CN101007357A - Nanometer nickel powder and its preparation method - Google Patents
Nanometer nickel powder and its preparation method Download PDFInfo
- Publication number
- CN101007357A CN101007357A CN 200710026458 CN200710026458A CN101007357A CN 101007357 A CN101007357 A CN 101007357A CN 200710026458 CN200710026458 CN 200710026458 CN 200710026458 A CN200710026458 A CN 200710026458A CN 101007357 A CN101007357 A CN 101007357A
- Authority
- CN
- China
- Prior art keywords
- nickel powder
- nickel
- preparation
- liquid
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 150000002815 nickel Chemical class 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 241000080590 Niso Species 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 abstract description 11
- 229920013657 polymer matrix composite Polymers 0.000 abstract description 6
- 239000011160 polymer matrix composite Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 5
- 230000005672 electromagnetic field Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- -1 and as seen Chemical compound 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Images
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a linear nanometer nickel powder and its preparation method. The linear nanometer nickel powder synthesized by the invention is slightly bend, part linear nickel powder is cross bonding and generates branched or netted structures, and the surface of each nickel line is full of lunge in nano-size. The invention uses macromolecular polymer or monomer as soft template, then microwave heats liquid phase and nickel salt is reduced chemically to synthesizing linear nickel powder in nanometer structure. The preparation method has simple art, easy operation, fast response rate and low needed temperature; the uniformity and crystallinity of synthesized nanometer structure nickel line is good, activity is high, it can meet the demand of various industries to high activity nickel powder; meanwhile the branched or netted structure nickel line and its nano lunge is fastened with polymer firmly, that can improve the strength and toughness and other mechanical properties of polymer matrix composite material.
Description
Technical field
The present invention relates to a kind of nanometer nickel powder and preparation method thereof, belong to field of nanometer technology.
Background technology
Nano-nickel powder because of the surface-active height, catalytic performance is good, electromagnetic performance is good, field extensive uses such as electrode, electrocondution slurry and catalyst in battery, magnetic recording material, multi-layer capacitor, the performance of Nano metal powder not only depends on its particle size, and is also closely related with its shape.As for reducing the contraction when the sintering of electrode in the multilayer ceramic capacitor, adopt the spherical nickel powder of better crystallinity degree best.And linear nickel powder is when improving the electromagnetic performance of polymer matrix composite, also can improve mechanical properties such as the intensity of polymer matrix composite and toughness, and therefore, the development of nanometer nickel powder has received very big concern.Hydro-thermal method, micro emulsion method, organic metal compound decomposition method, AAO template electric-sedimentation method and soft template method etc. all can prepare wire or bar-shaped nano-nickel powder.
According to Journal of Crystal Growth 252 (2003) 612~617 reports, in the microemulsion of water-butanols-potassium oleate-kerosene, use hydrazine hydrate reduction NiCl
26H
2It is 8~10nm that O prepares diameter, the rod-like nano nickel powder of long 100~200nm.
According to another Transactions of Nonferrous Metals Society of China 16 (2006) 96~100 reports, with the nickel oxalate is raw material, PVP, PEG is a soft template, having synthesized diameter by the thermal decomposition nickel hydroxide is 10~15nm, and length is the monocrystalline nickel nanometer rods of 70~120nm, but its complex procedures, the reaction temperature height, and the reaction time reach 18 hours.
Materials Letters 57 (2003) 3992-3997 report in ethylene glycol solution, is a raw material with the nickelous sulfate, and it is 0.1-0.5 μ m that the hydrazine hydrate reduction nickel hydroxide has synthesized diameter, and length is the bar-shaped nickel powder of 1~8 μ m.
Patent CN 1491762A report at first reacts nickel salt and compound precipitants to the presoma that obtains nickel powder, and the presoma of nickel powder has obtained the fibrous nano nickel powder 350~600 ℃ elevated temperature heat decomposition.
The heating using microwave reaction is a kind of means of very effective preparation super-fine metal powder, since adding chemical reaction from the discovery microwave thermal, has been widely used in the synthetic preparation of various nano materials.Journal ofCrystal Growth 273 (2005) 439-445 report adopts heating using microwave, reduces AgNO3 with natrium citricum, adds the Au crystal seed simultaneously, has obtained the nano-silver powder of wire.Generally speaking, wire precious metal powder (Au, Ag, Pt etc.) is synthesized in heating using microwave, existing report on the document.
Compare with noble metal, the chemism of nickel is higher, easy and other material generation chemical reaction; And nickel has magnetic, attracts each other between particle.The granularity of nano-nickel powder and pattern control ratio be difficulty, the synthetic method ubiquity complex procedures of present linear nickel powder, the reaction temperature height, deficiencies such as the reaction time is long, and synthetic linear nickel powder smooth surface, add in the macromolecular material, the not high enough problem of bond strength still exists between metal powder and organic matter, has influenced mechanical properties such as the intensity of polymer matrix composite and toughness.Therefore, seek an advantages of simplicity and high efficiency preparation method, rapidly and efficiently synthetic linear nickel powder is still one and is rich in challenging work; Simultaneously, develop a kind of linear nickel powder of special nanostructured, make it in the electromagnetic performance that improves as polymer matrix composite, also improve mechanical properties such as its intensity and toughness.The development of the linear nickel powder of this special construction has very high realistic meaning.
Summary of the invention
At the deficiency that existing linear nickel powder is used, primary and foremost purpose of the present invention provides a kind of nanometer nickel powder of function admirable.
Linear nickel powder is case of bending slightly, and part linear nickel powder is cross-linked with each other and forms dendritic or network structure.The nickel wire surface has been covered with the thorn of nano-scale, the specific area height of nickel wire, and catalytic activity is good, can satisfy the demand of domestic battery industry to high activity nickel.Dendritic or network structure nickel powder and nanometer thorn thereof combine firmly with polymer, can improve mechanical properties such as the intensity of polymer matrix composite and toughness greatly.
The nanostructured nickel wire diameter that the present invention synthesizes is 0.05~2 μ m, and line length is 5~20 μ m, has been covered with the thorn of nano-scale on every nickel wire surface, and thorn length is 20nm~100nm, and the diameter of thorn is 10nm-100nm, and the density of thorn is 4.9 * 10
5Individual/cm
2~1.8 * 0
6Individual/cm
2
Another object of the present invention provides above-mentioned preparation method with nanometer nickel powder.The present invention adopts the linear nickel powder of heating using microwave electronation nickel salt synthesis of nano structure, and its technology is simple, and reaction speed is fast, and temperature is low, rapidly and efficiently.
The preparation method of nanometer nickel powder of the present invention is as follows: nickel salt and high molecular polymer or monomer stirring soluble in water and abundant are obtained A liquid; With reducing agent and the alkali B liquid that obtains soluble in water; A liquid with after B liquid mixes, is reacted to reaction solution with heating using microwave and to become clear, and Separation of Solid and Liquid is carried out in cooling, makes described nanometer nickel powder.
As preferred version, carry out isothermal reaction to 60-100 ℃ with heating using microwave.Heating using microwave can be adopted dual mode: a kind of is to react with the firm power heating, or keeps steady temperature with different microwave powers and react.
In the mixed solution of described A and B, the concentration of nickel salt is 0.01~0.5mol/L, and the concentration of high molecular polymer or monomer is 0.1~50g/L, and the concentration of reducing agent is 0.01~1.0mol/L, and the concentration of alkali is 0.01~0.5mol/L.As preferred version, the concentration of nickel salt is 0.05~0.2mol/L, and the concentration of high molecular polymer or monomer is 0.1~20g/L, and the concentration of reducing agent is 0.1~1.0mol/L; The concentration of alkali is 0.02~0.2mol/L.
Described high molecular polymer or monomer comprise water soluble polymers such as PVP, polyvinyl alcohol, polyethylene glycol, polyacrylic acid.
Described nickel salt is NiSO
4Or NiCl
2, Ni (OH)
2, reducing agent is hydrazine hydrate or sodium borohydride.
Described alkali is NaOH, sodium carbonate or ammoniacal liquor.
Theoretical foundation of the present invention is as follows: water and PVP are polar molecules, under the microwave electromagnetic field action, the warm-up movement state of polar molecule is oriented according to the direction alternation of electromagnetic field, produce similar frictional heat, the energy of alternating electromagnetic field is converted into the heat energy in the medium in this microprocess, makes medium temperature rising on the macroscopic view occur.Because and heating using microwave speed does not need heat conducting process, each position of object usually can both the uniformly penetrating electromagnetic wave, produces the localized hyperthermia district and can promote reduction reaction, makes kinetics improve two orders of magnitude.As seen, PVP molecule and hydrone align according to alternation before and after the direction of electromagnetic field under the microwave electromagnetic field action, the frictional heat that produces promotes nickel crystallite to form and grows up, nickel crystallite forms and grows up to reunite becomes nickel wire, and as seen, PVP becomes the soft template that linear nickel powder forms.
It is under certain alkali condition that chemical reduction method prepares nickel powder, by reducing agent the corresponding metal nickel salt is reduced, utilize the effect of surfactant or high molecular polymer or monomer to particle surface, obtain the controlled nano-nickel powder of size shape, the advantage of chemical reduction method is that reaction temperature is lower, reaction condition is gentle, simple to operate.And heating using microwave is compared with the traditional heating method, and its advantage is that firing rate is fast, inside and outside heating simultaneously; In heating systems, produce local high-temperature region, promote reaction; Heating using microwave can improve the order of magnitude to kinetics one or two.Microwave is auxiliary to add thermal synthesis sodium metal ground rice has become a new technology that has a extensive future.With the mutual supplement with each other's advantages of heating using microwave and chemical reduction method, high efficiency is synthesized linear nickel powder just in the present invention.This preparation method technology is simple, processing ease, and reaction rate is fast, and temperature is low.
Description of drawings
Fig. 1 is the electron scanning micrograph of 5 dried times nanometer nickel powders.
Fig. 2 is the electron scanning micrograph of 20,000 times of nanometer nickel powders.
Fig. 3 is the transmission electron microscope photo of 200,000 times of nanometer thorns.
The specific embodiment
Embodiment one:
1) with 0.025mol NiCl
2With obtain 250ml A liquid in the water-soluble solution of 2g PVPK30, and fully stir A liquid evenly mixed.
2) with 0.5mol N
2H
4.H
2The miscible 250ml B liquid that in the aqueous solution, obtains of O and 0.025mol NaOH.
3) A liquid is mixed with B liquid, adopt low microwave power to be heated to 70 ℃ in 6 minutes after, keep stationary temperature with this power heating, become black to mixed liquor, the clear back adding of solution becomes cold water is cooled to room temperature (10~30 ℃).
4) nickel powder is carried out Separation of Solid and Liquid according to a conventional method, the diameter of the nickel powder of preparation is 0.5~0.6 μ m, and length is the linear nickel powder of 10~15 μ m, and linear nickel powder forms network structure.The lip-deep thorn length of linear nickel powder is 50nm~70nm, and the diameter of thorn is 10-30nm, and the density of thorn is 1.8 * 10
6Individual/cm
2
Embodiment two:
1) with 0.5mol NiSO
4With obtain 400ml A liquid in the water-soluble solution of 10g polyvinyl alcohol, and fully stir A liquid evenly mixed.
2) with 1mol sodium borohydride and the miscible 100ml B liquid that in the aqueous solution, obtains of 0.5mol sodium carbonate.
3) A liquid is mixed with B liquid, after microwave power was heated to 80 ℃ in 3 minutes in the employing, add thermal response with this power, become black to mixed liquor, the clear back of solution becomes adds cold water and is cooled to room temperature (10~30 ℃).
4) nickel powder is carried out Separation of Solid and Liquid according to a conventional method, the diameter of the nickel powder of preparation is 0.5~2 μ m, and length is the linear nickel powder of 5~15 μ m, and linear nickel powder forms dendritic morphology.The lip-deep thorn length of linear nickel powder is 20nm~40nm, and the diameter of thorn is 20-50nm, and the density of thorn is 8.1 * 10
5Individual/cm
2
Embodiment three:
1) with 0.025mol NiCl
2With obtain 400ml A liquid in the water-soluble solution of 20g NVP, and fully stir A liquid evenly mixed.
2) with 0.375mol and the miscible 100ml B liquid that in the aqueous solution, obtains of 0.025mol ammoniacal liquor.
3) A liquid is mixed with B liquid, adopt high microwave power to be heated to 100 ℃ in 1.5 minutes after, add thermal response with this power, become black to mixed liquor, the clear back of solution becomes adds cold water and is cooled to room temperature (10~30 ℃).
4) nickel powder is carried out Separation of Solid and Liquid according to a conventional method, the diameter of the nickel powder of preparation is 0.05~0.2 μ m, and length is the linear nickel powder of 5~10 μ m, and linear nickel powder forms network structure.The length of stinging on the linear nickel powder surface is 20nm~40nm, and the diameter of thorn is 40-100nm, and the density of thorn is 4.9 * 10
5Individual/cm
2
Embodiment four:
1) with 0.25mol Ni (OH)
2With obtain 250ml A liquid in the water-soluble solution of 0.2g polyacrylic acid, and fully stir A liquid evenly mixed.
2) with 0.5mol sodium borohydride and the miscible 250ml B liquid that in the aqueous solution, obtains of 0.025mol sodium carbonate.
3) A liquid is mixed with B liquid, adopt the highest microwave power to be heated to 60 ℃ in 1 minute after, keep stationary temperature with this grade heating, become black to mixed liquor, the clear back of solution becomes adds cold water and is cooled to room temperature (10~30 ℃).
4) nickel powder is carried out Separation of Solid and Liquid according to a conventional method, the diameter of the nickel powder of preparation is 0.1~0.5 μ m, and length is the linear nickel powder of 5~10 μ m, and linear nickel powder forms network structure.The length of the lip-deep thorn of linear nickel powder is 40nm~80nm, and the diameter of thorn is 30-50nm, and the density of thorn is 9.8 * 10
5Individual/cm
2
Embodiment five:
1) with 0.005molNiCl
2With obtain 400ml A liquid in the water-soluble solution of 10g ethylene glycol, and fully stir A liquid evenly mixed.
2) with 0.15mol N
2H
4.H
2The miscible 100ml B liquid that in the aqueous solution, obtains of O and 0.01molNaOH.
3) A liquid is mixed with B liquid, adopt minimum microwave power to be heated to 80 ℃ in 10 minutes after, keep stationary temperature with this grade heating, become black to mixed liquor, the clear back of solution becomes adds cold water and is cooled to room temperature (10~30 ℃).
4) nickel powder is carried out Separation of Solid and Liquid according to a conventional method, the diameter of the nickel powder of preparation is 0.1~0.2 μ m, and length is the linear nickel powder of 1~5 μ m, and linear nickel powder forms dendritic morphology.The lip-deep thorn length of linear nickel powder is 50nm~10nm, and the diameter of thorn is 10-30nm, and the density of thorn is 1.6 * 10
6Individual/cm
2
Claims (10)
1, a kind of nanometer nickel powder is characterized in that: be sweep state slightly, and be covered with the thorn of nano-scale on every nickel wire surface, being cross-linked with each other between the part linear nickel powder forms dendritic or network structure.
2, nanometer nickel powder as claimed in claim 1 is characterized in that: linear diameter is 0.05~2 μ m, and line length is 5~20 μ m, the thorn that has been covered with nano-scale on every nickel wire surface, thorn length is 20nm~100nm, and the thorn diameter is 10-100nm, and the density of thorn is 4.9 * 10
5Individual/cm
2~1.8 * 0
6Individual/cm
2
3, a kind of preparation method of nanometer nickel powder as claimed in claim 1 is characterized in that: nickel salt and high molecular polymer or high polymer monomer stirring soluble in water and abundant are obtained A liquid; With reducing agent and the alkali B liquid that obtains soluble in water; With after B liquid mixes, the heating using microwave reaction becomes clear to reaction solution with A liquid, and Separation of Solid and Liquid is carried out in cooling, makes described nanostructured linear nickel powder.
4, preparation method according to claim 3 is characterized in that: with microwave the mixed liquor of A liquid and B liquid is heated to 60-100 ℃ and carries out described reaction.
5, preparation method according to claim 4 is characterized in that following any mode of heating using microwave employing: react with the firm power heating, or keep steady temperature with different microwave powers and react.
6, preparation method according to claim 3, it is characterized in that: in the mixed solution of A and B, the concentration of nickel salt is 0.001~0.5mol/L, the concentration of high molecular polymer or monomer is 0.1~50g/L, the concentration of reducing agent is 0.01~1.0mol/L, and the concentration of alkali is 0.01~0.5mol/L.
7, preparation method according to claim 6 is characterized in that: in the solution, the concentration of nickel salt is 0.05~0.2mol/L after the mixing of A and B, and the concentration of high molecular polymer or monomer is 0.1~20g/L, and the concentration of reducing agent is 0.1~1.0mol/L; The concentration of alkali is 0.02~0.2mol/L.
8, preparation method according to claim 3 is characterized in that: described high molecular polymer is PVP, polyvinyl alcohol, polyethylene glycol or polyacrylic acid or their monomer.
9, preparation method according to claim 3 is characterized in that: described nickel salt is NiSO
4Or NiCl
2, Ni (OH)
2, reducing agent is hydrazine hydrate or sodium borohydride.
10, preparation method according to claim 3 is characterized in that: described alkali is NaOH, sodium carbonate or ammoniacal liquor.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100264584A CN100491026C (en) | 2007-01-22 | 2007-01-22 | Line-shape nanometer nickel powder and its preparation method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100264584A CN100491026C (en) | 2007-01-22 | 2007-01-22 | Line-shape nanometer nickel powder and its preparation method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101007357A true CN101007357A (en) | 2007-08-01 |
CN100491026C CN100491026C (en) | 2009-05-27 |
Family
ID=38696138
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2007100264584A Expired - Fee Related CN100491026C (en) | 2007-01-22 | 2007-01-22 | Line-shape nanometer nickel powder and its preparation method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100491026C (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103586482A (en) * | 2013-10-25 | 2014-02-19 | 江苏大学 | Method for preparing nanometer nickel under microwave and ultraviolet irradiation |
CN103978227A (en) * | 2014-05-22 | 2014-08-13 | 冷劲松 | Method for preparing controllable nickel nanowires conveniently at low cost |
CN104384525A (en) * | 2014-11-27 | 2015-03-04 | 东北大学 | Dispersing and assembling method of nickel-iron metal nano-wires |
CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
CN110340376A (en) * | 2019-07-16 | 2019-10-18 | 浙江大学 | A kind of flower-shaped nickel wire absorbing material and preparation method thereof |
CN115401208A (en) * | 2022-09-02 | 2022-11-29 | 江苏大学 | Preparation method of nickel-based nano powder with controllable morphology |
-
2007
- 2007-01-22 CN CNB2007100264584A patent/CN100491026C/en not_active Expired - Fee Related
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103586482A (en) * | 2013-10-25 | 2014-02-19 | 江苏大学 | Method for preparing nanometer nickel under microwave and ultraviolet irradiation |
CN103586482B (en) * | 2013-10-25 | 2016-06-15 | 江苏大学 | The preparation method of nano nickel under a kind of microwave, ultraviolet irradiation |
CN103978227A (en) * | 2014-05-22 | 2014-08-13 | 冷劲松 | Method for preparing controllable nickel nanowires conveniently at low cost |
CN103978227B (en) * | 2014-05-22 | 2016-06-08 | 冷劲松 | A kind of cheap convenient method preparing controlled nickel nano wire |
CN104384525A (en) * | 2014-11-27 | 2015-03-04 | 东北大学 | Dispersing and assembling method of nickel-iron metal nano-wires |
CN104384525B (en) * | 2014-11-27 | 2016-05-25 | 东北大学 | The dispersion of a kind of nickel or ferronickel metal nanometer line and assemble method |
CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
CN108500292B (en) * | 2018-04-08 | 2021-03-23 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
CN110340376A (en) * | 2019-07-16 | 2019-10-18 | 浙江大学 | A kind of flower-shaped nickel wire absorbing material and preparation method thereof |
CN110340376B (en) * | 2019-07-16 | 2020-11-13 | 浙江大学 | Flower-shaped nickel wire wave-absorbing material and preparation method thereof |
CN115401208A (en) * | 2022-09-02 | 2022-11-29 | 江苏大学 | Preparation method of nickel-based nano powder with controllable morphology |
CN115401208B (en) * | 2022-09-02 | 2024-02-27 | 江苏大学 | Preparation method of nickel-based nano powder with controllable morphology |
Also Published As
Publication number | Publication date |
---|---|
CN100491026C (en) | 2009-05-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN100491026C (en) | Line-shape nanometer nickel powder and its preparation method | |
CN101920942B (en) | Method for controlling synthesis of zinc selenide multi-morphological nano material | |
CN103305185B (en) | Method for preparing reduced-oxidized graphene/Fe3O4/Ag nano composite wave-absorbing material | |
CN101804459B (en) | Method for preparing nano nickel powder by using microchannel reactor | |
CN107867726B (en) | A kind of preparation method of nano oxidized ruthenium | |
CN101342598A (en) | Method for preparing metallic nickel nano-wire | |
CN101367044B (en) | Method for preparing nano-catalyst copper chromite and copper ferrite | |
CN102139909A (en) | Method for synthesizing micron-nano-sized cuprous oxide micropowder by controlling shape of micron-nano-sized cuprous oxide micropowder | |
CN104402041B (en) | A kind of SnO 2/ Ag composite nano-powder and preparation method thereof | |
CN107954483A (en) | A kind of class alpha-phase nickel hydroxide ultrathin nanometer piece and preparation method thereof | |
CN102198510B (en) | Method for preparing nano copper/carbon nano tube composite powder by liquid phase method | |
CN105293441A (en) | Three-dimensional high-dispersion nano layered double hydroxide synthesis method | |
CN100556587C (en) | Microwave auxiliary liquid phase reduction method preparing needle-shaped nanometer nickel | |
CN100431750C (en) | Liquid phase preparation process of nano nickle powder | |
CN109267091A (en) | A kind of method and its application of the ultrasonic method auxiliary preparation ultra-fine Ni/N-C composite catalyzing material of cross-linked structure | |
CN102962470B (en) | Method for preparing spherical ultrafine nickel powder at room temperature | |
CN106517361A (en) | Preparation method of spinel type nano nickel ferrite powder | |
CN1273251C (en) | Nano structure nickel powde and its preparing method | |
CN107487789A (en) | A kind of stratiform nickel cobalt hydroxide nano pipe cone and its preparation method and application | |
CN114950410B (en) | Synthetic method of zirconium-manganese composite material | |
CN100368281C (en) | Preparation method of nanometer metal oxide and composite metal oxide | |
CN108479761B (en) | Method for preparing spherical perovskite catalyst by taking casein as biological template | |
CN105753059B (en) | A kind of preparation method of carbon-based magnesium ferrite composite wave-absorbing film | |
CN109437337B (en) | Fireworks-shaped nickel cobaltate material composed of rods with necklace structure and preparation method and application thereof | |
CN103058241B (en) | High-efficiency synthetic method of nanometer aluminum particle |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090527 Termination date: 20160122 |
|
EXPY | Termination of patent right or utility model |