CN109136997A - A kind of pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder - Google Patents
A kind of pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder Download PDFInfo
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Abstract
The present invention provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic metallic powder, and the electrolyte system includes electrolyte, pH buffer and dispersing agent；The electrolyte is the sulfate or chlorate of metal；The concentration of metal ion is 0.5 ~ 2 mol/L in the electrolyte, and the concentration of pH buffer is 5 ~ 10 g/L in the electrolyte system, and the concentration amount of dispersing agent is 0.5 ~ 12 g/L in the electrolyte system.The present invention adds dispersing agent in electrolyte system, under the stabilization pH value that pH buffer adjusts control, utilize the synergistic effect of the two, realize the regulation of the composition of product, granularity and pattern, and it is uniform by the ultra-fine magnetic metallic powder particle that electrolyte circulation is received, particle size distribution range is narrow, good dispersion, prepares the yield of products obtained therefrom using electrolyte system of the invention and degree of purity effectively improves.
Description
Technical field
The invention belongs to magnetic nanometer powder preparation technical fields, prepare more particularly, to a kind of pulse-electrodeposition process
The electrolyte system of ultra-fine magnetic metallic powder.
Background technique
Nano-magnetic powder shows the unique physics different from conventional magnetic material, chemistry as a kind of new material
And electromagnetic property, and have a wide range of applications in fields such as machinery, electronics, optics, magnetics, chemistry and biologies, in state of the world
Extremely important effect is played in people's economy and military field.Currently, the common preparation method of magnetic nano-particle has gas phase
Reaction method, coprecipitation, Hydrolyze method and electrodeposition process etc..
Wherein, gas-phase reaction method be using compound steam chemical reaction a kind of method, though this method can synthesize compared with
Good nanometer powder, but it is ineffective for preparing not volatile substance；Co-electrodeposition method is dissolved in water using various
Substance, it is reacted to generate undissolved hydroxide, carbonate, sulfate etc., then heated decomposition generation ultra-micro powder, this side
Though method is simple and easy, that there are impurity is more for obtained ultra-micro powder, reunites the problems such as serious, and for certain metal simple-substances
Preparation be not easy to realize；Hydrolyze method is high-purity ultra-micro powder needed for being directly separated manufacture from the solution of substance, due to making
With the organo-metallic compound needed when Hydrolyze method by a large amount of valuableness, lead to that increased production cost, and there is pollution environment, instead
The problems such as answering process slow；And electrodeposition process refers to that metal or alloy is electric from its compound water solution, non-aqueous solution or fused salt
The process of chemical deposition, is compared with other methods, and electrodeposition process is with easy to operate, equipment is simple, low energy consumption and application range
The features such as wide, therefore, electrodeposition process, become the research hotspot for preparing nano-magnetic powder.
But nanometer magnetic metal powder is prepared using electrodeposition process and is had the following problems:
(1) how to effectively control the composition that electrodeposition process prepares electrolyte in nanometer magnetic metal powder process, acquisition groups
At relatively stable and satisfaction continuous operation electrolyte system.
(2) agglomeration traits of prepared nanometer magnetic metal powder how to be solved.
(3) how to solve the problems, such as that prepared magnetic metallic powder is nanoscale.
Therefore, research and development meet electrodeposition process prepare metal powder needs electrolyte system have very important significance.
Summary of the invention
The purpose of the present invention is to provide a kind of electrolyte systems, prepare ultra-fine magnetic gold to meet pulse-electrodeposition process
Belong to the requirement in powder process, the nano-scale magnetic metal powder of partial size and morphology controllable is obtained, using above-mentioned electrolyte
It is that the ultra-fine magnetic metallic powder being prepared has the characteristics that yield and degree of purity are high.
The technical solution adopted is as follows:
A kind of electrodeposition process prepares the electrolyte system of nanometer magnetic metal powder, and the electrolyte system includes electrolysis
Liquid, pH buffer and dispersing agent；The electrolyte is the sulfate or chlorate of metal；Metal ion is dense in the electrolyte
Degree is 0.5~2mol/L, and the concentration of pH buffer is 5~10g/L in the electrolyte system, is dispersed in the electrolyte system
The concentration amount of agent is 0.5~12g/L.
Further, the concentration of metal ion is 1~2mol/L in the electrolyte.
Further, the concentration of pH buffer is 5~8g/L in the electrolyte system, is dispersed in the electrolyte system
The concentration amount of agent is 2~6g/L.
The present invention uses specific dispersing agent, carries out surface to particle first and is modified, its surface is made to cover one layer of polymeric,
The effectively nucleating growth of control particle, can also improve the distribution of microcosmic electric current in solution, secondly to reach improvement electrolyte solution
Dispersibility, to obtain uniform, smooth nano metal powder；On the other hand, the particle made is kept in the solution
Dispersity is uniformly coated on the surface of particle, has to prevent from mutually assembling between the fine particle being precipitated in deposition process
The size of the control particle of effect, to reach Nano grade.
In order to enhance the stability and electric conductivity of solution, further, the electrolyte also contains ammonium sulfate.
Further, the concentration of the ammonium sulfate is 0~0.8mol/L.
Further, the pH buffer is boric acid, ammonium salt, acetate, any one in citrate.
Further, the dispersing agent is povidone, thiocarbamide, γ-aminopropyl triethoxysilane, dodecyl sulphate
At least one of sodium.
Further, the magnetic metal is any one in iron, cobalt, nickel and its alloy.
A kind of above-mentioned electrodeposition process prepares the preparation method of the electrolyte system of metal powder, and specific preparation process is as follows:
Electrolyte is configured by concentration ratio deionized water, pH buffer is then proportionally added into, is eventually adding dispersing agent.
Further, described to prepare the equipment that electrolyte system uses as autoclave mixing plant, tubular-mix equipment, static state
Any one in mixing apparatus.
Compared with prior art, the beneficial effects of the present invention are:
Electrolyte system of the invention prepares the particularity of ultra-fine magnetic metallic powder for pulse-electrodeposition process, in electricity
Dispersing agent is added in solution liquid system, under the stabilization pH value that pH buffer adjusts control, using the synergistic effect of the two, realizes and produces
The regulation of the composition of object, granularity and pattern, and, partial size uniform by the ultra-fine magnetic metallic powder particle that electrolyte circulation is received
Narrow distribution range, good dispersion prepare the yield of products obtained therefrom using electrolyte system of the invention and degree of purity effectively improve.
The present invention selects boric acid, citrate etc. to be used as buffer, and electrolyte pH value in electrodeposition process can be made steady
It is fixed, and electrolyte can be made to be under mild acid conditions, meet the requirement of electrodeposition process.
The present invention selects povidone, thiocarbamide etc. to be used as dispersing agent, is not only able to be modified nanoparticle progress surface, prevent
Its dissolution in the electrolytic solution, and its nucleating growth is effectively controlled, the dispersibility of electrolyte can also be improved, to improve super
The dispersibility of thin magnetic metallic powder, avoids reuniting between metal powder, effectively controls the granularity of metal powder.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram for the ultra-fine magnetic powder that the embodiment of the present invention 1 is prepared；
Fig. 2 is the X-ray diffractogram for the ultra-fine magnetic nickel powder that the embodiment of the present invention 3 is prepared.
Fig. 3 is the scanning electron microscope (SEM) photograph for the ultra-fine magnetic powder that the embodiment of the present invention 1 is prepared；
Fig. 4 is the scanning electron microscope (SEM) photograph for the ultra-fine magnetic powder that the embodiment of the present invention 2 is prepared；
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, it is no intended to limit of the invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder, specifically includes
Following steps:
First in autoclave mixing plant, ferrous sulfate solution is configured with deionized water, boric acid is then added, is eventually adding
Povidone and thiocarbamide；
(2) electrolyte system made from forms: ferrous ion concentration 1mol/L, and the concentration of boric acid is in electrolyte system
5g/L, povidone and the concentration of thiocarbamide are respectively 0.5g/L, 3g/L in electrolyte system；
(3) operating procedure for preparing ultra-fine magnetic powder using the electrolyte system is as follows:
S1. electrodeposition process: using iron plate as anode, using stainless steel as cathode, cathode material surface smoothness is 9 μm, is put
It is placed in above-mentioned electrolyte system, the electro-deposition 3h under the pulse field action of ultrasound field and alternating magnetic field, electrodeposition temperature is
40 DEG C, the blackish green powder of one layer of uniform and smooth is obtained on cathode plate；
Wherein, the frequency of ultrasound field is 20KHz, power 300W, and the frequency of alternating magnetic field is 5KHz, interpolar away from for
30mm, pH value 2.5, current density 300A/m2, electric current 0.5A, voltage 2V.
S2. it post-processes: step S1 being passed through into the black powder particle that electro-deposition generates, yin is detached under pulse field action
Pole, and decentralized processing is completed in the electrolytic solution, it is collected in the cyclic process of electrolyte, obtains black fine powder, i.e.,
Ultra-fine magnetic powder.
Embodiment 2
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder, specifically includes
Following steps:
First in tubular-mix equipment, ferrous sulfate solution is configured with deionized water, sodium citrate is then added, finally
Povidone and thiocarbamide is added；
(2) electrolyte system made from forms: ferrous ion concentration 1mol/L, and sodium citrate is dense in electrolyte system
Degree is 5g/L, and povidone and the concentration of thiocarbamide are respectively 8g/L, 2g/L in electrolyte system；
(3) operating procedure of ultra-fine magnetic powder is prepared using the electrolyte system referring to embodiment 1.
Embodiment 3
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic nickel powder, specifically includes
Following steps:
First in autoclave mixing plant, nickel sulfate solution is configured with deionized water, boric acid is then added, is eventually adding ten
Sodium dialkyl sulfate and γ-aminopropyl triethoxysilane；
(2) electrolyte system made from forms: nickel ion concentration 0.5mol/L, and the concentration of boric acid is in electrolyte system
10g/L, lauryl sodium sulfate and γ-aminopropyl triethoxysilane concentration are respectively 5g/L, 12g/ in electrolyte system
L；
(3) operating procedure for preparing ultra-fine magnetic nickel powder using the electrolyte system is as follows:
S1. electrodeposition process: using nickel plate as anode, using titanium plate as cathode, cathode material surface smoothness is 8 μm, is placed
In the electrolyte system of above-mentioned preparation, the electro-deposition 2h under ultrasound field effect, electrodeposition temperature is 80 DEG C, on cathode plate
Obtain the celadon powder of one layer of uniform and smooth；
Wherein, the frequency of ultrasound field is 20KHz, and power 600W, interpolar is away from for 80mm, pH value 4.5, current density
For 500A/m2, electric current 1A, voltage 3V.
S2. it post-processes: step S1 being passed through into the celadon powder particle that electro-deposition generates, yin is detached under pulse field action
Pole, and decentralized processing is completed in the electrolytic solution, it is collected in the cyclic process of electrolyte, obtains grey fine powder, i.e.,
Ultra-fine magnetism nickel powder.
Embodiment 4
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic nickel powder, specifically includes
Following steps:
First in static mixing device, with the mixed solution of deionized water configuration nickel chloride and ammonium sulfate, then it is added
Ammonium chloride is eventually adding povidone and thiocarbamide；
(2) composition of electrolyte system made from: nickel ion concentration 2mol/L, ammonium sulfate concentrations 0.2mol/L, electrolysis
The concentration of ammonium chloride is 8g/L in liquid system, and Povidone concentrations are 6g/L, thiourea concentration 8g/L in electrolyte system；
(3) operating procedure of ultra-fine magnetic nickel powder is prepared referring to embodiment 3 using the electrolyte system.
Embodiment 5
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic nickel powder, specifically includes
Following steps:
First in static mixing device, with the mixed solution of deionized water configuration nickel chloride and ammonium sulfate, then it is added
Boric acid is eventually adding lauryl sodium sulfate；
(2) composition of electrolyte system made from: nickel ion concentration 1.5mol/L, ammonium sulfate concentrations 0.8mol/L, electricity
The concentration for solving boric acid in liquid system is 6g/L, and the concentration of lauryl sodium sulfate is 10g/L in electrolyte system；
(3) operating procedure of ultra-fine magnetic nickel powder is prepared referring to embodiment 3 using the electrolyte system.
Embodiment 6
(1) it the present embodiment provides the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic cobalt powder, specifically includes
Following steps:
First in tubular-mix equipment, the mixed solution of cobaltous sulfate and ammonium sulfate is matched with deionized water, chlorine is then added
Change ammonium, is eventually adding povidone and thiocarbamide；
(2) electrolyte system made from forms: concentration of cobalt ions 1mol/L, and the concentration of boric acid is in electrolyte system
10g/L, povidone and the concentration of thiocarbamide are respectively 0.5g/L, 3g/L in electrolyte system；
(3) operating procedure for preparing ultra-fine magnetic cobalt powder using the electrolyte system is as follows:
S1. electrodeposition process: using cobalt plate as anode, using titanium plate as cathode, cathode material surface smoothness is 10 μm, is placed
In the electrolyte system of above-mentioned preparation, the electro-deposition 12h under the pulse field action of ultrasound field and alternating magnetic field, electro-deposition temperature
Degree is 10 DEG C, and the bois de rose powder of one layer of uniform and smooth is obtained on cathode plate；
Wherein, the frequency of ultrasound field is 40KHz, power 50W, and the frequency of alternating magnetic field is 10KHz, interpolar away from for
100mm, pH value 3, current density 100A/m2, electric current 2A, voltage 4V.
S2. it post-processes: step S1 being passed through into the bois de rose powder particle that electro-deposition generates, yin is detached under pulse field action
Pole, and decentralized processing is completed in the electrolytic solution, it is collected in the cyclic process of electrolyte, obtains grey fine powder, i.e.,
Ultra-fine magnetism cobalt powder.
Comparative example 1
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: the electrolyte in electrolyte system is carbonate.
Comparative example 2
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: electrolyte is contained only in electrolyte system, electrolyte is ferrous sulfate.
Comparative example 3
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: electrolyte system includes electrolyte and pH buffer.
Comparative example 4
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: electrolyte system includes electrolyte and dispersing agent.
Comparative example 5
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: electrolyte system composition obtained: ferrous ion concentration 0.1mol/L, electrolyte
The concentration of boric acid is 0.1g/L in system, and povidone and the concentration of thiocarbamide are respectively 13g/L, 13g/L in electrolyte system.
Comparative example 6
This comparative example provides the electrolyte that a kind of pulse-electrodeposition process prepares ultra-fine magnetic powder referring to embodiment 1
System, difference from example 1 is that: electrolyte system composition obtained: ferrous ion concentration 2.5mol/L, electrolyte
The concentration of boric acid is 13g/L in system, and povidone and the concentration of thiocarbamide are respectively 0.1g/L, 0.1g/L in electrolyte system.
X diffraction analysis is carried out to the ultra-fine magnetic metallic powder that embodiment 1 and embodiment 3 are prepared, testing result is shown in
Fig. 1~2.
As shown in Figure 1, the ultra-fine magnetic metallic powder that prepared by embodiment 1 is iron powder, ultra-fine magnetic gold prepared by embodiment 3
Category powder is nickel powder.
Electronic Speculum observation is scanned to the ultra-fine magnetic metal iron powder that Examples 1 to 2 is prepared, testing result is shown in Fig. 3
~4.
By Fig. 3~4 it is found that ultra-fine magnetic metal iron powder is prepared in spherical or near-spherical in Examples 1 to 2, particle is equal
Even, particle size distribution range is narrow, and dispersibility is very well.
Surface microstructure observation is carried out to the ultra-fine Magnaglo that Examples 1 to 6 and comparative example 1~5 are prepared, is put down
Performance detections, the current efficiency such as equal partial size, current efficiency and degree of purity are the yield of preparation method provided by the invention, specifically
It the results are shown in Table 1.
Table 1
By comparative example 1~4 it is found that electrolyte system of the invention prepares ultra-fine magnetic metal for pulse-electrodeposition process
The particularity of powder, adds dispersing agent in electrolyte system, under the stabilization pH value that pH buffer adjusts control, utilizes the two
Synergistic effect, realize the regulation of the composition of product, granularity and pattern, and recycle the ultra-fine magnetic metal received by electrolyte
Powder particle is uniform, and particle size distribution range is narrow, good dispersion.
By comparative example 5 and 6 it is found that electrolyte system of the invention prepares ultra-fine magnetic metal for pulse-electrodeposition process
The particularity of powder, the concentration of each components such as electrolyte, pH buffer and dispersing agent, not only makes in strict control electrolyte system
Electrolyte pH stable in electrodeposition process, moreover it is possible to surface be carried out to ultrafine particle and be modified, using electrolyte of the invention
The degree of purity that ultra-fine magnetic metallic powder is prepared in system reaches 99.5% or more, and current efficiency can reach 80% or more.
Obviously, above-described embodiment is only intended to clearly illustrate technical solution of the present invention example, and is not
Restriction to embodiments of the present invention.For those of ordinary skill in the art, on the basis of the above description also
It can make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all
Made any modifications, equivalent replacements, and improvements etc. within the spirit and principles in the present invention should be included in right of the present invention and want
Within the protection scope asked.
Claims (10)
1. the electrolyte system that a kind of pulse-electrodeposition process prepares ultra-fine magnetic metallic powder, which is characterized in that the electrolyte
System includes electrolyte, pH buffer and dispersing agent；The electrolyte is the sulfate or chlorate of metal；In the electrolyte
The concentration of metal ion is 0.5 ~ 2 mol/L, and the concentration of pH buffer is 5 ~ 10 g/L, the electrolysis in the electrolyte system
The concentration amount of dispersing agent is 0.5 ~ 12 g/L in liquid system.
2. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In the concentration of metal ion is 1 ~ 2 mol/L in the electrolyte.
3. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In, the concentration of pH buffer is 5 ~ 8 g/L in the electrolyte system, in the electrolyte system concentration amount of dispersing agent be 2 ~
6 g/L。
4. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In also containing ammonium sulfate in the electrolyte.
5. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 4, feature exists
In the concentration of the ammonium sulfate is 0 ~ 0.8 mol/L.
6. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In, the pH buffer be boric acid, ammonium salt, acetate, any one in citrate.
7. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In the dispersing agent is at least one of povidone, thiocarbamide, γ-aminopropyl triethoxysilane, lauryl sodium sulfate.
8. pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1, feature exists
In the magnetic metal is any one in iron, cobalt, nickel and its alloy.
9. any one pulse-electrodeposition process prepares the electrolyte system of ultra-fine magnetic metallic powder according to claim 1 ~ 8
Preparation method, which is characterized in that specific preparation process is as follows: configuring electrolyte by concentration ratio deionized water, then presses
PH buffer is added in ratio, is eventually adding dispersing agent.
10. the preparation method of electrolyte system according to claim 9, which is characterized in that the electrolyte system for preparing is adopted
Equipment is autoclave mixing plant, tubular-mix equipment, any one in static mixing device.
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| CN101126165A (en) * | 2007-06-15 | 2008-02-20 | 武汉理工大学 | Method for preparing one-dimensional nano material |
| CN103276412A (en) * | 2013-05-29 | 2013-09-04 | 辽宁科技大学 | Method for preparing copper or nickel powder and electrolysis device based on same |
| CN105239104A (en) * | 2015-10-14 | 2016-01-13 | 中国矿业大学 | Method for electrolyzing scaly zinc powder by alkaline process |
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Application publication date: 20190104 |