CN108436100A - A kind of preparation method of ultra-thin porous nanometer nickel foil - Google Patents
A kind of preparation method of ultra-thin porous nanometer nickel foil Download PDFInfo
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- CN108436100A CN108436100A CN201810320654.0A CN201810320654A CN108436100A CN 108436100 A CN108436100 A CN 108436100A CN 201810320654 A CN201810320654 A CN 201810320654A CN 108436100 A CN108436100 A CN 108436100A
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. 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
- 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
- B22F1/0551—Flake form nanoparticles
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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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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Abstract
The present invention provides a kind of preparation methods of ultra-thin porous nanometer nickel foil, using Ni2+, trisodium citrate or ascorbic acid, chloroplatinic acid or gold chloride mixed aqueous solution as precursor liquid, hydrazine hydrate is as reducing agent, by the way that ultra-thin porous nanometer nickel foil is prepared under specified conditions.The nickel foil is attached in walls of beaker, it is arranged by the spheric granules self assembly of diameter about 300~400nm, in cellular, thickness is only the diameter of single nickel particle, it is conductive good, light weight, bent excellent properties can coordinate different substrates for fields such as sensor, electrode material, storage material, electromagnetic shielding materials.Preparation process of the present invention is simple, time-consuming short, at low cost, can meet the needs of large-scale production.
Description
Technical field：
The present invention relates to the preparing technical fields of nano material, and in particular, to a kind of system of ultra-thin porous nanometer nickel foil
Preparation Method.
Background technology
Nickel foil is one of industrial basic materials such as electronics, telecommunication, instrument, is usually used in electromagnetic shielding, high energy storage density
The applications such as alkaline storage battery, surface resistance are alternatively arranged as fire prevention, moisture-proof, antimagnetic new packaging material by processing.In recent years,
Due to the demand industrially to some specific use metal materials, nickel foil is towards thinner and smaller microstructure development.One side
Face, ultra-thin nickel foil can reduce material, mitigate quality, improve flexible, increase specific surface area；On the other hand, nickel foil surface is more
Hole nano-array provides active site and huge surface area, is conducive to further functionalization, becomes excellent compound
Material support.Ultra-thin porous nanometer nickel foil is due to excellent physics and chemical property, receiving the extensive pass of researchers
Note.
Existing nickel foil preparation method is mostly carbonyl process or electrolysis, but there is prodigious deficiency.
For example, CN1110726A discloses a kind of process electrolytically producing nickel foil, it is sun with electrolytic nickel
Pole carries out electrolytic deposition using rotatable titanium roller as cathode under the rotation of cathode.Contain NiSO in electrolyte4·7H2O2
40-360 grams/l, NiCl2·6H2O 8-40 gram/l, H3BO330-45 grams/l, the pH 1.8-3.4 of electrolyte.Electricity
It solves liquid to overflow through electrolytic cleaning, preheating from electrolytic cell, enters back into electrolytic cell, control certain flow closed cycle.It is prepared by this method
The particle size of gained nickel foil is larger, is micron order, and the electrolyte used in this method has toxicity and pollutes environment, increases
Treatment cost of waste liquor.
CN103031578A discloses a kind of electrolytic method producing nickel foil, makees anode with lead silver plate or titanium plate, with can be with
The titanium roller or stainless steel rod of rotation and rotation rate-controllable make cathode, by two anode distance controls of cathode and anode in 9~15mm, to electricity
Solution slot in recycle pass to be made of the nickel sulfate of 200~300g/L and the boric acid of 40~45g/L and PH be 1.7~3.5 electricity
Liquid is solved, electrolyzer power source is connected and controlling voltage makes cathode-current density be 21~35A/dm2, electrolyte temperature is controlled 50
~60 DEG C, rotation titanium roller at the uniform velocity or stainless steel rod, by the continuous rotation of titanium roller or stainless steel rod so that separate titanium roller or
Stainless steel rod powers on the nickel foil of solution deposition, and then obtained nickel foil is washed, dries and batched and becomes continuous coiled nickel foil,
As gained article of manufacture.This method preparation process needs whole process to be controlled, prepare gained nickel foil it is thicker, particle size compared with
Greatly, the electrolyte and used in this method has toxicity and pollutes environment.
CN102995085A discloses a kind of method of electrolysis production roughening nickel foil, and the electrolysis for being applied to nickel foil produces
Field.It includes the following steps：Step 1：Choose semi-bright nickel foil as be roughened nickel foil base material, and to semi-bright nickel foil into
Row activation process；Step 2：By in step 1 it is activated treated semi-bright nickel foil is placed in by 18~25g/L nickel sulfate and
In the roughening electrolytic cell of the ammonium sulfate composition of 21~23g/L, to the cathode and anodal closure of roughening electrolytic cell, in roughening electrolytic cell
Carry out roughening treatment；Step 3：Treated that nickel foil is placed in the nickel sulfate by 200g/L~250g/L by roughened in step 2
In the solidification electrolytic cell of the solution formed with the boric acid and 40g/L nickel chlorides of 40~45g/L, cathode to solidification electrolytic cell and
Anodal closure carries out curing process；Step 4：By the nickel foil drying after curing process in step 3.This method preparation process is multiple
Miscellaneous, energy consumption is big, and the particle size for preparing gained nickel foil is larger, and the electrolyte used in this method has toxicity and pollutes ring
Border increases treatment cost of waste liquor.
Although carbonyl process productivity is high, meet industrialization demand, carbonylation process to production technology and equipment requirement compared with
It is high and easily cause toxic gas leakage, cause serious environmental pollution.Although electrolysis equipment is simple, production technology is complicated, easily
By such environmental effects, energy consumption is big, and productivity is relatively low.In addition, method made above does not all have special ultra-thin porous nanometer
Structure, therefore, the present invention are of great significance to meeting special applications demand, raising productivity, reducing energy consumption.
Invention content
In view of the deficienciess of the prior art, present invention firstly provides a kind of water-baths to prepare ultra-thin porous nanometer nickel foil
Method.Its basic principle is to utilize the nano nickel for reacting and being formed self assembly arrangement form single layered porous nano nickel in walls of beaker
Foil.This method is easy to operate, and productivity is high, at low cost.
The method that a kind of water-bath of technical scheme of the present invention prepares ultra-thin porous nanometer nickel foil, includes the following steps：
Step S1：It prepares and contains Ni2+Precursor liquid-A liquid, specially Ni2+, trisodium citrate or ascorbic acid, chloroplatinic acid
Or the mixed aqueous solution of gold chloride, it is uniformly mixed；
Step S2：Prepare reducing solution-B liquid, i.e. hydrazine hydrate (NH4·H2O) aqueous solution；
Step S3：The pH value of A liquid and B liquid is adjusted with sodium hydroxide；
Step S4：B liquid is poured into the beaker equipped with A liquid, then heating water bath 15min~1h at 70~90 DEG C；
Step S5：It waits for cooling down after reaction, takes out the nickel foil being grown in walls of beaker, be put into after being washed with absolute ethyl alcohol
Processing is dried in vacuum drying chamber.
Preferably, the Ni2+Selected from one or more of nickel chloride, nickel sulfate, nickel nitrate, nickel acetate；Ni in solution2 +Concentration range be 0.01~2M, the concentration range of trisodium citrate or ascorbic acid is 0.01~2M, chloroplatinic acid or gold chloride
Concentration range be 0.01~5mM.The selection of each material concentration range is according to the amount of each substance, reduction in redox reaction
It continuously attempts in agent excess principle, crystal seed growing principle scheduling theory calculations incorporated experimentation and gropes to obtain.
Preferably, in the hydrazine hydrate aqueous solution, the concentration range of hydrazine hydrate is 0.01~1M.This is preferably with reducing agent mistake
Amount is principle, ensure that the abundant progress for not wasting and reacting of material.
Preferably, the volume ratio of the A liquid and B liquid is 1:1.This is preferably that next step A liquid and the mixing of B liquid provide one
A environment mildly stablized.
Preferably, naoh concentration ranging from 0.01~1M during the pH value adjustment.Should be preferably that hydrazine hydrate carries
The alkaline environment that a pH is about 12 has been supplied, hydrazine hydrate is contributed to play its reproducibility, has preferably carried out redox reaction.
Preferably, reaction temperature is 80 DEG C upon mixing for the A liquid and B liquid, reaction time 30min.This preferably can be with
The abundant progress for ensureing reaction in a relatively short period of time, obtains ideal nickel foil.
Another object of the present invention is to provide a kind of ultra-thin porous nanometer nickel foil, the ultra-thin porous nanometer nickel foil passes through
Preparation method above-mentioned is prepared.
The nickel foil surfacing is clean, has metallic luster, by the spheric granules self assembly of diameter about 300~400nm
It arranges, is in cellular, the thickness with single layer nano nickle granules.
The nickel foil has excellent electric conductivity and magnetism, and different substrates can be coordinated for sensor, electrode material
The fields such as material, storage material, electromagnetic shielding material.
The ultra-thin porous nanometer nickel foil of the present invention also provides a kind of in substrate growth in situ, pastes solid in walls of beaker
Fixed different substrate (such as filter paper, fabric, ITO substrate), the ultra-thin porous nanometer nickel foil that aforementioned preparation process is prepared exist
Growth in situ in substrate.
Compared with prior art, the present invention has following advantageous effect：
1. preparation process of the present invention is simple, short, productivity height is taken, it is at low cost, can meet the needs of large-scale production.
2. the ultra-thin porous nanometer nickel foil that present invention production obtains has the thickness (about 500nm) of single layer nano nickle granules,
Quality greatly is alleviated, flexibility is improved, increases specific surface area, certain special application demands can be met.
3. the obtained ultra-thin porous nanometer nickel foil of present invention production has porous nanometer structure, active site and huge is provided
Big surface area is conducive to further functionalization, becomes excellent composite material carrier.
4. the present invention can go out ultra-thin porous receive by growth in situ in different substrates (such as filter paper, fabric, ITO substrate)
Rice nickel foil, directly obtains the flexible substrates of conductive magneto-conductive, to realize the application on wearable device field.
5. the ultra-thin porous nanometer nickel foil that present invention production obtains has excellent electric conductivity and magnetism, can coordinate not
Same substrate is for fields such as sensor, electrode material, storage material, electromagnetic shielding materials.
Description of the drawings：
Attached drawing 1 is the ultra-thin porous nanometer nickel foil figure being attached in the present invention in walls of beaker.
Attached drawing 2 is the XRD diagram of ultra-thin porous nanometer nickel foil in the present invention.
Attached drawing 3 is the SEM figures of ultra-thin porous nanometer nickel foil in the present invention；Wherein 3 (a) is nickel foil plan view, and 3 (b) is nickel
Foil layer figure.
Wherein：
It is face-centered cubic crystal structure by attached drawing 2 it is found that material and the standard PDF cards of Ni are completely corresponding.
By attached drawing 3 (a) it is found that the nickel foil prepared is arranged by the spheric granules self assembly of diameter about 300~400nm,
In cellular；By attached drawing 3 (b) it is found that nickel foil has the thickness (about 500nm) of single layer nano nickle granules.
Specific implementation mode：
Using embodiment and attached drawing below, the invention will be further described, and however, it is not limited to this.
Embodiment 1：
The preparation method of ultra-thin porous nanometer nickel foil, comprises the following steps：
(1) it prepares and contains Ni2+Precursor liquid (A liquid)：Weigh 1.1g nickel chlorides, 5.6mg chloroplatinic acids and 1.8g citric acids three
Sodium is added in 30mL deionized waters, is uniformly mixed.
(2) reducing solution (B liquid) is prepared：It measures 4mL hydrazine hydrates (40~50%) to be added in 26mL deionized waters, stirring is mixed
It closes uniform.
(3) sodium hydrate aqueous solution is prepared：It weighs 0.4g NaOH to be added in 40mL deionized waters, be uniformly mixed.
(4) 20mL sodium hydrate aqueous solutions are separately added into A liquid and B liquid, be uniformly mixed.
(5) B liquid is poured into the beaker equipped with A liquid, then the heating water bath 15min at 80 DEG C.
(6) it waits for cooling down after reaction, takes out the nickel foil being grown in walls of beaker, be put into after being washed with water and absolute ethyl alcohol
Processing is dried in vacuum drying chamber.
The ultra-thin porous nanometer nickel foil that this implementation obtains, surface smooth pieces have metallic luster, and nano nickle granules diameter is about
For 300~400nm, nickel foil thickness is about 500nm.
As shown in Fig. 1, ultra-thin porous nanometer nickel foil is attached in walls of beaker.The ultra-thin porous nanometer nickel foil
XRD is as shown in Fig. 2, and the SEM figures of ultra-thin porous nanometer nickel foil are as shown in Figure 3；Wherein 3 (a) is nickel foil plan view, and 3 (b) is nickel
Foil layer figure.
It is face-centered cubic crystal structure by attached drawing 2 it is found that material and the standard PDF cards of Ni are completely corresponding.
By attached drawing 3 (a) it is found that the nickel foil prepared is arranged by the spheric granules self assembly of diameter about 300~400nm,
In cellular；By attached drawing 3 (b) it is found that nickel foil has the thickness (about 500nm) of single layer nano nickle granules.
Embodiment 2：
The method of the ultra-thin porous nanometer nickel foil of growth in situ, comprises the following steps in substrate：
The substrate (chemical ＆ blended fabric) of certain size is fixed on adhesive tape in the walls of beaker equipped with A liquid, and by heating water bath
Time lengthening is 1h, remaining step is the same as embodiment 1.
This implementation obtains ultra-thin porous nanometer nickel foil of the growth in situ in substrate, and nano nickle granules diameter is about 300~
400nm, nickel foil thickness are about 400nm.
Embodiment 3：
The method of the ultra-thin porous nanometer nickel foil of growth in situ, comprises the following steps in substrate：
It prepares and contains Ni2+Precursor liquid (A liquid) when, the amount of chloroplatinic acid is expanded into ten times greater (0.056g), remaining step is the same as real
Apply example 2.
This implementation obtains ultra-thin porous nanometer nickel foil of the growth in situ in substrate, and nano nickle granules diameter is about 200~
300nm, nickel foil thickness are about 300nm.
4 performance detection of embodiment
Method for testing performance and result are as follows：
| Diameter (nm) | Thickness (nm) | Surface resistance (Ω/cm2) | Coercivity (Oe) | |
| Embodiment 1 | 300~400 | 500 | 0.9 | 130 |
| Embodiment 2 | 300~400 | 400 | 1.8 | 116 |
| Embodiment 3 | 200~300 | 300 | 15 | 109 |
It can illustrate nickel particle of the present invention obtained ultra-thin porous nanometer nickel foil of production by reduced size from the above
Self assembly rearranges, and can accomplish single layer superthin structure, and have excellent electric conductivity and magnetism, can coordinate different
Substrate is for fields such as sensor, electrode material, storage material, electromagnetic shielding materials.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of ultra-thin porous nanometer nickel foil, which is characterized in that comprise the steps of：
Step S1：It prepares and contains Ni2+Precursor liquid-A liquid, specially Ni2+, trisodium citrate or ascorbic acid, chloroplatinic acid or chlorine
The mixed aqueous solution of auric acid, is uniformly mixed；
Step S2：Prepare reducing solution-B liquid, i.e. hydrazine hydrate aqueous solution；
Step S3：The pH value of A liquid and B liquid is adjusted with sodium hydroxide；
Step S4：B liquid is poured into the beaker equipped with A liquid, then heating water bath 15min~1h at 70~90 DEG C；
Step S5：It waits for cooling down after reaction, takes out the nickel foil being grown in walls of beaker, washing, drying.
2. a kind of preparation method of ultra-thin porous nanometer nickel foil according to claim 1, which is characterized in that the step S1
In Ni2+Selected from one or more of nickel chloride, nickel sulfate, nickel nitrate, nickel acetate；Ni in solution2+Concentration range be
The concentration range of 0.01~2M, trisodium citrate or ascorbic acid is 0.01~2M, the concentration range of chloroplatinic acid or gold chloride is
0.01~5mM.
3. a kind of preparation method of ultra-thin porous nanometer nickel foil according to claim 1, which is characterized in that the step S2
In hydrazine hydrate concentration range be 0.01~1M.
4. a kind of preparation method of ultra-thin porous nanometer nickel foil according to claim 1, which is characterized in that the step S3
A concentration of 0.01~1M of middle sodium hydroxide adjusts PH=12.
5. a kind of preparation method of ultra-thin porous nanometer nickel foil according to claim 1, which is characterized in that the step S4
In reaction condition be specially：Reaction temperature is 70~90 DEG C, and the reaction time is 15min~1h.
6. a kind of preparation method of ultra-thin porous nanometer nickel foil according to claim 1, which is characterized in that the end of reaction
Postcooling refers to taking out beaker after reacting 15min~1h, cooled to room temperature.
7. a kind of ultra-thin porous nanometer nickel foil, which is characterized in that the ultra-thin porous nanometer nickel foil is any by claim 1-6
Preparation method described in claim is prepared.
8. a kind of ultra-thin porous nanometer nickel foil of growth in situ in substrate, which is characterized in that paste and fixed not in walls of beaker
Same substrate (such as filter paper, fabric, ITO substrate) passes through the preparation method described in claim 1-6 any claims and prepares
Obtained ultra-thin porous nanometer nickel foil growth in situ in substrate.
9. a kind of ultra-thin porous nanometer nickel foil according to claim 7, which is characterized in that the nickel foil surfacing is clean
Only, there is metallic luster, arranged by the spheric granules self assembly of diameter about 300~400nm, be in cellular, there is single layer
The thickness of nano nickle granules.
10. a kind of ultra-thin porous nanometer nickel foil according to claim 7, which is characterized in that the nickel foil has excellent
Electric conductivity and magnetism can coordinate different substrates for sensor, electrode material, storage material, electromagnetic shielding material etc.
Field.
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