CN104028780A - Preparation method of amorphous nickel nanometer particles - Google Patents
Preparation method of amorphous nickel nanometer particles Download PDFInfo
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- CN104028780A CN104028780A CN201410053723.8A CN201410053723A CN104028780A CN 104028780 A CN104028780 A CN 104028780A CN 201410053723 A CN201410053723 A CN 201410053723A CN 104028780 A CN104028780 A CN 104028780A
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- ethyl alcohol
- absolute ethyl
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 165
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 title abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000006185 dispersion Substances 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 27
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002608 ionic liquid Substances 0.000 claims abstract description 20
- 238000001291 vacuum drying Methods 0.000 claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims description 52
- 239000008367 deionised water Substances 0.000 claims description 44
- 229910021641 deionized water Inorganic materials 0.000 claims description 44
- 239000013049 sediment Substances 0.000 claims description 42
- 239000002244 precipitate Substances 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 239000006228 supernatant Substances 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 24
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 16
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000376 reactant Substances 0.000 claims description 14
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract 2
- 238000002242 deionisation method Methods 0.000 abstract 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract 1
- 238000010668 complexation reaction Methods 0.000 abstract 1
- 230000036571 hydration Effects 0.000 abstract 1
- 238000006703 hydration reaction Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910001453 nickel ion Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 14
- 238000013019 agitation Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 239000002086 nanomaterial Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000004064 cosurfactant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of amorphous nickel nanometer particles which are good in dispersion performance. The preparation method of the amorphous nickel nanometer particles includes: firstly, replacing deionization water with absolute ethyl alcohol for dissolving a nickel resource, and then replacing a traditional surface active agent with [BMIN] BF4 ionic liquid; firstly, adding hydration hydrazine water solution so as to perform complexation on nickel ions after homogeneous mixing, and then using NaBH4 in stirring reduction so as to prepare the amorphous nickel nanometer particles which are good in dispersion performance; using the deionization water and the absolute ethyl alcohol to clear salt and other substances in a reaction system; performing centrifugal separation on the obtained nickel nanometer particles and placing the nickel nanometer particles in a vacuum drying oven for vacuum drying so as to obtain the nickel nanometer particles which are good in dispersion performance. According to the preparation method of the amorphous nickel nanometer particles, raw materials are easy to obtain, and low in cost, and the obtained amorphous nickel nanometer particles have the good dispersion performance.
Description
(1) technical field
The present invention relates to a kind of preparation method of nano material, is a kind of preparation method with the amorphous nickel nano particle of good dispersion specifically.
(2) background technology
Because nano material has special performance different and common material, more and more receive people's concern.Nanometer technology is as a kind of emerge science technology most with market application potential, and its potential importance is unquestionable.
Nickel nano material has the feature of the nano materials such as size is little, surface energy is high, specific area is large; and there is good electric conductivity and magnetic, be widely used in the numerous areas such as national defense industry, chemical industry, environmental protection, space flight and aviation, catalysis, magnetic recording material, carbide alloy and powder metallurgy.The method of preparing at present nickel nano particle mainly contains sol-gal process, electrochemical deposition method, chemical vapour deposition technique, hydrothermal reduction method, microemulsion method, chemical reduction method etc.Sol-gal process prepares that nickel nano particle purity is higher, good uniformity, particle are tiny, but owing to needing high temperature to remove impurity in preparation process, even need protection air-flow and reduction air-flow, preparation is rather complicated; Nickel nano particle purity prepared by electrochemical deposition method is high, form is even, but preparation method is complicated, cost compared with high, compared with the existing certain bearing capacity of difficult acquisition, be easily removed again and the template of pollution products not; It is higher that chemical deposition is prepared nickel nano particle cost, and operating difficulties; Hydrothermal reduction legal system for nickel nano particle owing to being to carry out in autoclave, so higher to equipment requirement, cause high expensive; Nickel nano particle particle diameter prepared by microemulsion method is little, and monodispersity is good, but surfactant, cosurfactant and the oils introduced will clean repeatedly with organic solvent, and easy-clear not; Chemical preparation nickel nano particle is simple to operate, mild condition, pollution less, be convenient to large-scale production, but product bad dispersibility.
(3) summary of the invention
Object of the present invention is for solving technical problem in above-mentioned preparation, and a kind of method of preparing the nickel nano particle with good dispersion is provided, and has advantages of simple, the with low cost and easy operating of technique.
The present invention is the deficiency solving the problems of the technologies described above, and the technical scheme adopting is: a kind of preparation method with the nickel nano particle of good dispersion, and its preparation method carries out as follows:
(1) prepare nickel nano particle
(1-1) get absolute ethyl alcohol and transfer in reaction vessel, in absolute ethyl alcohol, pass into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, make the molal volume concentration of nickel chloride between 0.01mol/L～0.1mol/L, then add [BMIN] BF
4ionic liquid, as dispersant, stirs, and makes nickel source dispersion soln, standby, described absolute ethyl alcohol and [BMIN] BF
4the volume ratio of ionic liquid is 100:2～14, preferably absolute ethyl alcohol and [BMIN] BF
4the volume ratio of ionic liquid is 100:6～10;
(1-3) weigh a certain amount of sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under stirring, to dripping volumetric concentration in the dispersion soln of nickel source, it is 20%～25% hydrazine hydrate aqueous solution complex ni-ion, add while stirring again sodium borohydride aqueous solution, be stirred to and generate after black precipitate, continue to stir 1～24 hour, obtain reactant liquor, absolute ethyl alcohol in described step (1-2) and the volume ratio of hydrazine hydrate aqueous solution are 100:1～10, preferably the absolute ethyl alcohol in described step (1-2) and the volume ratio of hydrazine hydrate aqueous solution are 100:1～6, absolute ethyl alcohol in described step (1-2) and the volume ratio of sodium borohydride aqueous solution are 100:5～15, preferably the absolute ethyl alcohol in described step (1-2) and the volume ratio of sodium borohydride aqueous solution are 100:5～10.
(2) clean amorphous nickel nano particle:
(2-1) reactant liquor step (1-4) being obtained carries out centrifugal, is precipitated thing A and supernatant liquor A, pours out supernatant liquor A, and sediment A is standby.
(2-2) 1:4～9 taking precipitate A and deionized water by volume, in sediment A, add deionized water, by deionized water, sediment A is washed, then put into centrifuge and carry out centrifugally, be precipitated thing B and supernatant liquor B, supernatant liquor B is poured out, sediment B is standby, 1:4～9 taking precipitate B and deionized water repeating step (2-2) by volume, washing precipitate B tri-to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4～9 taking precipitate C and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) sediment D of step (2-3) (containing a small amount of absolute ethyl alcohol) is put into vacuum drying chamber, at 10～100 pascal pressures, 80～90 ℃, vacuum drying chamber is 24～48 hours, remove moisture and absolute ethyl alcohol in sediment, obtain finished product amorphous nickel nano particle.
Further, the stirring described in described step (1-2) is to open mixer, with the speed of 100～200 revs/min, stirs 10 minutes.
Further again, centrifugal described in described step (2-1) is under the condition of 1000～2000 revs/min centrifugal 10～20 minutes.
Further, centrifugal described in described step (2-2) is under the condition of 1000～2000 revs/min centrifugal 10～20 minutes.
Described step (2-1) at the middle and upper levels clear liquid A and step (2-2) at the middle and upper levels clear liquid B after reclaiming, adopt the way of distillation to reclaim ethanol and distilled water, by the ethanol obtaining for producing again.
Described nickel nano particle is non crystalline structure, and the nickel nano particle particle diameter of conventionally preparing by the inventive method is 30～50nm, and crystal grain is little, good dispersion.
Compared with prior art, adopting nickel chloride is nickel source in the present invention, and because nickel chloride belongs to general commercial goods, it is convenient, cheap to buy, and simple in production process operation, and low production cost does not produce and pollutes environment, is beneficial to environmental protection.
In technique of the present invention, use absolute ethyl alcohol, for deionized water as solvent, has reduced the polarity of solution to a certain extent, is conducive to the dispersion of nano particle.
In technique of the present invention, adopt [BMIN] BF
4ionic liquid is as template and dispersant, [BMIN] BF
4adding of ionic liquid existingly impels synthetic nano material to have better dispersiveness, and this ionic liquid physical efficiency in the cleaning in later stage by removing completely in the cleaning repeatedly of deionized water and absolute ethyl alcohol.
The present invention utilizes [BMIN] BF
4the difference of ionic liquid addition, can prepare different big or small nano nickel particles, with respect to prior art, and amorphous nickel nano particle good dispersion of the present invention.
The inventive method is simple, and device therefor is simple, and operating condition is easy to grasp, and is convenient to large-scale production, does not need high temperature roast simultaneously in preparation process, saves the energy, reduces costs.
(4) accompanying drawing explanation
The nickel nano particle XRD figure that Fig. 1: embodiment bis-(absolute ethyl alcohol and ionic liquid volume ratio are 100:6) makes.
Fig. 2: embodiment bis-(absolute ethyl alcohol and ionic liquid volume ratio are 100:6) makes
Nickel nano particle SAED figure.
The nickel nano particle TEM figure that Fig. 3: embodiment bis-(absolute ethyl alcohol and ionic liquid volume ratio are 100:6) makes.
(5) specific embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Prepare a nickel nano particle preparation method with good dispersion, the step of its preparation method is as follows:
(1) prepare nickel nano particle
(1-1) absolute ethyl alcohol of getting 30～50mL is transferred in reaction vessel, in absolute ethyl alcohol, passes into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, make the molal volume concentration of nickel chloride between 0.01mol/L～0.1mol/L, then add [BMIN] BF
4ionic liquid, as dispersant, is opened mechanical agitation, with the rotating speed of 100-200 rev/min, stirs 10 minutes, makes nickel source dispersion soln, standby, described absolute ethyl alcohol and [BMIN] BF
4the volume ratio of ionic liquid is 100:2～14.
(1-3) weigh a certain amount of sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under mechanical agitation state, to dripping volumetric concentration in the dispersion soln of nickel source, it is 20%～25% hydrazine hydrate aqueous solution complex ni-ion, measure while stirring again the sodium borohydride aqueous solution of 5～10mL in the solution of nickel source, be stirred to and generate after black precipitate, continue to stir 1～24 hour to obtain reactant liquor, described absolute ethyl alcohol and the volume ratio of hydrazine hydrate aqueous solution are 100:1～10, and described absolute ethyl alcohol and the volume ratio of sodium borohydride aqueous solution are 100:5～15.。
(2) clean amorphous nickel nano particle:
(2-1) step (1-4) is made to reactant liquor and pour in centrifuge tube, put into centrifuge, with the rotating speeds of 1000～2000 revs/min centrifugal 10～20 minutes, be precipitated thing A and supernatant liquor A, pour out supernatant liquor A, sediment A is standby.
(2-2) 1:4～9 taking precipitate A and deionized water by volume, in sediment, add deionized water, by deionized water, to sediment washing 5～10 minutes, then put into centrifuge, with the rotating speeds of 1000～2000 revs/min centrifugal 10～20 minutes, be precipitated thing and supernatant liquor B, supernatant liquor B is poured out, and sediment B is standby, by volume 1:4～9 taking precipitate B and deionized water, repeating step (2-2) washing three to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4～9 taking precipitate C and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) sediment D that contains a small amount of absolute ethyl alcohol of step (2-3) is put into vacuum drying chamber, at 10～100 pascal pressures, 80～90 ℃, vacuum drying chamber is 24～48 hours, remove moisture and absolute ethyl alcohol in sediment, obtain finished product amorphous nickel nano particle.
Embodiment mono-
A preparation method with the nickel nano particle of good dispersion, the step of its preparation method is:
(1) prepare nickel nano particle
(1-1) ethanol solution that measures 50mL is transferred in reaction vessel, in absolute ethyl alcohol, passes into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, the molal volume concentration that makes nickel chloride is 0.01mol/L, then adds [BMIN] BF of 1mL
4ionic liquid, as dispersant, is opened mechanical agitation, with the rotating speeds of 100 revs/min, stirs 10 minutes, makes nickel source dispersion soln, standby.
(1-3) weigh sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under mechanical agitation state, to the volumetric concentration that drips 1mL in the dispersion soln of nickel source, it is 20% hydrazine hydrate complex ni-ion, the sodium borohydride aqueous solution that measures while stirring again 5mL joins in the solution of nickel source, is stirred to and generates after black precipitate, continues to stir 2 hours to obtain reactant liquor.
(2) clean amorphous nickel nano particle:
(2-1) the described reactant liquor of step (1-4) is poured in centrifuge tube, put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing A and supernatant liquor A, pour out supernatant liquor A, sediment A is standby.
(2-2) 1:4 taking precipitate A and deionized water by volume, in sediment, add deionized water, utilize deionized water to sediment A washing 10 minutes, then put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing and supernatant liquor B, supernatant liquor B is poured out, sediment B is standby, and 1:4 taking precipitate B and deionized water repeating step (2-2) washing by volume three to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4 taking precipitate C and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) step (2-3) is obtained the sediment D that contains a small amount of absolute ethyl alcohol put into vacuum drying chamber, at 10 pascal pressures, 80 ℃, vacuum drying chamber is 24 hours, removes moisture and absolute ethyl alcohol in sediment, obtains finished product amorphous nickel nano particle.
Embodiment bis-
A preparation method with the nickel nano particle of good dispersion, the step of its preparation method is:
(1) prepare nickel nano particle
(1-1) ethanol solution that measures 50mL is transferred in reaction vessel, in absolute ethyl alcohol, passes into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, the molal volume concentration that makes nickel chloride is 0.05mol/L, then adds [BMIN] BF of 3mL
4ionic liquid, as dispersant, is opened mechanical agitation, with the rotating speeds of 100 revs/min, stirs 10 minutes, makes nickel source dispersion soln, standby.
(1-3) weigh sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under mechanical agitation state, to dripping 3mL volumetric concentration in the dispersion soln of nickel source, it is 25% hydrazine hydrate complex ni-ion, the sodium borohydride aqueous solution that measures while stirring again 7mL joins in the solution of nickel source, is stirred to and generates after black precipitate, continues to stir 12 hours to obtain reactant liquor.
(2) clean amorphous nickel nano particle:
(2-1) step (1-4) is obtained to reactant liquor and pour in centrifuge tube, put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing A and supernatant liquor A, pour out supernatant liquor A, sediment A is standby.
(2-2) 1:4 taking precipitate A and deionized water by volume, in sediment, add deionized water, by deionized water, to sediment A washing 10 minutes, then put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing B and supernatant liquor B, supernatant liquor B is poured out, and sediment B is standby, by volume 1:4 taking precipitate B and deionized water, repeating step (2-2) washing three to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4 taking precipitate C and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) sediment D that contains a small amount of absolute ethyl alcohol step (2-3) being obtained is put into vacuum drying chamber, at 10 pascal pressures, 80 ℃, vacuum drying chamber is 24 hours, remove moisture and absolute ethyl alcohol in sediment, obtain finished product amorphous nickel nano particle, XRD figure is shown in Fig. 1, SAED figure is shown in Fig. 2, and TEM figure is shown in Fig. 3.
Embodiment tri-
A preparation method with the nickel nano particle of good dispersion, the step of its preparation method is:
(1) prepare nickel nano particle
(1-1) ethanol solution that measures 50mL is transferred in reaction vessel, in absolute ethyl alcohol, passes into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, the molal volume concentration that makes nickel chloride is 0.1mol/L, then adds [BMIN] BF of 5mL
4ionic liquid, as dispersant, is opened mechanical agitation, with the rotating speeds of 200 revs/min, stirs 10 minutes, makes nickel source dispersion soln, standby.
(1-3) weigh sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under mechanical agitation state, to the volumetric concentration that drips 5mL in the dispersion soln of nickel source, it is 23% hydrazine hydrate aqueous solution complex ni-ion, the sodium borohydride aqueous solution that measures while stirring again 7.5mL joins in the solution of nickel source, be stirred to and generate after black precipitate, continue to stir 1 hour, obtain reactant liquor.
(2) clean amorphous nickel nano particle:
(2-1) by (1-4) reactant liquor is poured in centrifuge tube, put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 20 minutes, be precipitated thing A and supernatant liquor A, pour out supernatant liquor A, sediment A is standby.
(2-2) 1:4 taking precipitate A and deionized water by volume, in sediment A, add deionized water, by deionized water, sediment A is washed 10 minutes, then put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing B and supernatant liquor B, supernatant liquor B is poured out, sediment B is standby, and 1:4 taking precipitate B and deionized water repeating step (2-2) washing by volume three to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4 taking precipitate C and absolute ethyl alcohol by volume, repeating step (2-2) washing three to four times, is precipitated thing D;
(3) sediment D that contains a small amount of absolute ethyl alcohol of step (2-3) is put into vacuum drying chamber, at 10 pascal pressures, 80 ℃, vacuum drying chamber is 24 hours, removes moisture and absolute ethyl alcohol in sediment, obtains finished product amorphous nickel nano particle.
Embodiment tetra-
A preparation method with the nickel nano particle of good dispersion, the step of its preparation method is:
(1) prepare nickel nano particle
(1-1) ethanol solution that measures 50mL is transferred in reaction vessel, in absolute ethyl alcohol, passes into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, the molal volume concentration that makes nickel chloride is 0.1mol/L, then adds [BMIN] BF of 7mL
4ionic liquid, as dispersant, is opened mechanical agitation, with the rotating speeds of 100 revs/min, stirs 10 minutes, makes nickel source dispersion soln, standby.
(1-3) weigh sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby.
(1-4) under mechanical agitation state, to nickel source dispersion soln, drip the hydrazine hydrate aqueous solution complex ni-ion that 5mL volumetric concentration is 20%, then the sodium borohydride aqueous solution that measures while stirring 7mL joins in the solution of nickel source, be stirred to and generate after black precipitate, continue to stir 1 hour, obtain reactant liquor.
(2) clean amorphous nickel nano particle:
(2-1) step (1-4) is obtained to reactant liquor and pour in centrifuge tube, put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing A and supernatant liquor A, pour out supernatant liquor A, sediment A is standby.
(2-2) 1:9 taking precipitate A and deionized water by volume, in sediment A, add deionized water, by deionized water, sediment A is washed 10 minutes, then put into centrifuge, with the rotating speeds of 1000 revs/min centrifugal 10 minutes, be precipitated thing B and supernatant liquor B, supernatant liquor B is poured out, sediment B is standby, and 1:9 taking precipitate B and deionized water repeating step (2-2) washing by volume three to four times, is precipitated thing C.
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:9 taking precipitate A and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) sediment D that contains a small amount of absolute ethyl alcohol step (2-3) being obtained is put into vacuum drying chamber, and at 10 pascal pressures, 80 ℃, vacuum drying chamber is 48 hours, removes moisture and absolute ethyl alcohol in sediment, obtains finished product amorphous nickel nano particle.
Claims (8)
1. a preparation method for amorphous nickel nano particle, is characterized in that described preparation method carries out as follows:
(1) prepare nickel nano particle
(1-1) get absolute ethyl alcohol and transfer in reaction vessel, in absolute ethyl alcohol, pass into nitrogen, to get rid of the oxygen in reaction system and reaction vessel;
(1-2) under nitrogen atmosphere, in absolute ethyl alcohol, add nickel chloride, make the molal volume concentration of nickel chloride between 0.01mol/L～0.1mol/L, then add [BMIN] BF
4ionic liquid, as dispersant, stirs, and makes nickel source dispersion soln, standby, described absolute ethyl alcohol and [BMIN] BF
4the volume ratio of ionic liquid is 100:2～14;
(1-3) weigh sodium borohydride and deionized water, the sodium borohydride aqueous solution that configuration molal volume concentration is 0.85mol/L, standby;
(1-4) under stirring, to dripping volumetric concentration in the dispersion soln of nickel source, it is 20%～25% hydrazine hydrate aqueous solution complex ni-ion, add while stirring again sodium borohydride aqueous solution, be stirred to and generate after black precipitate, continue to stir 1～24 hour, obtain reactant liquor, the absolute ethyl alcohol in described step (1-2) and the volume ratio of hydrazine hydrate aqueous solution are 100:1～10, and the absolute ethyl alcohol in described step (1-2) and the volume ratio of sodium borohydride aqueous solution are 100:5～15;
(2) clean amorphous nickel nano particle:
(2-1) reactant liquor step (1-4) being obtained carries out centrifugal, is precipitated thing A and supernatant liquor A, pours out supernatant liquor A, and sediment A is standby;
(2-2) 1:4～9 taking precipitate A and deionized water by volume, in sediment A, add deionized water, by deionized water, sediment A is washed, then put into centrifuge and carry out centrifugally, be precipitated thing B and supernatant liquor B, supernatant liquor B is poured out, sediment B is standby, 1:4～9 taking precipitate B and deionized water repeating step (2-2) by volume, washing precipitate B tri-to four times, is precipitated thing C;
(2-3) with absolute ethyl alcohol, replace deionized water, washing and precipitating thing C, 1:4～9 taking precipitate C and absolute ethyl alcohol repeating step (2-2) washing by volume three to four times, is precipitated thing D;
(3) sediment D of step (2-3) is put into vacuum drying chamber, at 10～100 pascal pressures, 80～90 ℃, vacuum drying chamber is 24～48 hours, removes moisture and absolute ethyl alcohol in sediment, obtains finished product amorphous nickel nano particle.
2. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that the stirring described in described step (1-2) is to open mixer, stirs 10 minutes with the speed of 100～200 revs/min.
3. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that in described step (1-2) absolute ethyl alcohol and [BMIN] BF
4the volume ratio of ionic liquid is 100:6～10.
4. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that centrifugal described in described step (2-1) is under the condition of 1000～2000 revs/min centrifugal 10～20 minutes.
5. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that in described step (1-4), the absolute ethyl alcohol in step (1-2) and the volume ratio of hydrazine hydrate aqueous solution are 100:1～6.
6. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that in described step (1-4), the absolute ethyl alcohol in described step (1-2) and the volume ratio of sodium borohydride aqueous solution are 100:5～10.
7. the preparation method of amorphous nickel nano particle as claimed in claim 1, is characterized in that centrifugal described in described step (2-2) is under the condition of 1000～2000 revs/min centrifugal 10～20 minutes.
8. the preparation method of amorphous nickel nano particle as claimed in claim 1, it is characterized in that described step (2-1) at the middle and upper levels clear liquid A and step (2-2) at the middle and upper levels clear liquid B after reclaiming, adopt the way of distillation to reclaim ethanol and distilled water, by the ethanol obtaining for producing again.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644282A (en) * | 2005-01-13 | 2005-07-27 | 南京大学 | Production for nanometer nickel powder |
| KR100508693B1 (en) * | 2004-03-03 | 2005-08-17 | 한국화학연구원 | Synthetic method of nano-sized ni powder |
| CN1792521A (en) * | 2005-12-30 | 2006-06-28 | 中山大学 | Liquid phase preparation process of nano nickle powder |
| CN101168196A (en) * | 2006-10-27 | 2008-04-30 | 同济大学 | Method for preparing nickel-base amorphous nano particles |
| CN101555375A (en) * | 2009-05-14 | 2009-10-14 | 上海第二工业大学 | Preparation method for solar selective heat-absorbing paint adopting nano nickel powder as absorber |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100508693B1 (en) * | 2004-03-03 | 2005-08-17 | 한국화학연구원 | Synthetic method of nano-sized ni powder |
| CN1644282A (en) * | 2005-01-13 | 2005-07-27 | 南京大学 | Production for nanometer nickel powder |
| CN1792521A (en) * | 2005-12-30 | 2006-06-28 | 中山大学 | Liquid phase preparation process of nano nickle powder |
| CN101168196A (en) * | 2006-10-27 | 2008-04-30 | 同济大学 | Method for preparing nickel-base amorphous nano particles |
| CN101555375A (en) * | 2009-05-14 | 2009-10-14 | 上海第二工业大学 | Preparation method for solar selective heat-absorbing paint adopting nano nickel powder as absorber |
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