CN104384525A - Dispersing and assembling method of nickel-iron metal nano-wires - Google Patents
Dispersing and assembling method of nickel-iron metal nano-wires Download PDFInfo
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- CN104384525A CN104384525A CN201410705845.0A CN201410705845A CN104384525A CN 104384525 A CN104384525 A CN 104384525A CN 201410705845 A CN201410705845 A CN 201410705845A CN 104384525 A CN104384525 A CN 104384525A
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- nickel
- ferronickel
- nanometer line
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Abstract
The invention belongs to the field of nanometer materials, and particularly relates to a dispersing and assembling method of nickel-iron metal nano-wires. According to the technical scheme, the dispersing and assembling method comprises the steps of: firstly, performing hydrothermal reaction to prepare the nickel-iron metal nano-wires, then putting the nickel-iron metal nano-wires in a hydrochloric acid solution with the pH value of 3-6 for ultrasonic stirring for 0.5-24 hours, dispersing the nickel-iron metal nano-wires into nickel-iron metal nano-particles, then putting the dispersed nickel-iron metal nano-particles in a sodium hydroxide solution with the pH value of 8-12 for stirring for 0.5-3 hours, then transferring the mixture in a hydrothermal reaction kettle, keeping the temperature of 80-120 DEG C for 2-10 hours, then cooling to the room temperature naturally, and compounding the nickel-iron metal nano-particles into nickel-iron metal nano-wires again. By virtue of controlling the pH value, dispersion and assembling of the nickel-iron metal nano-wires is realized, and control on shape of the nickel-iron metal nano-materials is realized.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to dispersion and the assemble method of a kind of ferronickel system metal nanometer line.
Background technology
The discovery of CNT of 20th century causes the broad interest of scientists to other monodimension nanometer materials, and when the size of material is equal to or less than its characteristic length, as Bohr radius, optical wavelength, phonon free path etc., quantum effect will become highly significant.From pattern, monodimension nanometer material comprises nano wire, nanobelt, nanotube, nanometer rods etc.The wherein monodimension nanometer material of nano wire to be a kind of diameter be nanometer scale, owing to there being the characteristic of very large major diameter when limited, the one dimension conducting of two-dimensions, nano wire has a lot of unique optics and electromagnetic property.In addition, as a kind of desirable energy transmitting materials, the high length-diameter ratio of nano wire makes it can the quantization particle such as transmission electronic, photon, phonon, and therefore it has very important application in high-tech sector.
Ferronickel based nano-material, as magnetic material, has unique electricity, magnetic and catalysis characteristics, in magnetic recording, catalyst, sensor and biomedicine field etc., shows huge application potential.
Nano material preparation technology is through development in recent decades, and the appearance of especially the field of chemical synthesis important breakthrough and innovation, makes the nano material of various material all can prepare in laboratory scope.The preparation method of nano wire just includes the multiple methods such as gas phase transformation approach, chemical vapour deposition technique, pulse laser ablation method, electrodeposition process, Rong Jiao – gel method, template, hydro-thermal method and microemulsion method.Especially in the last few years in the monodispersity of nano particle, component, size, pattern, structure control and certain scaleization batch production, all significant progress was achieved, the ferronickel nano wire etc. of the adjustable gold nanorods of the draw ratio as prepared, structure-controllable.But current present technology also mainly concentrates on the single sintering of nano wire, cannot realize the fractionation of nano wire, more cannot realize assembling again after splitting, this will be unfavorable for the controllable operating of the nano-device that nano wire is formed.
Summary of the invention
For prior art Problems existing, the invention provides dispersion and the assemble method of a kind of ferronickel system metal nanometer line, object is by adopting Hydrothermal Synthesis, be that ferronickel system nano wire prepared by reducing agent with hydrazine hydrate, by the control to additive citric acid sodium consumption, realize control to ferronickel based nano-material pattern, and by the regulation and control of pH value, achieve nano wire and nano particle mutually transforms and assembles.
The technical scheme realizing the object of the invention is carried out according to following steps:
(1) mixture of soluble nickel salt or soluble nickel salt and soluble ferrite is dissolved in deionized water, form nickel salt or ferronickel salting liquid, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel or nickel and iron is (1 ~ 2): 1, then hydrazine hydrate is added, the hydrazine hydrate added is 20 ~ 60 times of nickel or nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 100 ~ 150 DEG C of constant temperature 1 ~ 10h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel system metal nanometer line,
(2) above-mentioned ferronickel system metal nanometer line is placed in hydrochloric acid solution ultrasonic agitation 0.5 ~ 24h that pH value is 3 ~ 6, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel system metal nanometer line is dispersed into as ferronickel system metal nanoparticle;
(3) the ferronickel system metal nanoparticle after dispersion is placed in sodium hydroxide solution stirring 0.5 ~ 3h that pH value is 8 ~ 12, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 80 ~ 120 DEG C of constant temperature 2 ~ 10h, magnetic product is separated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel system metal nanoparticle is reassembled into ferronickel system metal nanometer line.
Wherein, described soluble nickel salt is nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate, and described soluble ferrite is ferrous sulfate, frerrous chloride, ferrous nitrate, ferrous acetate.
Described soluble nickel salt and soluble ferrite can according to any mixed in molar ratio.
The ratio of the mixture of described deionized water and soluble nickel salt or soluble nickel salt and soluble ferrite is the mixture of 100 ~ 1000ml water every gram of soluble nickel salt or soluble nickel salt and soluble ferrite.
Described ferronickel system metal nanometer line and the ratio of hydrochloric acid are 100 ~ 200ml hydrochloric acid every gram of metal nanometer lines.
Described ferronickel system metal nanoparticle and the ratio of sodium hydroxide solution are 100 ~ 200ml sodium hydroxide solution every gram of metal nanoparticles.
Compared with prior art, feature of the present invention and beneficial effect are:
Nickel salt and molysite are hydrated hydrazine in the basic conditions and are reduced to elemental nickel and fe, and its reaction principle is as follows:
2Fe
2++4OH
-+N
2H
4→2Fe+N
2+4H
2O (1);
2Ni
2++4OH
-+N
2H
4→2Ni+N
2+4H
2O (2);
The one-tenth nuclear reaction of dilval is as follows:
xNi+yFe=Ni
xFe
y;x=0~1,y=0~1; (3);
The side reaction produced in course of reaction:
3N
2H
4→N
2+4NH
3(4);
The structural formula of natrium citricum is
after ferronickel system magnetic-particle generates, bearing on natrium citricum is coated on newly-generated ferronickel system magnetic-particle surface from oxygen groups, prevent its further growth to be large particle, this is also the reason utilizing excessive natrium citricum to control grain diameter formation nano material.Meanwhile, natrium citricum molecule there are three negative oxygen ions, can be connected with other metallic particles respectively, and then be polymerized to large metal wire.
Equally, regulate the pH value of solution 3 ~ 6 scope, the negative oxygen ion of natrium citricum can substep binding hydrogen ions, thus loses the adsorption capacity in metal surface.Therefore regulate the pH value of solution, make the negative oxygen ion binding hydrogen ions of natrium citricum, and then break linear structure.
Regulate solution ph 8 ~ 12 scope, the hydrogen ion be combined with natrium citricum negative oxygen ion is neutralized by alkali, again the natrium citricum containing three negative oxygen ions is obtained, namely three negative oxygen ions that can be adsorbed on metal surface are again obtained, thus, dispersed metal wire is reassembled into metal wire again, and the present invention, by the control to pH value, realizes dispersion and the assembling of ferronickel system nano metal line.
Accompanying drawing explanation
Fig. 1 is the nickel nano wire prepared in the embodiment of the present invention 1;
Fig. 2 is the nano nickel particles disperseing in the embodiment of the present invention 1 to obtain;
Fig. 3 re-assemblies the nickel nano wire obtained in the embodiment of the present invention 1.
Detailed description of the invention
Embodiment 1
Dispersion and the assemble method of the ferronickel system metal nanometer line of the present embodiment carry out according to following steps:
(1) nickel chloride is dissolved in deionized water, form nickel salt solution, the volume of deionized water is 100ml/g nickel chloride, under nitrogen protection, in solution, add natrium citricum and mix, the natrium citricum added is 2:1 with the ratio of the molal quantity of nickel, then hydrazine hydrate is added, the hydrazine hydrate added is 20 times of nickel molal quantity, is transferred in hydrothermal reaction kettle by above-mentioned solution system, after 150 DEG C of constant temperature 1h, naturally cool to room temperature, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain nickel metal nanometer line, as shown in Figure 1;
(2) above-mentioned nickel nano wire is placed in the hydrochloric acid solution ultrasonic agitation 15h that pH value is 4, the ratio of nickel nano wire and hydrochloric acid is 180ml hydrochloric acid every gram of nickel metal nanometer line, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, nickel nano wire is dispersed into as nano nickel particles, as shown in Figure 2;
(3) by dispersion after nano nickel particles be placed in pH value be 11 sodium hydroxide solution stir 0.5h, the ratio of nano nickel particles and sodium hydroxide solution is 100ml sodium hydroxide solution every gram of nano nickel particles, then be transferred in hydrothermal reaction kettle, after 80 DEG C of constant temperature 10h, naturally cool to room temperature, be separated magnetic product with magnetic field, clean twice respectively with deionized water and ethanol, dry up with nitrogen, now, as shown in Figure 3, nano nickel particles is reassembled into nickel nano wire.
Embodiment 2
Dispersion and the assemble method of the ferronickel system metal nanometer line of the present embodiment carry out according to following steps:
(1) by nickelous sulfate and ferrous sulfate according to mol ratio 2:1 mixed dissolution in deionized water, form ferronickel salting liquid, the volume of deionized water is 500ml/g ferronickel salt, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel and iron is 2:1, then hydrazine hydrate is added, the hydrazine hydrate added is 40 times of nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 110 DEG C of constant temperature 8h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel metal nanometer line,
(2) above-mentioned ferronickel nano wire is placed in the hydrochloric acid solution ultrasonic agitation 0.5h that pH value is 3, the ratio of ferronickel nano wire and hydrochloric acid is 200ml hydrochloric acid every gram of ferronickel nano wire, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano wire is dispersed into as ferronickel nano particle;
(3) by dispersion after ferronickel nano particle be placed in pH value be 8 sodium hydroxide solution stir 1.5h, the ratio of ferronickel nano particle and sodium hydroxide solution is 180ml sodium hydroxide solution every gram of ferronickel nano particle, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 120 DEG C of constant temperature 2h, be separated magnetic product with magnetic field, clean twice respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano particle is reassembled into ferronickel nano wire.
Embodiment 3
Dispersion and the assemble method of the ferronickel system metal nanometer line of the present embodiment carry out according to following steps:
(1) by nickel nitrate and frerrous chloride according to mol ratio 3:1 mixed dissolution in deionized water, form ferronickel salting liquid, the volume of deionized water is 1000ml/g ferronickel salt, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel and iron is 1.5:1, then hydrazine hydrate is added, the hydrazine hydrate added is 50 times of nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 120 DEG C of constant temperature 5h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel metal nanometer line,
(2) above-mentioned ferronickel nano wire is placed in the hydrochloric acid solution ultrasonic agitation 24h that pH value is 6, the ratio of ferronickel nano wire and hydrochloric acid is 200ml hydrochloric acid every gram of ferronickel nano wire, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano wire is dispersed into as ferronickel nano particle;
(3) by dispersion after ferronickel nano particle be placed in pH value be 9 sodium hydroxide solution stir 3h, the ratio of ferronickel nano particle and sodium hydroxide solution is 150ml sodium hydroxide solution every gram of ferronickel nano particle, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 80 ~ 120 DEG C of constant temperature 2 ~ 10h, be separated magnetic product with magnetic field, clean twice respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano particle is reassembled into ferronickel nano wire.
Embodiment 4
Dispersion and the assemble method of the ferronickel system metal nanometer line of the present embodiment carry out according to following steps:
(1) by nickel acetate and ferrous nitrate according to mol ratio 1:9 mixed dissolution in deionized water, form ferronickel salting liquid, the volume of deionized water is 800ml/g ferronickel salt, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel and iron is 1:1, then hydrazine hydrate is added, the hydrazine hydrate added is 60 times of nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 150 DEG C of constant temperature 1h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel metal nanometer line,
(2) above-mentioned ferronickel nano wire is placed in hydrochloric acid solution ultrasonic agitation 0.5 ~ 24h that pH value is 5, the ratio of ferronickel nano wire and hydrochloric acid is 150ml hydrochloric acid every gram of ferronickel nano wire, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano wire is dispersed into as ferronickel nano particle;
(3) by dispersion after ferronickel nano particle be placed in pH value be 10 sodium hydroxide solution stir 2.5h, the ratio of ferronickel nano particle and sodium hydroxide solution is 200ml sodium hydroxide solution every gram of ferronickel nano particle, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 100 DEG C of constant temperature 6h, be separated magnetic product with magnetic field, clean twice respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano particle is reassembled into ferronickel nano wire.
Embodiment 5
Dispersion and the assemble method of the ferronickel system metal nanometer line of the present embodiment carry out according to following steps:
(1) by nickel chloride and ferrous acetate according to mol ratio 5:1 mixed dissolution in deionized water, form ferronickel salting liquid, the volume of deionized water is 600ml/g ferronickel salt, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel and iron is 2:1, then hydrazine hydrate is added, the hydrazine hydrate added is 30 times of nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 100 DEG C of constant temperature 10h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel metal nanometer line,
(2) above-mentioned ferronickel nano wire is placed in the hydrochloric acid solution ultrasonic agitation 0.5h that pH value is 3, the ratio of ferronickel nano wire and hydrochloric acid is 100ml hydrochloric acid every gram of ferronickel nano wire, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano wire is dispersed into as ferronickel nano particle;
(3) by dispersion after ferronickel nano particle be placed in pH value be 12 sodium hydroxide solution stir 0.5h, the ratio of ferronickel nano particle and sodium hydroxide solution is 100ml sodium hydroxide solution every gram of ferronickel nano particle, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 90 DEG C of constant temperature 9h, be separated magnetic product with magnetic field, clean twice respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel nano particle is reassembled into ferronickel nano wire.
Claims (6)
1. the dispersion of ferronickel system metal nanometer line and an assemble method, is characterized in that carrying out according to following steps:
(1) mixture of soluble nickel salt or soluble nickel salt and soluble ferrite is dissolved in deionized water, form nickel salt or ferronickel salting liquid, under nitrogen protection, in solution, add natrium citricum and mix, the ratio of the total mole number of the natrium citricum added and nickel or nickel and iron is (1 ~ 2): 1, then hydrazine hydrate is added, the hydrazine hydrate added is 20 ~ 60 times of nickel or nickel and iron total mole number, above-mentioned solution system is transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 100 ~ 150 ° of C constant temperature 1 ~ 10 h, the product deionized water obtained and ethanol washing, dry up with nitrogen, obtain ferronickel system metal nanometer line,
(2) above-mentioned ferronickel system metal nanometer line is placed in hydrochloric acid solution ultrasonic agitation 0.5 ~ 24h that pH value is 3 ~ 6, magnetic product is isolated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel system metal nanometer line is dispersed into as ferronickel system metal nanoparticle;
(3) the ferronickel system metal nanoparticle after dispersion is placed in sodium hydroxide solution stirring 0.5 ~ 3h that pH value is 8 ~ 12, then be transferred in hydrothermal reaction kettle, room temperature is naturally cooled to after 80 ~ 120 ° of C constant temperature 2 ~ 10 h, magnetic product is separated with magnetic field, twice is cleaned respectively with deionized water and ethanol, dry up with nitrogen, now, ferronickel system metal nanoparticle is reassembled into ferronickel system metal nanometer line.
2. the dispersion of a kind of ferronickel system according to claim 1 metal nanometer line and assemble method, it is characterized in that described soluble nickel salt is nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate, described soluble ferrite is ferrous sulfate, frerrous chloride, ferrous nitrate, ferrous acetate.
3. the dispersion of a kind of ferronickel system according to claim 1 metal nanometer line and assemble method, is characterized in that described soluble nickel salt and soluble ferrite can according to any mixed in molar ratio.
4. the dispersion of a kind of ferronickel system according to claim 1 metal nanometer line and assemble method, is characterized in that the ratio of the mixture of described deionized water and soluble nickel salt or soluble nickel salt and soluble ferrite is the mixture of 100 ~ 1000ml water every gram of soluble nickel salt or soluble nickel salt and soluble ferrite.
5. the dispersion of a kind of ferronickel system according to claim 1 metal nanometer line and assemble method, is characterized in that the ratio of described ferronickel system metal nanometer line and hydrochloric acid is 100 ~ 200ml hydrochloric acid every gram of metal nanometer line.
6. the dispersion of a kind of ferronickel system according to claim 1 metal nanometer line and assemble method, is characterized in that the ratio of described ferronickel system metal nanoparticle and sodium hydroxide solution is 100 ~ 200ml sodium hydroxide solution every gram of metal nanoparticle.
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CN105947971A (en) * | 2016-05-26 | 2016-09-21 | 清华大学深圳研究生院 | Preparation method of ferromagnetic nanowire array |
CN107252674A (en) * | 2017-07-21 | 2017-10-17 | 中国环境科学研究院 | A kind of dephosphorization agent based on ferronickel binary hydrotalcite |
CN108274020A (en) * | 2018-04-10 | 2018-07-13 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of superfine spherical ferronickel powder |
CN110976898A (en) * | 2019-12-12 | 2020-04-10 | 沈阳工业大学 | Soft magnetic metal iron porous micron wire and preparation method thereof |
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CN107252674A (en) * | 2017-07-21 | 2017-10-17 | 中国环境科学研究院 | A kind of dephosphorization agent based on ferronickel binary hydrotalcite |
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