CN101758242A - Preparation method of ultrahigh monodisperse nickel sol for preparing colloidal crystal - Google Patents
Preparation method of ultrahigh monodisperse nickel sol for preparing colloidal crystal Download PDFInfo
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- CN101758242A CN101758242A CN200910128181A CN200910128181A CN101758242A CN 101758242 A CN101758242 A CN 101758242A CN 200910128181 A CN200910128181 A CN 200910128181A CN 200910128181 A CN200910128181 A CN 200910128181A CN 101758242 A CN101758242 A CN 101758242A
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Abstract
The invention discloses a preparation method of ultrahigh monodisperse nickel sol for preparing colloidal crystal. The preparation method is characterized in comprising the steps of: dropping protective agent solution with weight percentage concentration of 1-7% into nickel-containing main solution with weight percentage concentration of 3-13%, and evenly stirring; and inserting the solution into high-energy ultrasonic wave energy converter; and leading the ultrasonic wave energy converter to work according to the specific timing sequence given by an ultrasonic wave controller; and applying timing sequence ultrasonic wave to the solution. When impulse ultrasound works, reducing solution is added gradually, wherein the reducing solution is mixed solution by mixing organic reducing agent with weight percentage concentration of 1-10% with alkaline solution with weight percentage concentration of 10-20%. The granularity of sol grains synthesized by the method can be changed from 5 nanometers to 500 nanometers through the parameter of ultrasound timing sequence. The distribution of grain diameter is narrow, wherein the standard deviation of the average granularity of the nickel sol grains is within 5%. The method is simple and easy, and is particularly suitable for directly preparing the colloidal crystal with high quality and large size.
Description
Technical field
The present invention relates to a kind of manufacture method technical field of ultrahigh monodisperse nickel Nano sol.
Background technology
We often only paid attention to powder diameter is controlled to observe the special photoelectricity that may occur of reducing along with grain graininess to the research of nano particle in the past, magnetic, yet catalytic property. produce the not available character of some elementary cells even as a kind of can being showed by the special nature of nano material-those elementary cells (nano particle) of applied material in our the productive life reality-become by the basic structural group of nanometer, depend on also that to a great extent these elementary cells form the institutional framework of macroscopical block. such as, two kinds of submicrometer structure unit with differing dielectric constant are at one dimension, the photonic crystal that alternately extending on two dimension or the three-dimensional formed has incomparable handling to visible light, visible light, near-infrared, when the infrared band photon is propagated therein because Bragg diffraction, electromagnetic wave can be modulated and be formed band structure, dropping in the photon band gap light can not propagate, therefore suppress or the spontaneous radiation of enhancing light, there is not the threshold value laser instrument at high Q, the super narrow-band filtering frequency-selector of high-quality, photoelectron and integrated opto-electronic devices such as efficient photon completely reflecting mirror, in the miniature optical element of integrated optical circuit and the light transmission process device wide application prospect (Fang N is arranged, Lee H, Sun C et al.Science, 2005,308,534).Be expected to become the basic material that leads following optical communication, integrated photonic device, novel high speed computer.And the colloidal crystal that colloidal nanoparticles periodicity emphasis complex spatially becomes the in these years emphasis of material science scientists study and focus especially have potential significant application value at the nano-device of field colloidal crystal classes such as catalysis, communication, electronics, semiconductor and military affairs.Yet these preparation of devices have very strict requirement to the shape of the basic structural unit that constitutes these devices and the uniformity and the controllability of granularity.Lattice point particle diameter standard deviation just can cause the photonic crystal functional characteristic to reduce as if＞5% or disappear.Have only being of similar shape of these nano structured units, yardstick can spatially periodically be arranged in the structure of rule uniformly, and also have only the yardstick and the shape of these basic structures are effectively controlled, just can be finely tuned the character of nano-device.So, seek and a kind ofly can effectively control the nano particle yardstick and keep shape of particle and the highly homogeneous preparation method of granularity is that these nano-devices move towards the important prerequisite used, also be the new focus in present investigation of materials field.
Nucleation and nucleus growth from crystal growth
Theoretical (Clemens Burda, Xiaobo Chen, RadhaNarayanan, Mostafa A.El-Sayed, Chem.Rev.2005,105,1025.), if obtain the good monodisperse particle of uniform particles degree, be wherein key to the control of crystal nucleation and nucleus growth speed.At first initial reaction stage is wished can fast reaction to improve as far as possible the solution saturation degree and is impelled disposable a large amount of nucleation in the short time.After nucleus forms, the degree of supersaturation of solution is reduced under the critical value, subsequent reaction speed need be controlled at the material consumption speed that causes with nucleus growth does not quite have new nucleus to form to keep constant degree of supersaturation and to guarantee in this stage, make the colloidal particle granularity owing to sized particles speed of growth difference trends towards single dispersion (Peng, X., Wickham, J., Alivisatos, A.P., J.Am.Chem.Soc.1998,120,5343.) avoid simultaneously causing critical grain size to increase the Ostwald defocusing that causes because degree of supersaturation descends.(growth) time of drawing of control colloidal particle just can be realized the regulation and control to the colloidal particle granularity in this process, and must take appropriate measures in addition (as adding suitable surfactant selective absorption on the colloidal particle surface) prevents the offspring gathering that colloidal solid causes because of running foul of each other.The preparation of the height list dispersion colloid particle of some reported in literature is just according to this principle contrived experiment, as quick interpolation (a large amount of nucleation in the short time) and/or reaction system high temperature/low temperature (control reaction speed and solubility) (Peng, the Z.A. of reactant; Peng, X.J.Am.Chem.Soc.2001,123,183.).Yet the speed that the control reactant adds and the quick variation of system temperature are difficult to receive desirable effect sometimes.We know that the sufficient intensity ultrasonic wave can cause acoustic cavitation in liquid-phase system, bubble formation in the ultrasonic excitation liquid, growth, contraction, regrowth, contraction again, through periodically concussion, these bubble populations finally at full speed burst apart, and discharge huge energy, and generation speed is high to 110mS
-1The height microjet; Cavitation bubble can produce local high temperature (about 5000K) in the moment of blast, local high pressure (about 100Mpa), and the speed of heating and cooling is greater than 10
10K/S.These extreme conditions can the speed as reactions such as hydrolysis, redox of carrying out be tens of times lifting so that nano-colloid particle nucleation is rely, thereby control reaction rate apace, obtain the highly homogeneous sol particles of granularity.
In sum, the physicochemical characteristic of impulse ultrasound in liquid-phase system of intensity and sequential appropriate design is very beneficial for the preparation of highly single dispersion, the controlled sol particles of particle diameter.
Though ultrasonic wave as a kind of means of nano materials be suggested and be subjected to paid certain attention (Li Chunxi, prince's pick,
The chemistry circular,
2001 (5), 268-271.), a collection of report that utilizes the ultrasonic wave radiation to prepare nanoparticle has appearred, as Zhang Kai (Zhang Kai, Fu Qiang, Fan Jinghui, Zhou Dehui, Materials Letters, preparation Ag/PS complex microsphere under ultrasonic radiation such as 2005,59 (28), 3682.); Dantsin G. (Dantsin G., Suslick K.S., J.Am Chem.Soc.2000,122,5214.) etc. has prepared attached to the Mo on the molecular sieve
2The C nanoparticle; Okitsu and Qiu Xiaofeng (Qiu Xiaofeng, Zhu person of outstanding talent, Chinese Journal of Inorganic Chemistry, 2003,19 (7), 766.) prepared nanometer palladium particle; From present applicable cases both domestic and external, great majority research prepares nano particle as a kind of supplementary means usually under supersonic wave cleaning machine (power is less than 200W) mode of operation, the input power of this cleaning machine generally has only tens to 100 watts, and the water yield is more in the water-bath, power density is very little, the mode of effect is single continuous ultrasound, the monodispersity of the nanoparticle that obtains not is very desirable, the standard deviation that is difficult to accomplish particle also is difficult to the sol particle that regulation and control easily obtain different-grain diameter (several nanometers-tens nanometer) less than 5%.
It as number of patent application 02148673.5 Chinese patent application " a kind of method that in the aqueous solution, prepares nanometer nickel and alloy powder thereof " with chemical reduction method; this method is the main salt of 40～120g/L with content; the reducing agent of 10～100g/L; the additive A of 1～10mg/L; the additive B of 10～50g/L; the addition of C of 20～60g/L is evenly mixed; be heated to 70～90 ℃; add ultrasonic field; after treating that material reaction produces nickel powder; the material that will contain nickel powder with condenser is cooled to room temperature; separate nickel powder and solution with supercentrifuge; nickel powder is dry under protective atmosphere, obtained the nanometer nickel-base alloy powder.Therefrom we see that adding ultrasonic field in the preparation process has only 100-200 watt, finish in water-bath because of entire reaction again, the ultrasonic power density of reactive site is very little, the mode of action is simple continuous ultrasound, lack the effective and reasonable ultrasonic control of sequential, less to the control action that is reacted into crystalline nucleation and growth of sodium rice nickel particle.The number average bead diameter of the nickel particle that it obtains is difficult to satisfy the application on some occasion more than 50 nanometers.Secondly, the final products of this technology are pulverous nano nickle granules, (as electrocondution slurry) also needs to be deployed into suspension in the use of a lot of occasions, trouble in the use, inconvenience, even in the process of allotment slurry, can further cause the reunion of its particle, granularity increases, and purity descends, and influences the performance of slurry.Moreover its reducing agent has adopted the very strong reducing agent of inorganic reduction performance, also is unfavorable for the synthetic little particle of particle diameter, and has certain toxicity, cause environmental pollution easily, similar problem, also being present in number of patent application is in the patent application technology of 01107728.X.
Compare the single small particle diameter nanometer nickel sol that disperses of the water vast Chinese invention patent 200410067965.9 flash ultrasonic waves preparation that wait to propose, though also adopted strong ultrasonic, but because the ultrasonication mode does not design according to the nucleus growth theory, just comparatively simple impulse ultrasound, from the figure that patent provides, the particle diameter uniformity coefficient has been compared tangible gap with the present invention.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of sequential the strong ultrasonic method for preparing height dispersed nano nickel sol at existing background technology, and its synthetic nano nickle granules number average bead diameter can change between tens nanometers in several nanometers by regulating ultrasonic sequential.High degree of dispersion, number average bead diameter standard deviation are in 5%, and equipment is simple relatively, speed is fast, and efficient height, the nickel sol of acquisition are particularly suitable for preparing the large-sized colloidal crystal device of high-quality.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the strong ultrasonic method for preparing height dispersed nano nickel sol of this sequential; it is characterized in that nickeliferous main salting liquid at 3～13% mass percent concentrations drips the protective agent solution of 1～7% mass percent concentration and stirs; insert the high-energy ultrasonic wave transducer in the solution; and the specific time sequence work that this ultrasonic transducer is provided by ultrasonic controller; solution is applied the sequential ultrasonic field; in impulse ultrasound work; add reducing liquid gradually; this reducing liquid is selected the organic reducing agent of 1～10% mass percent concentration and the composite mixed liquor of alkaline solution of 10～20% mass percent concentrations for use; their mixed volumes ratio is 1: 0.8～1.2; adding reducing liquid amount is 1.1～1.6 times of nickeliferous main salting liquid volume; after the reducing liquid adding finishes; the temperature of the hierarchy of control 30～40 degrees centigrade and keep 30～50 minutes after; take out reactant, promptly get highly dispersed nano nickel sol after the solution that obtains is removed small ion.
Above-mentioned supersonic generator power bracket is 1000～3000 watts/100 milliliters nickeliferous main salting liquids, the position of ultrasonic probe under liquid level 3-5 centimetre, this ultrasonic sequential is 10-30 one-period second, the pulse of each cycle with 100 milliseconds of-1 second width 1-3 kilowatt intensity begins, it then is the 1-3 blank of second, following by intensity is the 1/10-1/20 of 1-3 kilowatt of pulse strength, and time remaining is the 7-29 low energy impulse ultrasound of second, and such cycle carries out 60-150 time; Whole process is by regulating particle diameter and the epigranular degree that a plurality of technical parameters such as length pulsed ultrasonic power, length impulse ultrasound time, blank space time, number of cycles are regulated the product nano nickle granules, and method is simple, implements easily.
Above-mentioned nickeliferous main salting liquid can be selected for use in nickelous sulfate, nickel acetate, the nickel chloride, nickel nitrate one or more.
Very useful is, above-mentioned ultrasonic transducer directly inserts in the reaction system, and it can directly be distributed in ultrasound field in the solution, improves power density and be beneficial in the crystallization of particle and growth course effectively to stop particle to be reunited because of running foul of each other.
Very useful is, above-mentioned organic reducing agent is selected ascorbic acid, glucose or the more weak organic reducing agent of hydroxylamine hydrochloride reproducibility for use, they are natural organic matter, basically there is not toxicity, and cost is cheap, reproducibility is medium on the weak side, do not apply strong ultrasonic can not reduced nickel master salt, be beneficial to ultrasonic wave reaction speed directly and fast controlled.
Very useful is; above-mentioned protective agent solution selects for use the solution of polyethylene pyrrolidone PVP, PVAC polyvinylalcohol, shitosan a kind of; it makes protective agent form the macromolecule network system of a three-dimensional in the environment of solution; stop the nickel particle that forms in the chemical reaction process owing to growth is condensed in collision, thereby be beneficial to the homogeneity of keeping the nickel sol particle diameter.
Above-mentioned alkaline solution is selected a kind of in NaOH, barium hydroxide or the aqua calcis for use.
Very useful is, this ultrasonic sequential one-period is made of three parts, first is 100ms to the high strength (1-3KW) of 1s and very narrow pulse, this pulse can make to be reflected at and take place in the extremely short time and in the instantaneous a large amount of nucleation of product in addition, this nucleation process can not take place in other period; The intermittent time of second part 1-3 second be used for making during previous strong short pulse in the micelle of nucleation stable; Last 7-29 intensity second is used for providing lentamente crystal growth needed product for the weak long period of short pulse intensity 1/10-1/20 is ultrasonic, and match with the speed of material dropping and to keep the constant degree of supersaturation of solution, thereby obtain highly monodispersed sol particles.
Compared with prior art, the invention has the advantages that: the granularity of the nickel sol particle that it is synthetic can change to 500 nanometers from 5 nanometers by the parameter of ultrasonic sequential; Particle diameter distributes very narrow, and the standard deviation of the number average particle size of nickel sol particle is within 5%, and method is simple, is particularly suitable for directly preparing colloidal crystal.Colloidal crystal (colloidal-crystal) is the long range ordered structure that monodispersed colloidal solid self-organizing forms, and is one of research focus of physics, chemistry, material science in recent years.The colloidal particle granularity that constitutes crystal lattice can be nanometer, sub-micron, micron, distinct characteristic of each self-forming and application.There are not photoelectron and integrated opto-electronic devices such as threshold value laser instrument, the super narrow-band filtering frequency-selector of high-quality, efficient photon completely reflecting mirror at high Q, in the integrated information carrier of the miniature optical element of integrated optical circuit and light transmission process device, the full light of nanometer, nanocomposite optical imaging, the nano-photoetching wide application prospect is arranged, be expected to become the basic material that leads following optical communication, integrated photonic device, novel high speed computer.Above-mentioned ultrasonic transducer directly inserts in the reaction system, and it can directly be distributed in ultrasound field in the solution, improves power density and be beneficial in the crystallization of particle and growth course effectively to stop particle to be reunited because of running foul of each other.Macromolecule network system in conjunction with good organic reducing agent and protective agent solution three-dimensional; stop the nickel particle that forms in the chemical reaction process owing to growth is condensed in collision, be beneficial to the uniform particle diameter of keeping nickel sol, whole process speed is fast; the efficient height is beneficial to it and applies.In a word, the invention provides a kind of method for preparing height monodisperse sol micelle, the granularity of using the synthetic sol particle of this method can change to 500 nanometers from 5 nanometers by the parameter of ultrasonic sequential.Particle diameter distributes very narrow, and the standard deviation of the number average particle size of nickel sol particle is within 5%.
Description of drawings
Fig. 1 is the AFM figure of nanometer nickel sol particle;
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Examples of implementation 1
Certain density main salt nickelous sulfate is mixed with the solution 100mL of 10wt% and adds several protective agents; protective agent is a kind of in the shitosan (shrimp shell or crab shell); concentration is 3wt%; be loaded in the beaker of certain volume; mixed liquor placed on the magnetic stirring apparatus stirred 5 minutes; then this beaker is put into the direct insertion processor of ultrasonic wave, about 4 centimetres away from liquid level of ultrasonic wave transmitting terminals be.Regulate ultrasonic intensity 1500w, this ultrasonic sequential is 15 seconds one-periods, the pulse of each cycle with 1500 watts of intensity of 20 milliseconds of width begins, it then is 2 seconds blank, following by intensity is 1/10 of 1.5 kilowatts of pulse strengties, time remaining is 10 seconds a low energy impulse ultrasound, and such cycle carries out 70 times.Select 15 millimeters of ultrasonic wave end face diameters for use.Begin to drip reducing agent liquid after ultrasonic instrument begins to start, reducing liquid is that concentration is the mixed liquor of the sodium hydroxide solution of the more weak organic reducing agent of the ascorbic acid reproducibility of 5wt% and isopyknic 15wt%.Dropping must be carried out off and on, and is synchronous with hyperacoustic flash stage, and drips near the ultrasonic wave emitting facet.Amounting to the amount that adds reducing liquid continues ultrasonic up to reaching total degree for the 130mL. reactant liquor drips the back.The temperature of regulation system is 40 degrees centigrade and kept 40 minutes.Take out product, promptly obtain height dispersed nano nickel sol after the solution that obtains is removed small ion in the solution through dialysis.Its particle diameter of nanometer nickel sol can be controlled at 5～500 nanometer range, see Fig. 1,6.000 microns of its scan size Scan size, scan frequency Scan rate 1.001Hz, the Number of samples of catalogue number(Cat.No.) 256, pictorial data Image Data height H eight, data area Data scale 60nm, particle diameter distributes very narrow, and the particle number average bead diameter is about 45nm.
Examples of implementation 2
Certain density main salt nickel chloride is mixed with the solution 100mL of 5wt% and adds several protective agents; protective agent is polyethylene pyrrolidone PVP; concentration is 5wt%; be loaded in the beaker of certain volume; mixed liquor placed on the magnetic stirring apparatus stirred 5 minutes; then this beaker is put into the direct insertion processor of ultrasonic wave, about 4 centimetres away from liquid level of ultrasonic wave transmitting terminals be.Regulate ultrasonic intensity 2000w, this ultrasonic sequential is 20 seconds one-periods, the pulse of each cycle with 2000 watts of intensity of 40 milliseconds of width begins, it then is 2.5 seconds blank, following by intensity is 1/10 of 2.0 kilowatts of pulse strengties, time remaining is 12 seconds a low energy impulse ultrasound, and such cycle carries out 100 times.Select 15 millimeters of ultrasonic wave end face diameters for use.Begin to drip reducing agent liquid after ultrasonic instrument begins to start, reducing liquid is that concentration is the mixed liquor of the barium hydroxide solution of the more weak organic reducing agent of the hydroxylamine hydrochloride reproducibility of 9wt% and isopyknic 15wt%.Dropping must be carried out off and on, and is synchronous with hyperacoustic flash stage, and drips near the ultrasonic wave emitting facet.Amounting to the amount that adds reducing liquid continues ultrasonic up to reaching total degree for the 120mL. reactant liquor drips the back.The temperature of regulation system is 40 degrees centigrade and kept 45 minutes.Take out product, promptly obtain height dispersed nano nickel sol after the solution that obtains is removed small ion in the solution through dialysis.
Examples of implementation 3
Certain density main salt nickel acetate is mixed with the solution 100mL of finite concentration 13wt% and adds several protective agents, and protective agent is a PVAC polyvinylalcohol, and concentration is 2wt%, is loaded in the beaker of certain volume, mixed liquor is placed on the magnetic stirring apparatus stirred 15 minutes.Then this beaker is put into the direct insertion processor of ultrasonic wave, about 4 centimetres away from liquid level of ultrasonic wave transmitting terminals be.Regulate ultrasonic intensity 2500w, this ultrasonic sequential is 25 seconds one-periods, the pulse of each cycle with 2500 watts of intensity of 42 milliseconds of width begins, it then is 2.8 seconds blank, following by intensity is 1/15 of 2.5 kilowatts of pulse strengties, time remaining is 10 seconds a low energy impulse ultrasound, and such cycle carries out 120 times.Select 15 millimeters of ultrasonic wave end face diameters for use.Begin to drip reducing agent liquid after ultrasonic instrument begins to start, reducing liquid is that concentration is the mixed liquor of the aqua calcis of the more weak organic reducing agent of the glucose reproducibility of 1wt% and isopyknic 17wt%.Dropping must be carried out off and on, and is synchronous with hyperacoustic flash stage, and drips near the ultrasonic wave emitting facet.Amounting to the amount that adds reducing liquid continues ultrasonic up to reaching total degree for the 150mL. reactant liquor drips the back.The temperature of regulation system is 30 degrees centigrade and kept 30 minutes.Take out product, promptly obtain height dispersed nano nickel sol after the solution that obtains is removed small ion in the solution through dialysis.
Examples of implementation 4
Certain density main salt nickel nitrate and nickel chloride are mixed with the solution 100mL of finite concentration 10wt% and add several protective agents with 2: 1 mass ratios; protective agent is a kind of in polyethylene pyrrolidone PVP, PVAC polyvinylalcohol, the shitosan (shrimp shell or crab shell); concentration is 3wt%; be loaded in the beaker of certain volume, mixed liquor placed stir 10～20 minutes on the magnetic stirring apparatus.Then this beaker is put into the direct insertion processor of ultrasonic wave, about 4 centimetres away from liquid level of ultrasonic wave transmitting terminals be.Regulate ultrasonic intensity 2500w, this ultrasonic sequential is 25 seconds one-periods, the pulse of each cycle with 2500 watts of intensity of 42 milliseconds of width begins, it then is 2.3 seconds blank, following by intensity is 1/20 of 2.5 kilowatts of pulse strengties, time remaining is 15 seconds a low energy impulse ultrasound, and such cycle carries out 130 times.Select 15 millimeters of ultrasonic wave end face diameters for use.Begin to drip reducing agent liquid after ultrasonic instrument begins to start, reducing liquid is that concentration is a kind of mixed liquor in NaOH, barium hydroxide or the calcium hydroxide of a kind of and isopyknic 15wt% in the more weak organic reducing agent of reproducibility such as the ascorbic acid, glucose, hydroxylamine hydrochloride of 7wt%.Dropping must be carried out off and on, and is synchronous with hyperacoustic flash stage, and drips near the ultrasonic wave emitting facet.Amounting to the amount that adds reducing liquid is 140mL.Reactant liquor drips the back and continues ultrasonic up to reaching total degree.The temperature of regulation system is 35 degrees centigrade and kept 30 minutes.Take out product, promptly obtain height dispersed nano nickel sol after the solution that obtains is removed small ion in the solution through dialysis.
Claims (8)
1. a flash ultrasonic wave prepares single method of disperseing small particle diameter nanometer nickel sol; it is characterized in that nickeliferous main salting liquid at 3～13% mass percent concentrations drips the protective agent solution of 1～7% mass percent concentration and stirs; insert the high-energy ultrasonic wave transducer in the solution; and the specific time sequence work that this ultrasonic transducer is provided by ultrasonic controller; solution is applied the sequential ultrasonic field; in impulse ultrasound work; add reducing liquid gradually; this reducing liquid is selected the organic reducing agent of 1～10% mass percent concentration and the composite mixed liquor of alkaline solution of 10～20% mass percent concentrations for use; their mixed volumes ratio is 1: 0.8～1.2; adding reducing liquid amount is 1.1～1.6 times of nickeliferous main salting liquid volume; after the reducing liquid adding finishes; the temperature of the hierarchy of control 30～40 degrees centigrade and keep 30～50 minutes after; take out reactant, promptly get highly dispersed nano nickel sol after the solution that obtains is removed small ion.
2. method according to claim 1, it is characterized in that described supersonic generator power bracket is 1000～3000 watts/100 milliliters nickeliferous main salting liquids, the position of ultrasonic probe under liquid level 3-5 centimetre, this ultrasonic sequential is 10-30 one-period second, the pulse of each cycle with 100 milliseconds of-1 second width 1-3 kilowatt intensity begins, it then is the 1-3 blank of second, follow by intensity is the 1/10-1/20 of 1-3 kilowatt of pulse strength, time remaining is the 7-29 low energy impulse ultrasound of second, and such cycle carries out 60-150 time.
3. method according to claim 1 and 2 is characterized in that described processor for ultrasonic wave selects direct insertion processor for ultrasonic wave for use.
4. method according to claim 1 is characterized in that described nickeliferous main salting liquid selects for use in nickelous sulfate, nickel acetate, nickel chloride, the nickel nitrate one or more as main salt.
5. method according to claim 1 is characterized in that described protective agent solution selects for use the solution of polyethylene pyrrolidone PVP, PVAC polyvinylalcohol, shitosan a kind of.
6. method according to claim 1 is characterized in that described organic reducing agent selects ascorbic acid, glucose or the more weak organic reducing agent of hydroxylamine hydrochloride reproducibility for use.
7. method according to claim 1 is characterized in that described alkaline solution selects for use the solution of NaOH, barium hydroxide or calcium hydroxide a kind of.
8. method according to claim 1 is characterized in that its particle number average bead diameter of described nanometer nickel sol can change to 500 nanometers from 5 nanometers.Particle is even, and the number average bead diameter standard deviation is in 5%.
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| CN102699348A (en) * | 2012-07-02 | 2012-10-03 | 昆明理工大学 | Method of preparing micron-sized spherical high-purity nickel powder |
| CN104105562A (en) * | 2012-02-09 | 2014-10-15 | 田中贵金属工业株式会社 | Metal colloidal solution and method for producing same |
| CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | A kind of preparation method of chain-like metal Ni nanopowders |
| CN108636437A (en) * | 2018-05-09 | 2018-10-12 | 天津理工大学 | A kind of preparation method of the monatomic catalyst of nitrogen-doped carbon carried metal |
| CN111618314A (en) * | 2020-05-15 | 2020-09-04 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of nano silver-coated copper solder based on sonochemistry |
| CN113976905A (en) * | 2016-03-18 | 2022-01-28 | 住友金属矿山株式会社 | Nickel powder, method for producing nickel powder, and internal electrode paste and electronic component using nickel powder |
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| CN104105562A (en) * | 2012-02-09 | 2014-10-15 | 田中贵金属工业株式会社 | Metal colloidal solution and method for producing same |
| CN104105562B (en) * | 2012-02-09 | 2017-02-22 | 田中贵金属工业株式会社 | Metal colloidal solution and method for producing same |
| CN102699348A (en) * | 2012-07-02 | 2012-10-03 | 昆明理工大学 | Method of preparing micron-sized spherical high-purity nickel powder |
| CN113976905A (en) * | 2016-03-18 | 2022-01-28 | 住友金属矿山株式会社 | Nickel powder, method for producing nickel powder, and internal electrode paste and electronic component using nickel powder |
| CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | A kind of preparation method of chain-like metal Ni nanopowders |
| CN108500292B (en) * | 2018-04-08 | 2021-03-23 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
| CN108636437A (en) * | 2018-05-09 | 2018-10-12 | 天津理工大学 | A kind of preparation method of the monatomic catalyst of nitrogen-doped carbon carried metal |
| CN111618314A (en) * | 2020-05-15 | 2020-09-04 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of nano silver-coated copper solder based on sonochemistry |
| CN111618314B (en) * | 2020-05-15 | 2023-01-03 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of nano silver-coated copper solder based on sonochemistry |
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