention is not limited to following examples.
Embodiment 1
(1) 1gSDS is dissolved in 120mL distilled water, with mechanical stirring and ultrasonic treatment, (churned mechanically revolving speed is
1000rpm, after the power of ultrasonic treatment is the fully dispersed dissolution of 120W), by (APT's is dense in the solution of 10gAPT addition preparation
Degree is 0.08g/mL, and the quality of surfactant is the 10% of ammonium paratungstate quality).
(2) 140mL concentrated nitric acid (1.17 times of distilled water volume) is added to progress chemical precipitation reaction in above-mentioned solution,
It reacts and continues 30min, form suspension.
(3) entire anti-by 260mL dehydrated alcohol (1 times of the suspension total volume) 4h that is added in the suspension that the reaction was continued
Mechanical stirring and ultrasonic treatment are in working condition during answering and its revolving speed and power remain unchanged, then to suspension into
Row is filtered by vacuum and by the precipitating of acquisition with washes of absolute alcohol 3 times.
(4) precipitating after cleaning is put into drying 1 day in the vacuum oven that set temperature is 60 DEG C, then at 450 DEG C
1h is calcined in argon stream obtains tungsten oxide powder.
(5) tungsten oxide powder is carried out to two step reduction (600 DEG C of heat preservations 3h, 800 DEG C of heat preservation 6h) to obtain in hydrogen gas stream
To pure tungsten powder.Heating rate is 5 DEG C/min, throughput 100mL/min.Finally the powder is cooled in hydrogen atmosphere
Room temperature obtains even grain size, the pure tungsten powder that average grain size is 49.6nm, as shown in Figure 1.With conventional wet chemical with
The tungsten powder of mechanical alloying preparation is compared, and this method can effectively control the size and dimensional homogeneity of tungsten grain.
Embodiment 2
(1) 1gSDS is dissolved in 60mL distilled water, with mechanical stirring and ultrasonic treatment, (churned mechanically revolving speed is
2000rpm, after the power of ultrasonic treatment is the fully dispersed dissolution of 200W), by (APT's is dense in the solution of 10gAPT addition preparation
Degree is 0.17g/mL, and the quality of surfactant is the 10% of ammonium paratungstate quality).
(2) 60mL concentrated nitric acid (1 times of distilled water volume) is added to progress chemical precipitation reaction in above-mentioned solution, reaction
Continue 20min, forms suspension.
(3) entire anti-by 120mL dehydrated alcohol (1 times of the suspension total volume) 5h that is added in the suspension that the reaction was continued
Mechanical stirring and ultrasonic treatment are in working condition during answering and its revolving speed and power remain unchanged, then to suspension into
Row is filtered by vacuum and by the precipitating of acquisition with washes of absolute alcohol 3 times.
(4) precipitating after cleaning is put into drying 1 day in the vacuum oven that set temperature is 60 DEG C, then at 450 DEG C
2h is calcined in argon stream obtains tungsten oxide powder.
(5) tungsten oxide powder is carried out to two step reduction (580 DEG C of heat preservations 2h, 750 DEG C of heat preservation 5h) to obtain in hydrogen gas stream
To pure tungsten powder.Heating rate is 5 DEG C/min, throughput 100mL/min.Finally the powder is cooled in hydrogen atmosphere
Room temperature obtains even grain size, the pure tungsten powder that average grain size is 43.9nm, as shown in Figure 2.This method can be significant
The shortcomings that overcoming tradition machinery alloying to be easily introduced impurity when preparing tungsten powder, so that the purity of the tungsten powder of preparation substantially improves.
Embodiment 3
(1) 1gPVP (K12) is dissolved in 120mL distilled water, with mechanical stirring and ultrasonic treatment (churned mechanically revolving speed
For 1000rpm, after the power of ultrasonic treatment is the fully dispersed dissolution of 400W), 20gAPT is added in the solution of preparation (APT's
Concentration is 0.17g/mL, and the quality of surfactant is the 5% of ammonium paratungstate quality).
(2) 30mL concentrated nitric acid (0.25 times of distilled water volume) is added to progress chemical precipitation reaction in above-mentioned solution,
It reacts and continues 30min, form suspension.
(3) entire anti-by 450mL dehydrated alcohol (3 times of the suspension total volume) 4h that is added in the suspension that the reaction was continued
Mechanical stirring and ultrasonic treatment are in working condition during answering and its revolving speed and power remain unchanged, then to suspension into
Row is filtered by vacuum and by the precipitating of acquisition with washes of absolute alcohol 3 times.
(4) precipitating after cleaning is put into drying 1 day in the vacuum oven that set temperature is 60 DEG C, then at 500 DEG C
3h is calcined in argon stream obtains tungsten oxide powder.
(5) tungsten oxide powder is carried out to two step reduction (600 DEG C of heat preservations 3h, 800 DEG C of heat preservation 6h) to obtain in hydrogen gas stream
To pure tungsten powder.Heating rate is 5 DEG C/min, throughput 100mL/min.Finally the powder is cooled in hydrogen atmosphere
Room temperature obtains even grain size, the pure tungsten powder that average grain size is 13nm, as shown in Figure 3.This method can be controlled effectively
The pattern of tungsten grain processed is unified spherical shape.
Embodiment 4
(1) 6gSDS is dissolved in 120mL distilled water, with mechanical stirring and ultrasonic treatment, (churned mechanically revolving speed is
3000rpm, after the power of ultrasonic treatment is the fully dispersed dissolution of 300W), by (APT's is dense in the solution of 40gAPT addition preparation
Degree is 0.33g/mL, and the quality of surfactant is the 15% of ammonium paratungstate quality).
(2) 80mL concentrated nitric acid (0.67 times of distilled water volume) is added to progress chemical precipitation reaction in above-mentioned solution,
It reacts and continues 40min, form suspension.
(3) entire anti-by 200mL dehydrated alcohol (1 times of the suspension total volume) 4h that is added in the suspension that the reaction was continued
Mechanical stirring and ultrasonic treatment are in working condition during answering and its revolving speed and power remain unchanged, then to suspension into
Row is filtered by vacuum and by the precipitating of acquisition with washes of absolute alcohol 3 times.
(4) precipitating after cleaning is put into drying 1 day in the vacuum oven that set temperature is 60 DEG C, then at 480 DEG C
1h is calcined in argon stream obtains tungsten oxide powder.
(5) tungsten oxide powder is carried out to two step reduction (650 DEG C of heat preservations 5h, 800 DEG C of heat preservation 2h) to obtain in hydrogen gas stream
To pure tungsten powder.Heating rate is 5 DEG C/min, throughput 100mL/min.Finally the powder is cooled in hydrogen atmosphere
Room temperature obtains even grain size, the pure tungsten powder that average grain size is 40.3nm.
Embodiment 5
(1) 3gPVP (K17) is dissolved in 120mL distilled water, with mechanical stirring and ultrasonic treatment (churned mechanically revolving speed
For 5000rpm, after the power of ultrasonic treatment is the fully dispersed dissolution of 100W), 20gAPT is added in the solution of preparation (APT's
Concentration is 0.17g/mL, and the quality of surfactant is the 15% of ammonium paratungstate quality).
(2) 50mL concentrated nitric acid (0.42 times of distilled water volume) is added to progress chemical precipitation reaction in above-mentioned solution,
It reacts and continues 60min, form suspension.
(3) entire anti-by 85mL dehydrated alcohol (0.5 times of the suspension total volume) 2h that is added in the suspension that the reaction was continued
Mechanical stirring and ultrasonic treatment are in working condition during answering and its revolving speed and power remain unchanged, then to suspension into
Row is filtered by vacuum and by the precipitating of acquisition with washes of absolute alcohol 3 times.
(4) precipitating after cleaning is put into drying 1 day in the vacuum oven that set temperature is 60 DEG C, then at 480 DEG C
2h is calcined in argon stream obtains tungsten oxide powder.
(5) tungsten oxide powder is carried out to two step reduction (600 DEG C of heat preservations 3h, 700 DEG C of heat preservation 6h) to obtain in hydrogen gas stream
To pure tungsten powder.Heating rate is 5 DEG C/min, throughput 100mL/min.Finally the powder is cooled in hydrogen atmosphere
Room temperature obtains even grain size, the pure tungsten powder that average grain size is 10.9nm.
Claims (7)
1. a kind of preparation method of ultrafine tungsten powder, it is characterised in that the following steps are included:
(1) surfactant is dissolved in deionized water or distilled water, makes its dispersion, dissolution with mechanical stirring and ultrasonic treatment,
Then ammonium paratungstate is added in the solution of preparation by obtained solution；
It (2) is 65%~68%HNO by concentration3It is added under mechanical stirring and ultrasound condition in above-mentioned solution and carries out chemical precipitation
Reaction forms suspension；
(3) by dehydrated alcohol be added suspension in the reaction was continued, mechanical stirring and ultrasonic treatment are in entire reaction process
Working condition and its revolving speed and power remain unchanged, the suspension after reaction is filtered and is obtained with washes of absolute alcohol
Sediment；
(4) obtained sediment is placed in drying in drying box to be placed in tube furnace, is calcined in nitrogen or argon stream
To tungsten oxide powder；450~500 DEG C of calcination temperature；
(5) in tube furnace with pure hydrogen at 580~650 DEG C, first step reductase 12~5h；It is warming up to 700~800 DEG C again,
Second step reductase 12~6h；Obtain ultrafine tungsten powder；
Surfactant in the step 1 selects the one of lauryl sodium sulfate (SDS) or polyethylene pyrrole network alkanone (PVP)
Kind；
Dense HNO in the step 23Volume be 0.25~1.17 times of deionized water or the volume of distilled water in step 1.
2. according to the method described in claim 1, it is characterized in that the concentration of ammonium paratungstate in the solution in the step (1)
Are as follows: 0.08~0.33g/mL；The quality of surfactant is the 5%~15% of ammonium paratungstate quality.
3. according to the method described in claim 1, it is characterized in that the time that the chemical precipitation in the step (2) is reacted are as follows:
20~60min.
4. according to the method described in claim 1, it is characterized in that the volume of the addition dehydrated alcohol in the step (3) is outstanding
0.5~3 times of supernatant liquid total volume.
5. according to the method described in claim 1, it is characterized in that the reaction was continued after addition dehydrated alcohol in the step (3)
Time be 2~5h.
6. according to the method described in claim 1, it is characterized in that churned mechanically revolving speed 1000 in the step~
5000rpm, the power of ultrasonic treatment are 100~400W.
7. according to the method described in claim 1, it is characterized in that in the step (4)；Calcination time is 1~3h.
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| CN108705097B (en) * | 2018-06-25 | 2021-04-02 | 天津大学 | Preparation method of surfactant-added freeze-dried nano tungsten powder |
| CN108772569B (en) * | 2018-06-25 | 2021-03-16 | 天津大学 | Hydrothermal preparation method of superfine nano tungsten powder |
| CN116177604B (en) * | 2023-05-04 | 2023-07-21 | 崇义章源钨业股份有限公司 | Preparation process of uniform nano tungstic acid |
| CN116375090B (en) * | 2023-06-05 | 2023-09-01 | 赣州市海龙钨钼有限公司 | Preparation method of ammonium paratungstate |
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