CN106799490A - The method that the room temperature aqueous solution prepares three-dimensional bicontinuous structure nanoporous tungsten - Google Patents
The method that the room temperature aqueous solution prepares three-dimensional bicontinuous structure nanoporous tungsten Download PDFInfo
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Abstract
The method that the room temperature aqueous solution prepares three-dimensional bicontinuous structure nanoporous tungsten, belongs to de- alloying and prepares nano porous metal field.The molar fraction of aluminium is weighed into tungsten powder and aluminium powder adds the stearic acid to carry out high-energy ball milling as process control agent for 70% 90%, wherein stearic addition is the 0.5 1.5% of ball-milled powder gross mass, abrading-ball is 20 40 with powder quality ratio：1, drum's speed of rotation is 300 600r/min, and Ball-milling Time is 20 30h, obtains tungsten aluminium alloy powder；Prepared tungsten aluminium alloy powder is placed in carries out the de- 25h of alloying 15 in the aqueous solution of 0.5 1M of deoxygenation acid or alkali, after being cleaned and dried through ultra-pure water and ethanol, obtain the nanoporous tungsten with three-dimensional bicontinuous structure.High temperature present invention, avoiding liquid metal is to the roughening of loose structure effect.
Description
Technical field
The nanoporous with three-dimensional bicontinuous structure feature are prepared in room temperature aqueous environment the present invention relates to a kind of
The method of tungsten, belongs to de- alloying and prepares nano porous metal field.
Background technology
Nano porous metal due to specific surface area it is big, avtive spot is more the features such as and be widely used in energy and deposit
The fields such as storage, catalysis and sensing.De- alloying process is to prepare one of conventional method of nano porous metal material at present.The party
The principle of method is, using difference in Electrode Potential larger between foundry alloy constituent element, alloy optionally to be removed in certain corrosive medium
The more active composition of middle chemical property, and remaining inert fraction forms (tough with three-dimensional co-continuous by way of self assembly
Band and duct are continuous) nano-porous structure.Receiving for the metals such as gold, platinum, palladium and copper is successfully prepared by the technology
Rice loose structure.The characteristics of refractory metal has high-melting-point and high intensity, has wide as the structure member under high-temperature service
General application prospect.In order to extend category and the application of nano porous metal, Recent study person are devoted to exploitation and prepare hardly possible
The new technology of molten metal nano loose structure.A kind of de- alloying process of new liquid metal, this method have been developed at present
Using motlten metal as alloy media is removed, de- conjunction is realized using the intermiscibility different in the molten metal of different component in alloy
Golden process.But because the technology is carried out in high temperature fluent metal, inevitably there is institutional framework roughening, be unfavorable for obtaining
Nanostructured is obtained, the characteristic size of the porous niobium prepared by the technology is 170-400nm.It can be seen from above present Research,
Obtain characteristic size and the technical barrier for being badly in need of solving is still in the refractory metal loose structure of nanoscale.
Regarding to the issue above, present inventor is water-soluble by mechanical alloying and room temperature by taking refractory metals tungsten as an example
De- alloying process in pendular ring border, develops a kind of side for preparing the nanoporous tungsten with three-dimensional bicontinuous structure feature
Method, the method is simple to operate, be easy to industrialized production, and prepared POROUS TUNGSTEN particle size can be controlled in below 100nm.
The content of the invention
The present invention is proposed for the problem that the nanoporous tungsten with three-dimensional bicontinuous structure feature is faced is prepared at present
Using mechanical alloying and in room temperature aqueous environment, chemistry takes off the solution technology that alloying is combined.
The method that the room temperature aqueous solution prepares three-dimensional bicontinuous structure nanoporous tungsten, comprises the following steps：
(1) by the molar fraction of aluminium for 70%-90% weighs tungsten powder and aluminium powder, and stearic acid is added as process control agent
High-energy ball milling is carried out, wherein stearic addition is the 0.5-1.5% of ball-milled powder gross mass, abrading-ball is with powder quality ratio
20-40：1, drum's speed of rotation is 300-600r/min, and Ball-milling Time is 20-30h, obtains tungsten aluminium alloy powder；
(2) by prepared tungsten aluminium alloy powder be placed in deoxygenation 0.5-1M acid (acid preferably is selected from sulfuric acid, hydrochloric acid and hydrogen fluorine
Acid) or the aqueous solution of alkali (the preferred NaOH of alkali) in carry out de- alloying 15-25h, after being cleaned and dried through ultra-pure water and ethanol,
Obtain the nanoporous tungsten with three-dimensional bicontinuous structure feature.
Compared with the de- alloy of existing liquid metal prepares the method for nanoporous refractory metal, advantage of the invention exists
In：De- alloy process is carried out in the room temperature aqueous solution, it is to avoid roughening effect of the high temperature of liquid metal to loose structure, therefore
Porous tungsten structure of the particle size in nanoscale is obtained in that, POROUS TUNGSTEN particle size can be controlled in below 100nm.
Brief description of the drawings
The phase transition process of different ball milling stage tungsten aluminium alloy powders in Fig. 1 embodiments 1
The microstructure of the final tungsten aluminium alloy powder for obtaining in Fig. 2 embodiments 1
The microstructure of the nanoporous tungsten powder obtained in Fig. 3 embodiments 1
The microstructure of the nanoporous tungsten powder obtained in Fig. 4 embodiments 2
The microstructure of the nanoporous tungsten powder obtained in Fig. 5 embodiments 3
The microstructure of (b) powder after (a) and de- alloy before alloy is taken off in Fig. 6 comparative examples 1.
Specific embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1：
By 1：4 mol ratio weighs 3.1507g tungsten powders, 1.8493g aluminium powders and 0.05g stearic acid and carries out high-energy ball milling, mill
Ball is 20 with powder quality ratio：1, drum's speed of rotation is 600r/min, and Ball-milling Time is 30h, obtains single-phase tungsten aluminium alloy powder,
The X-ray diffraction result of different ball milling stage powder is shown in Fig. 1, microstructure such as Fig. 2 institutes of the final tungsten aluminium alloy powder for obtaining
Show.High-purity argon gas are passed through in the beaker equipped with 1M sulfuric acid solutions after 10min, being put into tungsten aluminium alloy powder, to carry out de- alloy anti-
Should, continue logical argon gas 10min, it is ensured that the oxygen in solution is thoroughly removed, and beaker mouthful is sealed with sealed membrane.Alloy reaction to be taken off
After carrying out 15h, with ultra-pure water and ethanol be respectively washed 3 times with suction filtration mode and collect powder sample, that is, obtain have it is three-dimensional double
The nanoporous tungsten powder of continuous structure feature, its microstructure is as shown in Figure 3.
Embodiment 2：
Tungsten powder and aluminium powder are weighed for 70% by the molar fraction of aluminium, add the stearic acid that mass fraction is 1.5% as mistake
Program control preparation carries out high-energy ball milling, and abrading-ball is 40 with powder quality ratio：1, drum's speed of rotation is 300r/min, and Ball-milling Time is
20h, obtains tungsten aluminium alloy powder.High-purity argon gas are passed through in the beaker equipped with 1M hydrochloric acid solutions after 15min, partinium is put into
Powder carries out de- alloy reaction, continues logical argon gas 10min, is sealed beaker mouthful with sealed membrane.Alloy reaction to be taken off carries out 25h
Afterwards, with ultra-pure water and ethanol 3 times are respectively washed with suction filtration mode and collect powder sample, the micro- shape of the nanoporous tungsten of acquisition
Looks are as shown in Figure 4.
Embodiment 3：
Tungsten powder and aluminium powder are weighed for 90% by the molar fraction of aluminium, add the stearic acid that mass fraction is 0.5% as mistake
Program control preparation carries out high-energy ball milling, and abrading-ball is 30 with powder quality ratio：1, drum's speed of rotation is 500r/min, and Ball-milling Time is
25h, obtains tungsten aluminium alloy powder.High-purity argon gas are passed through in the beaker equipped with 0.5M sodium hydroxide solutions after 10min, tungsten is put into
Al alloy powder carries out de- alloy reaction, continues logical argon gas 10min, is sealed beaker mouthful with sealed membrane.Alloy to be taken off react into
After row 20h, with ultra-pure water and ethanol it is respectively washed 3 times with suction filtration mode and collects powder sample, the nanoporous tungsten of acquisition
Microstructure is as shown in Figure 5.
Comparative example 1：
Tungsten powder and aluminium powder are weighed for 50% by the molar fraction of aluminium, and the stearic acid for adding mass fraction to be 1% carries out high energy
Ball milling, abrading-ball is 20 with powder quality ratio：1, drum's speed of rotation is 600r/min, and Ball-milling Time is 30h, obtains single-phase tungsten aluminium and closes
Bronze end.High-purity argon gas are passed through in the beaker equipped with 1M sulfuric acid solutions after 10min, being put into tungsten aluminium alloy powder carries out de- alloy
Reaction, continues logical argon gas 10min, is sealed beaker mouthful with sealed membrane.After de- alloy reaction carry out 20h after, with suction filtration mode with
Ultra-pure water and ethanol are respectively washed 3 times and collect powder sample.There is no substantially change in the sample topography before and after de- alloy,
Nano-porous structure can not be obtained, as shown in Figure 6.
Comparative example 2：
Tungsten powder and aluminium powder are weighed for 50% by the molar fraction of aluminium, and the stearic acid for adding mass fraction to be 1% carries out high energy
Ball milling, abrading-ball is 30 with powder quality ratio：1, drum's speed of rotation is 500r/min, and Ball-milling Time is 20h, obtains single-phase tungsten aluminium and closes
Bronze end.High-purity argon gas are passed through in the beaker equipped with 1M sodium hydroxide solutions after 10min, tungsten aluminium alloy powder are put into and are taken off
Alloy reacts, and continues logical argon gas 10min, is sealed beaker mouthful with sealed membrane.After the reaction of de- alloy carries out 25h, suction filtration side is used
Formula is respectively washed 3 times and collects powder sample with ultra-pure water and ethanol.Sample topography before and after de- alloy does not occur substantially
Change, it is impossible to obtain nano-porous structure.
Claims (4)
1. a kind of method that room temperature aqueous solution prepares three-dimensional bicontinuous structure nanoporous tungsten, it is characterised in that including following step
Suddenly：
(1) by the molar fraction of aluminium for 70%-90% weighs tungsten powder and aluminium powder, and the stearic acid is added to be carried out as process control agent
High-energy ball milling, wherein 0.5-1.5% of the stearic addition for ball-milled powder gross mass, abrading-ball is 20- with powder quality ratio
40：1, drum's speed of rotation is 300-600r/min, and Ball-milling Time is 20-30h, obtains tungsten aluminium alloy powder；
(2) prepared tungsten aluminium alloy powder is placed in the aqueous solution of the 0.5-1M of deoxygenation acid or alkali carries out de- alloying 15-
25h, after being cleaned and dried through ultra-pure water and ethanol, obtains the nanoporous tungsten with three-dimensional bicontinuous structure feature.
2. the method that three-dimensional bicontinuous structure nanoporous tungsten is prepared according to a kind of room temperature aqueous solution described in claim 1, its
It is characterised by, acid is selected from sulfuric acid, hydrochloric acid and hydrofluoric acid.
3. the method that three-dimensional bicontinuous structure nanoporous tungsten is prepared according to a kind of room temperature aqueous solution described in claim 1, its
It is characterised by, alkali is NaOH.
4. a kind of three-dimensional bicontinuous structure nanoporous tungsten for being prepared according to the method described in claim any one of 1-3,
Characterized in that, POROUS TUNGSTEN particle size is in below 100nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107433328A (en) * | 2017-09-21 | 2017-12-05 | 上海交通大学 | A kind of flake copper for carrying nanometer copper crystal and preparation method thereof |
| CN107790733A (en) * | 2017-11-10 | 2018-03-13 | 上海交通大学 | A kind of copper nanoparticle and preparation method thereof |
| CN107983963A (en) * | 2017-11-30 | 2018-05-04 | 北京工业大学 | A kind of low temperature preparation method of pure W-Cu nanocomposite powder |
| CN111020329A (en) * | 2019-11-22 | 2020-04-17 | 武汉理工大学 | Method for preparing porous tungsten material based on W-Fe-C system corrosion method |
| CN113333748A (en) * | 2021-05-10 | 2021-09-03 | 武汉理工大学 | Two-stage pore porous tungsten and preparation method thereof |
| CN113458393A (en) * | 2021-06-16 | 2021-10-01 | 中国科学院金属研究所 | Construction method of block nano porous metal |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107433328A (en) * | 2017-09-21 | 2017-12-05 | 上海交通大学 | A kind of flake copper for carrying nanometer copper crystal and preparation method thereof |
| CN107790733A (en) * | 2017-11-10 | 2018-03-13 | 上海交通大学 | A kind of copper nanoparticle and preparation method thereof |
| CN107983963A (en) * | 2017-11-30 | 2018-05-04 | 北京工业大学 | A kind of low temperature preparation method of pure W-Cu nanocomposite powder |
| CN107983963B (en) * | 2017-11-30 | 2020-04-03 | 北京工业大学 | Low-temperature preparation method of pure nano W-Cu composite powder |
| CN111020329A (en) * | 2019-11-22 | 2020-04-17 | 武汉理工大学 | Method for preparing porous tungsten material based on W-Fe-C system corrosion method |
| CN113333748A (en) * | 2021-05-10 | 2021-09-03 | 武汉理工大学 | Two-stage pore porous tungsten and preparation method thereof |
| CN113458393A (en) * | 2021-06-16 | 2021-10-01 | 中国科学院金属研究所 | Construction method of block nano porous metal |
| CN113458393B (en) * | 2021-06-16 | 2022-09-13 | 中国科学院金属研究所 | Construction method of block nano porous metal |
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Effective date of registration: 20210204 Address after: No. 300, kejingshe, Haicang District, Xiamen City, Fujian Province, 361000 Patentee after: XIAMEN TUNGSTEN Co.,Ltd. Address before: 100124 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |