CN106903304A - A kind of Fe@Ni composite granules with core shell structure and preparation method thereof - Google Patents
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof Download PDFInfo
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- CN106903304A CN106903304A CN201710175312.XA CN201710175312A CN106903304A CN 106903304 A CN106903304 A CN 106903304A CN 201710175312 A CN201710175312 A CN 201710175312A CN 106903304 A CN106903304 A CN 106903304A
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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
- B22F1/17—Metallic particles coated with metal
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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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- 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
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
Abstract
The present invention relates to a kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Its technical scheme is：Iron powder is put into sodium hydroxide solution and is stirred, washing is placed into dilution heat of sulfuric acid, and stirring, washing is dried, the iron powder after being washed.Complexing agent and nickel salt are stirred under water bath condition, chelant liquid is obtained；Again by reducing agent addition chelant liquid, stirring obtains mixed liquor, and pH value is adjusted with sodium hydroxide solution, obtains nickel-plating liquid；Again to stabilizer is added in the nickel-plating liquid, stir, obtain final product the nickel-plating liquid of stabilization.The iron powder after the washing is added in nickel-plating liquid to stabilization, lasting stirring obtains covering liquid；By covering liquid washing, dry, the Fe@Ni composite granules with core shell structure are obtained.The characteristics of present invention has process is simple, with short production cycle, strong operability, high yield rate, low cost；Made product is without obvious reunion, uniform composition, stable chemical performance and oxidation resistant.
Description
Technical field
The invention belongs to Fe@Ni composite granule technical fields.Specifically related to a kind of Fe@Ni composite powders with core shell structure
Body and preparation method thereof.
Background technology
Carbon containing refractory is widely used in steel industry with its unique mechanics and chemical property, and species is various, main
There are carbonaceous article, magnesia carbon brick, graphite clay-ware, alumina-carbon material, silicon carbide product etc..Magnesium carbon and aluminum-carbon refractory material are
Current most widely used carbon containing refractory, magnesia-carbon refractory material has superior calorifics, chemistry and mechanical property, is employed
In steelmaking equipment and component, such as converter, electric arc furnaces and RH vacuum degassers.Aluminum-carbon refractory material is with its good anti-erosion
Property and thermal shock resistance, be widely used in making steel the continuous casting installation for casting of industry, such as slide plate, submersed nozzle and integral column of sagger.
Due to possessing good thermal property and mechanical performance, carbon containing refractory has and quickly develops and be widely applied.
Carbon is the important component of carbon containing refractory, is the key component that it obtains premium properties.Carbon nano-fiber or carbon
Nanotube can play positive role to carbon containing refractory combination property.And additional CNT or carbon nano-fiber are due to it
There is larger shortcoming in actual use in the problems such as expensive relatively costly, easy reunion.Added in carbon containing refractory and urged
Agent, in-situ preparation carbon nano-fiber or CNT, can be uniformly distributed, and carbon fiber and the CNT of generation have pattern
Controllable the advantages of be widely used with carbon containing refractory.
Transition metal simple substance, transition metal oxide, transition metal nitrate or transition are added in carbon containing refractory
Metal chloride is used as the main method that catalyst is currently acquired in-situ preparation CNT and carbon fiber.Made using ferrocene
For in catalyst addition carbonaceous material（Hu Qinghua, Wang Xitang, Wang Zhoufu, wait to mix the synthesis of Fe phenolic resin and its catalysis stone
Inkization studies [J], material engineering, 2010（Supplementary issue 2）：359~361）, with phenolic resin as matrix, by catalyzing and synthesizing carbon nanometer
Pipe, promotes resin to be changed from vitreous carbon structure to graphitized carbon structure.But catalyst is made using ferrocene, to phenolic resin carbon
It is structurally-modified to be influenceed by the characteristic that iron is easily aoxidized, cause its catalytic effect undesirable.
Using metal nickel powder do catalyst add carbon containing refractory in（Wei state puts down, and Zhu Baiquan, Li Xiangcheng wait not
[J] refractory materials, 2015 (4) are studied with the charing of Ni doping phenolic resin under carbonization condition:246~250.）, nano metal
Nickel powder has excellent catalysis activity, can obtain well-developed CNT.But metallic nickel is used as catalyst high cost,
It is difficult to large-scale industrial production.
Using cobalt oxide as in catalyst addition carbonaceous material（Zhao Lei, Yu Xiaoyan, kingdom fly, and wait cobalt oxides molten
Pyrolytic carbon structure change [J] Journal of Functional Polymers of glue composite phenolic resin, 2012,25 (1):58~61.）, can urge
Change obtains CNT, but first need to prepare cobalt oxide colloidal sol using sol-gal process, and preparation cost is higher, and sol-process control is multiple
It is miscellaneous.
Using nickel oxide as in catalyst addition carbonaceous material（Li Yawei, Xie Ting, Zhao Lei nickel oxide doping phenolic aldehyde
Structure and Study of Antioxidation [J] Wuhan University Of Technologies the journal natural science edition of Resin Char, 2011,34 (1):18
~22.）, the addition of nickel oxide powder can be catalyzed generation carbon fiber, but dispersion effect is poor in phenolic resin, easily because of group
It is poly- to lose catalysis activity.
" a kind of modified phenolic resin for fire resistive material and preparation method thereof "（CN200810047051.4）Patented technology, leads to
Cross in the metal oxide sol presoma addition phenolic resin that sol-gal process prepares iron or cobalt or nickel, can be in refractory material
Fabricated in situ CNT, but catalyst preparation process is complicated and preparation time is more long.
" Transition metal compound composite lignin phenol-formaldehyde resin modified and preparation method thereof "（CN201310261304.9）
Patented technology, by adding transition metal nitrate or transition metal chloride catalysis generation carbon fiber in carbonaceous material, but
Nitrate is decomposed at low temperature, produces a large amount of gases, and a large amount of stomatas are produced in matrix of materials, destroys the matrix knot of material
Structure；Its pyrolytic process is difficult to control to simultaneously, and nano particle can still occur agglomeration in pyrolytic process, and the nano particle of formation is total
Particle diameter is also relatively large for body.
The content of the invention
It is contemplated that overcoming the deficiencies in the prior art, it is therefore an objective to provide a kind of process is simple, with short production cycle, operability
By force, high yield rate, the Fe@Ni composite granule preparation methods with core shell structure of low cost；With having obtained by the method
The Fe@Ni composite granules of core shell structure are without obvious reunion, uniform composition, stable chemical performance and oxidation resistant.
To achieve the above object, the step of the technical solution adopted by the present invention is：
（1）Iron powder is put into the sodium hydroxide solution that concentration is 10wt%, 1 ~ 3min is stirred, is washed with deionized to neutrality,
Place into the dilution heat of sulfuric acid that concentration is 5wt%, stir 1 ~ 3min, be then washed with deionized to neutrality, dry, obtain
Iron powder after washing.
（2）By complexing agent: the mass ratio of nickel salt is（1.9~2.8）: 1 dispensing, by the network under 35 ~ 90 DEG C of water bath conditions
Mixture and the nickel salt stir, and obtain chelant liquid；Again by reducing agent: the mass ratio of nickel salt is（1.0~1.3）: 1, will be described
Reducing agent stirs in adding the chelant liquid, obtains mixed liquor.
（3）To adding concentration to be 8 ~ 14 for sodium hydroxide solution to the pH value of 20wt% in the mixed liquor, nickel plating is obtained
Liquid；The stabilizer of the 0.06 ~ 0.15wt% of nickel-plating liquid is accounted for addition in the nickel-plating liquid again, 5 ~ 10min is stirred, stabilization is obtained final product
Nickel-plating liquid.
（4）Under agitation, to the institute that the 6 ~ 15wt% of nickel-plating liquid for accounting for the stabilization is added in the nickel-plating liquid of the stabilization
The iron powder after washing is stated, 10 ~ 100min is persistently stirred, covering liquid is obtained.
（5）The covering liquid is washed with deionized, is dried under the conditions of 50 ~ 110 DEG C, be obtained with core shell structure
Fe@Ni composite granules.
The Fe contents of the iron powder>95wt%, granularity≤300 μm.
The complexing agent be Triammonium citrate, sodium potassium tartrate tetrahydrate and sodium acetate solution in one kind, the complexing agent it is dense
It is 20 ~ 80g/L to spend.
The nickel salt is the one kind in nickel sulfate, nickel chloride and nickel acetate solution；The concentration of the nickel salt is 10 ~ 40g/L.
The stabilizer is the one kind in 2,2'- bipyridyls, thiocarbamide and potassium sulfate.
The reducing agent is the one kind in sodium borohydride, hypophosphorous acid hydrogen sodium and hydrazine solution, and the concentration of the reducing agent is 5
~20g/L。
There is advantages below compared with prior art due to using above-mentioned technical proposal, the present invention：
The present invention utilizes chemical nickel plating method, one layer of densification of Surface coating and the nickel alloy of stabilization in iron powder, so as to tool is obtained
There are the Fe@Ni composite granules of core shell structure.The method is only the priority mixing of several materials, and the iron powder in preparation process is used as base
Body need to only do simple carrying out washing treatment, without doing the treatment such as complicated sensitization, roughening again, you can in iron powder Surface coating stabilization
Nickel dam, the composite granule inoxidizability after cladding is good is strong, receives degree of oxidation smaller with catalyst is made with iron powder compared with, and with proof gold
Category nickel powder makees catalyst compared to more economical；Required raw material iron powder and other chemical reagent, wide material sources, preparation process cycle
Short, process is simple, workable, high yield rate and cost are low.
The Fe@Ni composite granules with core shell structure prepared in the present invention not only plating it is uniform, without it is obvious reunite, into
Point uniform, stable chemical performance and oxidation resistant, and nickel coating has, and hardness is high, the low advantage of contact resistance.With boron hydrogen
Compound or sodium hypophosphite or hydrazine can effectively slow down the corrosion of iron powder for the alkali plating solution of reducing agent, improve coating and with
Iron powder as matrix plating body between adhesion, also commercial weight is big, therefore uses boron hydride or sodium hypophosphite or hydrazine conduct
The chemical nickel plating of reducing agent significantly improves.
Therefore, the characteristics of present invention has process is simple, with short production cycle, strong operability, high yield rate, low cost；System
The Fe@Ni composite granules with core shell structure for obtaining are excellent without obvious reunion, uniform composition, stable chemical performance and inoxidizability
It is good.
Brief description of the drawings
Fig. 1 is a kind of Fe@Ni composite granule X ray diffracting spectrums with core shell structure prepared by the present invention；
Fig. 2 is the electron scanning micrograph of the Fe@Ni composite granules with core shell structure shown in Fig. 1.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and detailed description, not to the limit of its protection domain
System.
To avoid repeating, first the iron powder involved by this specific embodiment is described as follows, is repeated no more in embodiment：
The Fe contents of the iron powder>95wt%, granularity≤300 μm.
Embodiment 1
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.It is the step of preparation method described in the present embodiment：
（1）Iron powder is put into the sodium hydroxide solution that concentration is 10wt%, 1 ~ 3min is stirred, is washed with deionized to neutrality,
Place into the dilution heat of sulfuric acid that concentration is 5wt%, stir 1 ~ 3min, be then washed with deionized to neutrality, dry, obtain
Iron powder after washing.
（2）By complexing agent: the mass ratio of nickel salt is（1.9~2.2）: 1 dispensing, by the network under 35 ~ 50 DEG C of water bath conditions
Mixture and the nickel salt stir, and obtain chelant liquid；Again by reducing agent: the mass ratio of nickel salt is（1.0~1.1）: 1, will be described
Reducing agent stirs in adding the chelant liquid, obtains mixed liquor.
（3）To adding concentration to be 8 ~ 10 for sodium hydroxide solution to the pH value of 20wt% in the mixed liquor, nickel plating is obtained
Liquid；The stabilizer of the 0.06 ~ 0.09wt% of nickel-plating liquid is accounted for addition in the nickel-plating liquid again, 5 ~ 10min is stirred, stabilization is obtained final product
Nickel-plating liquid.
（4）Under agitation, to the institute that the 6 ~ 9wt% of nickel-plating liquid for accounting for the stabilization is added in the nickel-plating liquid of the stabilization
The iron powder after washing is stated, 10 ~ 40min is persistently stirred, covering liquid is obtained.
（5）The covering liquid is washed with deionized, is dried under the conditions of 50 ~ 110 DEG C, be obtained with core shell structure
Fe@Ni composite granules.
The concentration of the complexing agent is 20 ~ 40g/L；The complexing agent is Triammonium citrate.
The concentration of the nickel salt is 10 ~ 20g/L；The nickel salt is nickel sulfate.
The stabilizer is 2,2'- bipyridyls.
The concentration of the reducing agent is 5 ~ 10g/L；The reducing agent is sodium borohydride.
Embodiment 2
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 1 in addition to following：
The complexing agent is sodium potassium tartrate tetrahydrate；
The nickel salt is nickel chloride；
The stabilizer is thiocarbamide；
The reducing agent is hypophosphorous acid hydrogen sodium.
Embodiment 3
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 1 in addition to following：
The complexing agent is sodium acetate solution；
The nickel salt is nickel acetate solution；
The stabilizer is potassium sulfate；
The reducing agent is hydrazine solution.
Embodiment 4
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.It is the step of preparation method described in the present embodiment：
（1）Iron powder is put into the sodium hydroxide solution that concentration is 10wt%, 1 ~ 3min is stirred, is washed with deionized to neutrality,
Place into the dilution heat of sulfuric acid that concentration is 5wt%, stir 1 ~ 3min, be then washed with deionized to neutrality, dry, obtain
Iron powder after washing.
（2）By complexing agent: the mass ratio of nickel salt is（2.2~2.5）: 1 dispensing, by the network under 50 ~ 70 DEG C of water bath conditions
Mixture and the nickel salt stir, and obtain chelant liquid；Again by reducing agent: the mass ratio of nickel salt is（1.1~1.2）: 1, will be described
Reducing agent stirs in adding the chelant liquid, obtains mixed liquor.
（3）To adding concentration to be 10 ~ 12 for sodium hydroxide solution to the pH value of 20wt% in the mixed liquor, nickel plating is obtained
Liquid；The stabilizer of the 0.09 ~ 0.12wt% of nickel-plating liquid is accounted for addition in the nickel-plating liquid again, 5 ~ 10min is stirred, stabilization is obtained final product
Nickel-plating liquid.
（4）Under agitation, to the institute that the 9 ~ 12wt% of nickel-plating liquid for accounting for the stabilization is added in the nickel-plating liquid of the stabilization
The iron powder after washing is stated, 40 ~ 70min is persistently stirred, covering liquid is obtained.
（5）The covering liquid is washed with deionized, is dried under the conditions of 50 ~ 110 DEG C, be obtained with core shell structure
Fe@Ni composite granules.
The concentration of the complexing agent is 40 ~ 60g/L；The complexing agent is Triammonium citrate.
The concentration of the nickel salt is 20 ~ 30g/L；The nickel salt is nickel sulfate.
The stabilizer is 2,2'- bipyridyls.
The concentration of the reducing agent is 10 ~ 15g/L；The reducing agent is sodium borohydride.
Embodiment 5
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 4 in addition to following：
The complexing agent is sodium potassium tartrate tetrahydrate；
The nickel salt is nickel chloride；
The stabilizer is thiocarbamide；
The reducing agent is hypophosphorous acid hydrogen sodium.
Embodiment 6
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 4 in addition to following：
The complexing agent is sodium acetate solution；
The nickel salt is nickel acetate solution；
The stabilizer is potassium sulfate；
The reducing agent is hydrazine solution.
Embodiment 7
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.It is the step of preparation method described in the present embodiment：
（1）Iron powder is put into the sodium hydroxide solution that concentration is 10wt%, 1 ~ 3min is stirred, is washed with deionized to neutrality,
Place into the dilution heat of sulfuric acid that concentration is 5wt%, stir 1 ~ 3min, be then washed with deionized to neutrality, dry, obtain
Iron powder after washing.
（2）By complexing agent: the mass ratio of nickel salt is（2.5~2.8）: 1 dispensing, by the network under 70 ~ 90 DEG C of water bath conditions
Mixture and the nickel salt stir, and obtain chelant liquid；Again by reducing agent: the mass ratio of nickel salt is（1.2~1.3）: 1, will be described
Reducing agent stirs in adding the chelant liquid, obtains mixed liquor.
（3）To adding concentration to be 12 ~ 14 for sodium hydroxide solution to the pH value of 20wt% in the mixed liquor, nickel plating is obtained
Liquid；The stabilizer of the 0.12 ~ 0.15wt% of nickel-plating liquid is accounted for addition in the nickel-plating liquid again, 5 ~ 10min is stirred, stabilization is obtained final product
Nickel-plating liquid.
（4）Under agitation, account for the 12 ~ 15wt%'s of nickel-plating liquid of the stabilization to addition in the nickel-plating liquid of the stabilization
Iron powder after the washing, persistently stirs 70 ~ 100min, obtains covering liquid.
（5）The covering liquid is washed with deionized, is dried under the conditions of 50 ~ 110 DEG C, be obtained with core shell structure
Fe@Ni composite granules.
The concentration of the complexing agent is 60 ~ 80g/L；The complexing agent is Triammonium citrate.
The concentration of the nickel salt is 30 ~ 40g/L；The nickel salt is nickel sulfate.
The stabilizer is 2,2'- bipyridyls.
The concentration of the reducing agent is 15 ~ 20g/L；The reducing agent is sodium borohydride.
Embodiment 8
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 7 in addition to following：
The complexing agent is sodium potassium tartrate tetrahydrate；
The nickel salt is nickel chloride；
The stabilizer is thiocarbamide；
The reducing agent is hypophosphorous acid hydrogen sodium.
Embodiment 9
A kind of Fe@Ni composite granules with core shell structure and preparation method thereof.Remaining is with embodiment 7 in addition to following：
The complexing agent is sodium acetate solution；
The nickel salt is nickel acetate solution；
The stabilizer is potassium sulfate；
The reducing agent is hydrazine solution.
This specific embodiment has advantages below compared with prior art：
This specific embodiment utilizes chemical nickel plating method, one layer of densification of Surface coating and the nickel alloy of stabilization in iron powder, from
And the Fe@Ni composite granules with core shell structure are obtained.The method is only the priority mixing of several materials, the iron in preparation process
Powder need to only do simple carrying out washing treatment as matrix, without doing the treatment such as complicated sensitization, roughening again, you can in iron powder surface bag
The nickel dam of stabilization is covered, the composite granule inoxidizability after cladding is good is strong, smaller by degree of oxidation compared with catalyst is made with iron powder,
It is more economical compared with catalyst is made with simple metal nickel powder；Required raw material iron powder and other chemical reagent, wide material sources, prepared
Journey cycle is short, process is simple, workable, high yield rate and cost are low.
Not only plating is uniform for the Fe@Ni composite granules with core shell structure prepared in this specific embodiment, nothing is obvious
Reunion, composition uniform, stable chemical performance and oxidation resistant, and nickel coating has, and hardness is high, contact resistance is low excellent
Point.Alkali plating solution with boron hydride or sodium hypophosphite or hydrazine as reducing agent can effectively slow down the corrosion of iron powder, improve
Coating and using iron powder as the adhesion between the plating body of matrix, also commercial weight is big, therefore uses boron hydride or sodium hypophosphite
Or hydrazine significantly improves as the chemical nickel plating of reducing agent.
Fig. 1 is a kind of Fe@Ni composite granule X ray diffracting spectrums with core shell structure prepared by embodiment 1, Fig. 1
It can be seen that the thing phase composition of made product is mainly Fe and Ni；Fig. 2 is that the Fe@Ni with core shell structure shown in Fig. 1 are combined
The electron scanning micrograph of powder.Made product surface wraps up one layer of comparatively dense and uniform nickel as can be seen from Figure 2
Layer, serves good antioxidation.
Therefore, this specific embodiment has process is simple, with short production cycle, strong operability, high yield rate, low cost
Feature；The obtained Fe@Ni composite granules with core shell structure are without obvious reunion, uniform composition, stable chemical performance and resist
Oxidisability is excellent.
Claims (7)
1. a kind of preparation method of the Fe@Ni composite granules with core shell structure, it is characterised in that the step of the preparation method
It is：
(1) iron powder is put into the sodium hydroxide solution that concentration is 10wt%, stirs 1~3min, be washed with deionized into
Property, place into the dilution heat of sulfuric acid that concentration is 5wt%, 1~3min is stirred, then it is washed with deionized to neutrality, dry,
Iron powder after being washed；
(2) by complexing agent: the mass ratio of nickel salt is (1.9~2.8): 1 dispensing, by the complexing under 35~90 DEG C of water bath conditions
Agent and the nickel salt stir, and obtain chelant liquid；Reducing agent is pressed again: the mass ratio of nickel salt is (1.0~1.3): 1, will be described
Reducing agent stirs in adding the chelant liquid, obtains mixed liquor；
(3) it is 8~14 for sodium hydroxide solution to the pH value of 20wt% to concentration is added in the mixed liquor, obtains nickel-plating liquid；
The stabilizer of the 0.06~0.15wt% of nickel-plating liquid is accounted for addition in the nickel-plating liquid again, 5~10min is stirred, stabilization is obtained final product
Nickel-plating liquid；
(4) under agitation, accounted for described in the 6~15wt% of nickel-plating liquid of the stabilization to addition in the nickel-plating liquid of the stabilization
Iron powder after washing, persistently stirs 10~100min, obtains covering liquid；
(5) covering liquid is washed with deionized, is dried under the conditions of 50~110 DEG C, the Fe@with core shell structure are obtained
Ni composite granules.
2. the preparation method of the Fe@Ni composite granules with core shell structure according to claim 1, it is characterised in that described
The Fe contents of iron powder>95wt%, granularity≤300 μm.
3. the preparation method of the Fe@Ni composite granules with core shell structure according to claim 1, it is characterised in that described
Complexing agent is the one kind in Triammonium citrate, sodium potassium tartrate tetrahydrate and sodium acetate solution, and the concentration of the complexing agent is 20~80g/
L。
4. the preparation method of the Fe@Ni composite granules with core shell structure according to claim 1, it is characterised in that described
Nickel salt is the one kind in nickel sulfate, nickel chloride and nickel acetate solution；The concentration of the nickel salt is 10~40g/L.
5. the preparation method of the Fe@Ni composite granules with core shell structure according to claim 1, it is characterised in that described
Stabilizer is the one kind in 2,2'- bipyridyls, thiocarbamide and potassium sulfate.
6. the preparation method of the Fe@Ni composite granules with core shell structure according to claim 1, it is characterised in that described
Reducing agent is the one kind in sodium borohydride, hypophosphorous acid hydrogen sodium and hydrazine solution, and the concentration of the reducing agent is 5~20g/L.
7. a kind of Fe@Ni composite granules with core shell structure, it is characterised in that the Fe@Ni composite powders with core shell structure
Body is prepared by the preparation method of the Fe@Ni composite granules with core shell structure according to any one of claim 1~6
The Fe@Ni composite granules with core shell structure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206122A (en) * | 2018-10-30 | 2019-01-15 | 苏州佳耐材料科技有限公司 | A method of improving Ultra-low carbon Magnesia-carbon material microstructure and thermal shock resistance |
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| CN109867529A (en) * | 2019-03-21 | 2019-06-11 | 武汉科技大学 | A kind of combination mutually enhances low-carbon MgO-C refractory material and preparation method thereof |
| CN109967736A (en) * | 2019-03-21 | 2019-07-05 | 武汉科技大学 | A kind of Fe2O3@Ni composite granule and preparation method thereof with core-shell structure |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487246A (en) * | 2018-10-18 | 2019-03-19 | 北京交通大学 | A kind of Ti of magnetism core/shell structure3C2Alkene/Ni powder and preparation method thereof |
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| CN109867529A (en) * | 2019-03-21 | 2019-06-11 | 武汉科技大学 | A kind of combination mutually enhances low-carbon MgO-C refractory material and preparation method thereof |
| CN109967736A (en) * | 2019-03-21 | 2019-07-05 | 武汉科技大学 | A kind of Fe2O3@Ni composite granule and preparation method thereof with core-shell structure |
| CN109867529B (en) * | 2019-03-21 | 2022-03-15 | 武汉科技大学 | Bonding phase reinforced low-carbon MgO-C refractory material and preparation method thereof |
| CN110157363A (en) * | 2019-06-11 | 2019-08-23 | 莱芜职业技术学院 | A kind of preparation method of electromagnetic shielding conductive glue conductive powder |
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