CN107338456A - A kind of method that ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder - Google Patents
A kind of method that ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder Download PDFInfo
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- CN107338456A CN107338456A CN201710560514.6A CN201710560514A CN107338456A CN 107338456 A CN107338456 A CN 107338456A CN 201710560514 A CN201710560514 A CN 201710560514A CN 107338456 A CN107338456 A CN 107338456A
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- lead
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- composite powder
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of method that ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, belong to technical field of new material preparation.Step includes：Soluble lead salt, supporting electrolyte, CNT, dispersant and water are well mixed, are configured to electrolyte, anode, titanium or aluminium are made with pure lead or metal or stainless steel makees negative electrode, in 10~75 DEG C of electrolyte temperature, 150~450mA/cm of cathode-current density2Under conditions of, make ultrasound works medium from water, to control supersonic frequency be 20~130kHz, ultrasonic power per liter is 10w/L~360w/L, carries out ultrasonic wave added electro-deposition, lead/carbon nano-tube composite powder can be made in negative electrode.Present invention process is simple to operate, and agents useful for same is cheap.
Description
Technical field
The invention belongs to new material to prepare manufacture field, specifically, is related to a kind of ultrasonic wave added electro-deposition and prepares lead/carbon
The method of nanometer composite powder.
Background technology
Double base propellant is actual because burn rate is relatively low, Pressure Exponent is higher as guided missile and a kind of high-energy fuel of rocket
Need to add burningrate catalyst in use to improve its combustibility.With the development of missilery, it is badly in need of the new burn rate of exploitation and urges
Agent improves the burning of novel solid propellant.
Burningrate catalyst-nanometer lead of the lead/carbon nano-tube composite powder because loading double base propellant, in addition CNT ratio
Surface area is huge, space structure is special, catalytic performance and absorption property are excellent, and there is excellent burn rate to urge to double base propellant for it
Change effect, and be developed the burningrate catalyst as double base propellant.The disclosed compound burn rate catalysis of lead/carbon nano-tube support type
The preparation method of agent is chemical plating.Open grant number CN101440010B proposes one kind using chemically plating for lead/carbon nano-tube
The method of composite granule, including after multi-walled carbon nanotube purified, is sensitized, activate, be placed in ultrasonic disperse in acetic acid lead solution, change
Plating is learned, lead is carried on carbon nano tube surface in the form of average grain diameter 30nm in obtained lead/carbon nano-tube composite powder, to double
Base propellant has excellent burn rate catalytic effect.But this method is related to CNT sensitization, activation, and process is relatively cumbersome, and uses
To expensive Pd reagents, in addition, the pH controls of plating solution are more strict.
In view of this it is special to propose the present invention.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of ultrasonic wave added electro-deposition system
The method of standby lead/carbon nano-tube composite powder, this method pass through ultrasonic wave added electricity in specific CNT-lead salt solution
Lead/carbon nano-tube composite powder is made in deposition.
In order to solve the above technical problems, the present invention is using the basic conception of technical scheme：
A kind of method that ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, comprises the following steps：
S1：Prepare electrolyte：Soluble lead salt, supporting electrolyte, CNT, dispersant and water are well mixed first, matched somebody with somebody
Electrolyte is made, dissoluble lead salinity is 0.001~0.2mol/L in electrolyte, and supporting electrolyte concentration is 0.1~4mol/
L, carbon nanotube concentration are 0.005~3g/L, and dispersant concentration is 0.1~8g/L；
S2：Ultrasonic wave added electrodeposition process：Using pure lead or metal as anode, titanium or aluminium or stainless steel make negative electrode, control electrolysis
Liquid temperature degree is 10~75 DEG C, cathode-current density is 150~450mA/cm2, the ultrasonic wave added in the electrolyte that step S1 is prepared
30~180min of electro-deposition, lead/carbon nano-tube composite powder can be made in negative electrode.
In the present invention, soluble lead salt in S1 be one kind in lead acetate, plumbi nitras, lead fluoborate or lead citrate or
Person is several.
In the present invention, the supporting electrolyte in S1 is acetic acid, boric acid, citric acid, sodium acetate, sodium propionate, Boratex, lemon
One or both of sour sodium, sodium fluoborate arbitrary proportion mixture.
In the present invention, the CNT in S1 is first in sulfuric acid solution, salpeter solution, hydrochloric acid solution or perchloric acid solution
One or several kinds of solution in be acidified, CNT is one or two kinds of any in multi-walled carbon nanotube or single-walled carbon nanotube
The mixture of ratio.
In the present invention, the dispersant in S1 is lauryl sodium sulfate, neopelex, lauryl alcohol polyoxyethylene
Ether sulfosuccinates disodium, cetyl trimethylammonium bromide, polyvinyl alcohol, polyethylene glycol, glycerine, Nonyl pheno
Ether, OPEO, alkyl alcohol APEO, aliphatic amine polyoxyethylene ether, alkylolamides polyoxyethylene
Ether, Block polyoxyethylene-polyethenoxy ether, alkylolamides, Monododecylphosphate triethanolamine, polyvinylpyrrolidine
The mixture of one or more of arbitrary proportions in ketone, gelatin.
In the present invention, ultrasound works medium is water in ultrasonic wave added electrodeposition process in S2, supersonic frequency is 20~
130kHz, ultrasonic power per liter are 10~360w/L.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
Present invention process is simple to operate, after CNT acidifying, without being sensitized, activating, through a ultrasonic wave added electro-deposition
Lead/carbon nano-tube composite powder can be made in negative electrode；Reagent cost is cheap, and carbon is received without using expensive Pd reagents
Mitron is sensitized, activated；Environment-friendly, raw materials used effect on environment is small.
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Brief description of the drawings
A part of the accompanying drawing as the application, for providing further understanding of the invention, of the invention is schematic
Embodiment and its illustrate to be used to explain the present invention, but do not form inappropriate limitation of the present invention.Obviously, drawings in the following description
Only some embodiments, to those skilled in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.In the accompanying drawings：
Fig. 1 is lead/carbon nano-tube composite powder scanning transmission energy spectrum diagram made from the embodiment of the present invention 1；
Fig. 2 is the pictorial diagram of lead/carbon nano-tube composite powder made from the embodiment of the present invention 1；
Fig. 3 is the electron microscope picture of lead/carbon nano-tube composite powder made from the embodiment of the present invention 1.
It should be noted that these accompanying drawings and word description are not intended as the design model limiting the invention in any way
Enclose, but be that those skilled in the art illustrate idea of the invention by reference to specific embodiment.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in embodiment is clearly and completely described, following examples be used for illustrate the present invention, but
It is not limited to the scope of the present invention.
Embodiment 1
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
Electrolyte is made, dissoluble lead salinity is 0.005mol/L in electrolyte, and soluble lead salt is lead acetate, and supporting electrolyte is dense
Spend for 2.5mol/L, the sodium acetate that supporting electrolyte is the acetic acid that molar concentration is 1.5mol/L and molar concentration is 1mol/L,
Carbon nanotube concentration is 3g/L, and CNT is multi-walled carbon nanotube, and dispersant concentration 3g/L, dispersant is detergent alkylate
Sodium sulfonate；
S2：Ultrasonic wave added electrodeposition process：Using pure lead as anode, titanium makees negative electrode, and 10 DEG C of electrolyte temperature of control, cathode current are close
Spend 150mA/cm2, ultrasonic wave added electro-deposition 180min in the electrolyte prepared in step sl, ultrasound works medium is water, control
Supersonic frequency 40kHz processed, ultrasonic power per liter 90w/L, can be made lead/carbon nano-tube composite powder in negative electrode.Obtained lead/carbon
Nanometer composite powder microscopic appearance is illustrated in Fig. 1, and Fig. 2 is the pictorial diagram of lead/carbon nano-tube composite powder.
Embodiment 2
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
It is made electrolyte, dissoluble lead salinity is 0.02mol/L in electrolyte, and soluble lead salt is lead fluoborate, supporting electrolyte
Concentration is 4mol/L, and supporting electrolyte is the acetic acid that molar concentration is 2mol/L and 2mol/L sodium fluoborate, and CNT is dense
It is multi-walled carbon nanotube to spend for 1.5g/L, CNT, and dispersant concentration 8g/L, dispersant is lauryl sodium sulfate；
S2：Ultrasonic wave added electrodeposition process：Using pure lead as anode, stainless steel makees negative electrode, and it is 50 DEG C, negative electrode to control electrolyte temperature
Current density is 300mA/cm2, ultrasonic wave added electro-deposition 30min in the electrolyte prepared in step sl, ultrasound works medium
For water, control supersonic frequency 40kHz, ultrasonic power per liter 150w/L, lead/carbon nano-tube composite powder can be made in negative electrode.
Embodiment 3
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
It is set to electrolyte, dissoluble lead salinity is 0.1mol/L in electrolyte, and soluble lead salt is plumbi nitras, supporting electrolyte concentration
For 3mol/L, the Boratex that supporting electrolyte is the boric acid that molar concentration is 1.2mol/L and molar concentration is 1.8mol/L, carbon
Concentrations of nanotubes is 1.5g/L, and CNT is mass ratio 1:1 multi-walled carbon nanotube and the mixture of single-walled carbon nanotube, point
Powder concentration is 4g/L, and dispersant is mass ratio 1:The mixture of 1 neopelex and gelatin；
S2：Ultrasonic wave added electrodeposition process：Using pure lead as anode, aluminium makees negative electrode, and it is 20 DEG C, cathode current to control electrolyte temperature
Density is 450mA/cm2, ultrasonic wave added electro-deposition 80min in the electrolyte prepared in step sl, ultrasound works medium is water,
Supersonic frequency 60kHz, ultrasonic power per liter 360w/L are controlled, lead/carbon nano-tube composite powder can be made in negative electrode.
Embodiment 4
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
It is made electrolyte, dissoluble lead salinity is 0.001mol/L in electrolyte, and soluble lead salt is lead citrate, supporting electrolyte
Concentration is 2mol/L, and supporting electrolyte is the acetic acid that molar concentration is 1.5mol/L and molar concentration is 0.5mol/L citric acids
Sodium, carbon nanotube concentration 0.05g/L, CNT are multi-walled carbon nanotube, and dispersant concentration 0.2g/L, dispersant is matter
Measure ratio 1:The mixture of 1 polyvinylpyrrolidone and gelatin；
S2：Ultrasonic wave added electrodeposition process：Using pure lead as anode, aluminium makees negative electrode, and it is 25 DEG C, cathode current to control electrolyte temperature
Density is 250mA/cm2, ultrasonic wave added electro-deposition 90min in the electrolyte prepared in step sl, ultrasound works medium is water,
Supersonic frequency 20kHz, ultrasonic power per liter 10w/L are controlled, lead/carbon nano-tube composite powder can be made in negative electrode.
Embodiment 5
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
It is made electrolyte, dissoluble lead salinity is 0.2mol/L in electrolyte, and soluble lead salt is lead acetate, supporting electrolyte concentration
For 4mol/L, the sodium acetate that supporting electrolyte is the citric acid that molar concentration is 1.3mol/L and molar concentration is 2.7mol/L,
Carbon nanotube concentration is 0.005g/L, and CNT is single-walled carbon nanotube, and dispersant concentration 3g/L, dispersant is mass ratio
1:1:1 lauryl sodium sulfate, gelatin, the mixture of glycerine.
S2：Ultrasonic wave added electrodeposition process：Using metal as anode, aluminium makees negative electrode, controls electrolyte temperature as 75 DEG C, the moon
Electrode current density is 240mA/cm2, ultrasonic wave added electro-deposition 150min in the electrolyte prepared in step sl, ultrasound works are situated between
Matter is water, control supersonic frequency 130kHz, ultrasonic power per liter 120w/L, lead/carbon nano-tube composite powder can be made in negative electrode.
Embodiment 6
The method that the ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, is comprised the following steps that：
S1：Prepare electrolyte：Match somebody with somebody after being first well mixed soluble lead salt, supporting electrolyte, CNT, dispersant and water
Electrolyte is made, dissoluble lead salinity is 0.001mol/L in electrolyte, and soluble lead salt is plumbi nitras, and supporting electrolyte is dense
Spend for 2.4mol/L, the boric acid that supporting electrolyte is the acetic acid that molar concentration is 2mol/L and molar concentration is 0.4mol/L, carbon
Concentrations of nanotubes is 0.005g/L, and CNT is single-walled carbon nanotube, and dispersant concentration 1.2g/L, dispersant is mass ratio
1:1:1:1 polyvinyl alcohol, gelatin, NPE, the mixture of OPEO；
S2：Ultrasonic wave added electrodeposition process：Using metal as anode, titanium makees negative electrode, controls electrolyte temperature as 40 DEG C, negative electrode electricity
Current density is 170mA/cm2, ultrasonic wave added electro-deposition 150min in the electrolyte prepared in step sl, ultrasound works medium is
Water, control supersonic frequency 60kHz, ultrasonic power per liter 100w/L, can be made lead/carbon nano-tube composite powder in negative electrode.
Described above is only presently preferred embodiments of the present invention, not makees any formal limitation to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people for being familiar with this patent
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompting make it is a little change or be modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within the present invention program.
Claims (6)
1. a kind of method that ultrasonic wave added electro-deposition prepares lead/carbon nano-tube composite powder, it is characterised in that including following step
Suddenly：
S1：Prepare electrolyte：Soluble lead salt, supporting electrolyte, CNT, dispersant and water are well mixed first, matched somebody with somebody
Electrolyte is made, dissoluble lead salinity is 0.001~0.2mol/L in electrolyte, and supporting electrolyte concentration is 0.1~4mol/
L, carbon nanotube concentration are 0.005~3g/L, and dispersant concentration is 0.1~8g/L；
S2：Ultrasonic wave added electrodeposition process：Using pure lead or metal as anode, titanium or aluminium or stainless steel make negative electrode, control electrolysis
Liquid temperature degree is 10~75 DEG C, cathode-current density is 150~450mA/cm2, the ultrasonic wave added in the electrolyte that step S1 is prepared
30~180min of electro-deposition, lead/carbon nano-tube composite powder can be made in negative electrode.
2. the method that a kind of ultrasonic wave added electro-deposition according to claim 1 prepares lead/carbon nano-tube composite powder, it is special
Sign is that the soluble lead salt in S1 is the one or several kinds in lead acetate, plumbi nitras, lead fluoborate or lead citrate.
3. the method that a kind of ultrasonic wave added electro-deposition according to claim 1 prepares lead/carbon nano-tube composite powder, it is special
Sign is that the supporting electrolyte in S1 is acetic acid, boric acid, citric acid, sodium acetate, sodium propionate, Boratex, sodium citrate, fluorine boron
One or both of sour sodium arbitrary proportion mixture.
4. the method that a kind of ultrasonic wave added electro-deposition according to claim 1 prepares lead/carbon nano-tube composite powder, it is special
Sign is, one kind first in sulfuric acid solution, salpeter solution, hydrochloric acid solution or perchloric acid solution of the CNT in S1 or
It is acidified in several solns, CNT is the mixing of one or two kinds of arbitrary proportions in multi-walled carbon nanotube or single-walled carbon nanotube
Thing.
5. the method that a kind of ultrasonic wave added electro-deposition according to claim 1 prepares lead/carbon nano-tube composite powder, it is special
Sign is that the dispersant in S1 is lauryl sodium sulfate, neopelex, Dodecyl Polyoxyethylene Ether sulfosuccinic
Acid esters disodium, cetyl trimethylammonium bromide, polyvinyl alcohol, polyethylene glycol, glycerine, NPE, octyl phenol
APEO, alkyl alcohol APEO, aliphatic amine polyoxyethylene ether, alkylolamides APEO, block gather
In oxygen ethene-polyethenoxy ether, alkylolamides, Monododecylphosphate triethanolamine, polyvinylpyrrolidone, gelatin
The mixture of one or more of arbitrary proportions.
6. the method that a kind of ultrasonic wave added electro-deposition according to claim 1 prepares lead/carbon nano-tube composite powder, it is special
Sign is that ultrasound works medium is water in ultrasonic wave added electrodeposition process in S2, and supersonic frequency is 20~130kHz, and ultrasound rises work(
Rate is 10~360w/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440010A (en) * | 2007-11-23 | 2009-05-27 | 深圳大学 | Lead / carbon nano-tube composite powder and preparation thereof |
| CN104131318A (en) * | 2014-08-01 | 2014-11-05 | 昆明理工大学 | Preparation method for carbon nanotube and/or graphene reinforced lead based composite anode |
| CN104233379A (en) * | 2014-09-05 | 2014-12-24 | 昆明理工大学 | Electro-deposition preparation method of carbon nano tube-copper base composite powder |
-
2017
- 2017-07-11 CN CN201710560514.6A patent/CN107338456A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440010A (en) * | 2007-11-23 | 2009-05-27 | 深圳大学 | Lead / carbon nano-tube composite powder and preparation thereof |
| CN104131318A (en) * | 2014-08-01 | 2014-11-05 | 昆明理工大学 | Preparation method for carbon nanotube and/or graphene reinforced lead based composite anode |
| CN104233379A (en) * | 2014-09-05 | 2014-12-24 | 昆明理工大学 | Electro-deposition preparation method of carbon nano tube-copper base composite powder |
Non-Patent Citations (2)
| Title |
|---|
| 刘开琪等: "《金属陶瓷的制备与应用》", 31 March 2008, 冶金工业出版社 * |
| 蒋国祥: "新型析氧阳极制备及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20171110 |