CN107541758A - A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating - Google Patents
A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating Download PDFInfo
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- CN107541758A CN107541758A CN201710644747.4A CN201710644747A CN107541758A CN 107541758 A CN107541758 A CN 107541758A CN 201710644747 A CN201710644747 A CN 201710644747A CN 107541758 A CN107541758 A CN 107541758A
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 73
- 238000000576 coating method Methods 0.000 title claims abstract description 42
- 239000011248 coating agent Substances 0.000 title claims abstract description 41
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 38
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000151 deposition Methods 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 4
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 14
- 230000000996 additive effect Effects 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 7
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 7
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 7
- 229940081974 saccharin Drugs 0.000 claims description 7
- 235000019204 saccharin Nutrition 0.000 claims description 7
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- HAHASQAKYSVXBE-WAYWQWQTSA-N (z)-2,3-diethylbut-2-enedioic acid Chemical compound CC\C(C(O)=O)=C(/CC)C(O)=O HAHASQAKYSVXBE-WAYWQWQTSA-N 0.000 claims description 3
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 claims description 3
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 claims description 3
- 229930016911 cinnamic acid Natural products 0.000 claims description 3
- 235000013985 cinnamic acid Nutrition 0.000 claims description 3
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 claims description 3
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 3
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims description 3
- 235000021419 vinegar Nutrition 0.000 claims description 3
- 239000000052 vinegar Substances 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- JSPXPZKDILSYNN-UHFFFAOYSA-N but-1-yne-1,4-diol Chemical class OCCC#CO JSPXPZKDILSYNN-UHFFFAOYSA-N 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- GHUURDQYRGVEHX-UHFFFAOYSA-N prop-1-ynylbenzene Chemical compound CC#CC1=CC=CC=C1 GHUURDQYRGVEHX-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 44
- 229910052799 carbon Inorganic materials 0.000 description 39
- 239000002131 composite material Substances 0.000 description 16
- 229910010271 silicon carbide Inorganic materials 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 7
- 239000004744 fabric Substances 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 150000001722 carbon compounds Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006263 metalation reaction Methods 0.000 description 2
- XNERWVPQCYSMLC-UHFFFAOYSA-N phenylpropiolic acid Chemical compound OC(=O)C#CC1=CC=CC=C1 XNERWVPQCYSMLC-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- MJBPUQUGJNAPAZ-UHFFFAOYSA-N Butine Natural products O1C2=CC(O)=CC=C2C(=O)CC1C1=CC=C(O)C(O)=C1 MJBPUQUGJNAPAZ-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon carbide compound Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
Abstract
The present invention relates to a kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, belong to technical field of surface.Carbon-based material is heat-treated by the present invention, and ultrasonic cleaning obtains pre-processing carbon-based material；Prepare iron-nickel alloy electric depositing solution, to pre-process carbon-based material as negative electrode, iron-nickel alloy plate is anode, iron-nickel alloy electric depositing solution is electroplate liquid, under the conditions of temperature is 30 ~ 50 DEG C, the min of electro-deposition 5 ~ 60 is carried out using dc source, negative electrode is taken out and is cleaned, is drying to obtain iron-nickel alloy coating.The present invention can deposit iron-nickel alloy coating on carbon-based material surface, the thermal coefficient of expansion of coating is close with carbon-based material, and there is the interface cohesion of micron level between coating and carbon-based material, remain to keep interface cohesion close after the thermal cycle of 800 DEG C of room temperature of experience.
Description
Technical field
The present invention relates to a kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, belong to process for treating surface
Field.
Background technology
The conventional method of carbon-based material surface metalation has spraying process, PVD method, CVD etc..Wherein spraying process, PVD, CVD
The methods of need special equipment and exacting terms, and gained metal level is there is stress, hole and crackle etc., thus limits
Their application and popularization；Use metal dust or slurry carbon-based material surface is coated after again high temperature sintering to realize surface
The method of metallization also has been reported that.But carbon-based material surface metalation is carried out using existing conventional method, for carbon-based material
Intrinsic micron order hole itself can not realize the deep filling of metal level and form intimate interfacial combination.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of in the side of carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating
Method, i.e., the deposition of iron-nickel alloy coating can be realized on carbon-based material surface using electrodeposition technology, interface has micron level
Combine closely, be greatly improved bond strength, and play the low bulk performance characteristics of iron-nickel alloy, realize and carbon-based material base
The thermal expansion matching of body.
A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, concretely comprise the following steps：
（1）Carbon-based material is heat-treated, ultrasonic cleaning obtains pre-processing carbon-based material；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.2~0.5
mol/L、NiCl2 0.1~0.2 mol/L、FeSO4 0.03~0.1 mol/L、H3BO3 0.2~0.5 mol/L、NaCl 0.1~
0.25 mol/L, the g/L of ascorbic acid 0.5 ~ 2,1 ~ 2.5g/L of saccharin, 0.05 ~ 0.3g/L of additive A,
Surplus is deionized water；
（3）With step（1）Gained pretreatment carbon-based material is negative electrode, and iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electricity
Deposition solution is electroplate liquid, and under the conditions of temperature is 30 ~ 50 DEG C, the min of electro-deposition 5 ~ 60 is carried out using dc source, is taken out cloudy
Cleaned, be drying to obtain iron-nickel alloy coating in pole；
The step（1）The temperature of middle heat treatment is 150 ~ 350 DEG C, and the time of heat treatment is 10 ~ 20min, and heat-treating atmosphere is
Air atmosphere or oxygen-containing atmosphere, ultrasonic cleaning frequency are 60 ~ 130KHZ, 3 ~ 10min of scavenging period；
The step（2）Middle additive A is adjacent sulfo group benzaldehyde, adjacent shuttle base cinnamic acid, diethyl maleic acid vinegar, 1,4- butine two
Alcohol or phenyl propiolic acid；
The step（3）The area ratio of middle negative electrode and anode is 1:(1 ~ 4), Anode-cathode Distance are 3 ~ 15cm；The moon during electro-deposition
Electrode current density is 2 ~ 5 A/dm2；
The step（3）Middle cleaning is cleaned using deionized water rinsing, soaked in absolute ethyl alcohol；
Iron-nickel alloy coating purity >=99.5% of the present invention, containing impurity≤0.5% such as C, S, thickness of coating is 0.006 ~ 0.5 mm；
Beneficial effects of the present invention：
（1）Method technique of the invention in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating is simple, safe and reliable, equipment letter
It is single；
（2）The layer of iron-nickel alloy that the inventive method deposits on carbon-based material surface, the interface cohesion between matrix is close, and for
Loose cavity, crackle or microfluctuation existing for composite material surface, show fabulous fill, deeply and covering energy
Power, micro interface adhesion are big；
（3）Surface metal-layer of the present invention and substrate composite similar thermal expansion coefficient, the surface metal-layer in Thermal Cycling
It is smaller with the interfacial thermal stress of substrate so that the carbon-based material after deposition layer of iron-nickel alloy, after undergoing certain elevated temperature thermal cycles,
It is in the interface combined closely still to retain coating and matrix, phenomena such as avoiding that interface unbound, cracking occurs.
Brief description of the drawings
Fig. 1 is interface microscopic appearance of the embodiment of the present invention 1 in surface of carbon/carbon composite Electrodeposition Bath of Iron nickel alloy coating
Figure；
Fig. 2 is that the embodiment of the present invention 1 is followed in surface of carbon/carbon composite Electrodeposition Bath of Iron nickel alloy coating experience room temperature ~ 800 DEG C heat
The interface microscopic appearance figure of ring；
Fig. 3 is interface microscopic appearance of the embodiment of the present invention 2 in carbon/carbon/silicon carbide composite material surface Electrodeposition Bath of Iron nickel alloy coating
Figure；
Fig. 4 is that the embodiment of the present invention 2 undergoes room temperature ~ 800 DEG C in carbon/carbon/silicon carbide composite material surface Electrodeposition Bath of Iron nickel alloy coating
The interface microscopic appearance figure of thermal cycle.
Embodiment
The present invention is described in further detail with reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1：A kind of method in surface of carbon/carbon composite Electrodeposition Bath of Iron nickel alloy coating, concretely comprise the following steps：
（1）Carbon/carbon compound material is heat-treated after sand paper is polished and is cleaned, and is cleaned by ultrasonic in deionized water to there is no black
Coloured particles thing separates out to obtain pretreatment carbon-based material, and wherein heat-treating atmosphere is air atmosphere, and the temperature of heat treatment is 200 DEG C,
The time of heat treatment is 20min；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.5mol/L、
NiCl2 0.2 mol/L、FeSO4 0.1 mol/L、H3BO30.25 0.15 mol/L of mol/L, NaCl, the g/ of ascorbic acid 1
L, saccharin 2g/L, additive A（Additive A is 1,4- butynediols）0.15g/L, surplus are deionized water；
（3）By step（2）Iron-nickel alloy electric depositing solution be ultrasonically treated 5min, with step（1）Gained pre-processes carbon-based material
For negative electrode, iron-nickel alloy plate is anode, and iron-nickel alloy electric depositing solution is electroplate liquid, is adjusted by the way of insulating tape parcel
The compound cathode area of carbon/carbon, negative electrode, the area ratio of anode are arranged to 1:2, adjustment Anode-cathode Distance is 5cm, by negative electrode, sun
Pole is connected and is soaked in electric depositing solution with dc source, carries out ultrasonic vibration and handles 20 min；It is 30 DEG C of conditions in temperature
Under, the min of electro-deposition 40 is carried out using dc source, wherein cathode-current density is 3.7 A/dm2, take out negative electrode using go from
Sub- water rinses, soaked in absolute ethyl alcohol cleans, is drying to obtain the iron-nickel alloy coating combined closely with carbon/carbon compound material；
Surface of carbon/carbon composite Electrodeposition Bath of Iron nickel alloy coating interface microscopic appearance is as shown in Figure 1 obtained by the present embodiment, it is seen that
Interface cohesion between coating and matrix is close, and is shown for micron order hole or crackle existing for matrix surface fabulous
Go deep into filling capacity；Surface of carbon/carbon composite Electrodeposition Bath of Iron nickel alloy coating experience room temperature ~ 800 DEG C heat obtained by the present embodiment
The interface microscopic appearance figure of circulation is as shown in Figure 2；It can be seen that after the thermal cycle of experience room temperature ~ 800 DEG C, still retain between coating and matrix
The interface combined closely.
Embodiment 2：A kind of method in carbon/carbon/silicon carbide composite material surface Electrodeposition Bath of Iron nickel alloy coating, specific steps
For：
（1）Carbon/composite material of silicon carbide is heat-treated after sand paper is polished and is cleaned, and is cleaned by ultrasonic in deionized water to no longer
There is black particle thing to separate out to obtain pretreatment carbon-based material, wherein heat-treating atmosphere is air atmosphere, and the temperature of heat treatment is 350
DEG C, the time of heat treatment is 20min；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.3mol/L、
NiCl2 0.1 mol/L、FeSO4 0.08mol/L、H3BO30.5 0.25 mol/L of mol/L, NaCl, the g/ of ascorbic acid 2
L, saccharin 2.5g/L, additive A（Additive A is adjacent shuttle base cinnamic acid）0.08g/L, surplus are deionization
Water；
（3）By step（2）Iron-nickel alloy electric depositing solution be ultrasonically treated 10min, with step（1）Gained pre-processes carbon/carbonization
Silicon composite is negative electrode, and iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electric depositing solution be electroplate liquid, using exhausted
The mode of edge adhesive tape parcel adjusts the cathode area of carbon/composite material of silicon carbide, and negative electrode, the area ratio of anode are arranged to 1:1,
Adjustment Anode-cathode Distance is 8cm, and negative electrode, anode and dc source are connected and be soaked in electric depositing solution, carries out ultrasonic shake
Swing 10 min of processing；Under the conditions of temperature is 50 DEG C, the min of electro-deposition 60, wherein cathode-current density are carried out using dc source
For 5A/dm2, take out negative electrode and cleaned, be drying to obtain and carbon/silicon carbide compound material using deionized water rinsing, soaked in absolute ethyl alcohol
Expect the iron-nickel alloy coating combined closely；
Carbon/carbon/silicon carbide composite material surface Electrodeposition Bath of Iron nickel alloy coating interface microscopic appearance obtained by the present embodiment as shown in figure 3,
It can be seen that the interface cohesion between coating and matrix is close, and for micron order hole existing for carbon/carbon/silicon carbide composite material surface or
Contoured surface, which is shown, fabulous gos deep into filling capacity；Carbon/carbon/silicon carbide composite material surface Electrodeposition Bath of Iron obtained by the present embodiment
The interface microscopic appearance figure of nickel alloy coating experience room temperature ~ 800 DEG C thermal cycle is as shown in Figure 4, it is seen that experience room temperature ~ 800 DEG C
Still retain the interface combined closely after thermal cycle, between coating and matrix.
Embodiment 3：A kind of method in graphitic surface galvanic deposit iron-nickel alloy coating, concretely comprise the following steps：
（1）Block graphite is heat-treated after sand paper is polished and is cleaned, and is cleaned by ultrasonic in deionized water to there is no black
Grain thing separates out to obtain pretreatment carbon-based material, and wherein heat-treating atmosphere is air atmosphere, and the temperature of heat treatment is 150 DEG C, at heat
The time of reason is 10min；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.2mol/L、
NiCl2 0.15 mol/L、FeSO4 0.03mol/L、H3BO30.2 0.1 mol/L of mol/L, NaCl, ascorbic acid 0.5
G/L, saccharin 1g/L, additive A（Additive A is phenyl propiolic acid）0.05g/L, surplus are deionized water；
（3）By step（2）Iron-nickel alloy electric depositing solution be ultrasonically treated 8min, with step（1）Gained pre-processes block graphite
For negative electrode, iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electric depositing solution be electroplate liquid, wrapped up using insulating tape
Mode adjust the cathode area of block graphite, negative electrode, the area ratio of anode are arranged to 1:3, adjustment Anode-cathode Distance is 3cm,
Negative electrode, anode and dc source are connected and be soaked in electric depositing solution, ultrasonic vibration is carried out and handles 10 min；It is in temperature
Under the conditions of 40 DEG C, the min of electro-deposition 45 is carried out using dc source, wherein cathode-current density is 4.2A/dm2, take out negative electrode and adopt
Cleaned with deionized water rinsing, soaked in absolute ethyl alcohol, be drying to obtain the iron-nickel alloy coating combined closely with graphite surface.
Embodiment 4：A kind of method in graphitic surface galvanic deposit iron-nickel alloy coating, concretely comprise the following steps：
（1）Block graphite is heat-treated after sand paper is polished and is cleaned, and is cleaned by ultrasonic in deionized water to there is no black
Grain thing separates out to obtain pretreatment carbon-based material, and wherein heat-treating atmosphere is oxygen-containing atmosphere, and the temperature of heat treatment is 150 DEG C, at heat
The time of reason is 10min；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.4mol/L、
NiCl2 0.1 mol/L、FeSO4 0.07mol/L、H3BO30.45 0.2 mol/L of mol/L, NaCl, the g/ of ascorbic acid 2
L, saccharin 1.75g/L, additive A（Additive A is diethyl maleic acid vinegar）0.25g/L, surplus for go from
Sub- water；
（3）By step（2）Iron-nickel alloy electric depositing solution be ultrasonically treated 6min, with step（1）Gained pre-processes block graphite
For negative electrode, iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electric depositing solution be electroplate liquid, wrapped up using insulating tape
Mode adjust the cathode area of block graphite, negative electrode, the area ratio of anode are arranged to 1:4, adjusting Anode-cathode Distance is
15cm, negative electrode, anode and dc source are connected and be soaked in electric depositing solution, carried out ultrasonic vibration and handle 10 min；
Under the conditions of temperature is 35 DEG C, the min of electro-deposition 60 is carried out using dc source, wherein cathode-current density is 3.5A/dm2, take out
Negative electrode is cleaned using deionized water rinsing, soaked in absolute ethyl alcohol, is drying to obtain the iron-nickel alloy plating combined closely with graphite surface
Layer.
Embodiment 5：A kind of method in carbon cloth surface Electrodeposition Bath of Iron nickel alloy coating, concretely comprise the following steps：
（1）Carbon cloth is once purged to be heat-treated, and is cleaned by ultrasonic to there is no black particle thing to separate out in deionized water
To pretreatment carbon cloth, wherein heat-treating atmosphere be oxygen-containing atmosphere, and the temperature of heat treatment is 150 DEG C, and the time of heat treatment is
20min；
（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.3mol/L、
NiCl2 0.1 mol/L、FeSO4 0.05mol/L、H3BO30.4 0.25 mol/L of mol/L, NaCl, the g/ of ascorbic acid 1
L, saccharin 2g/L, additive A（Additive A is adjacent sulfo group benzaldehyde）0.3g/L, surplus are deionized water；
（3）By step（2）Iron-nickel alloy electric depositing solution be ultrasonically treated 8min, with step（1）Gained pre-processes carbon cloth
For negative electrode, iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electric depositing solution be electroplate liquid, wrapped up using insulating tape
Mode adjust the cathode area of carbon cloth, negative electrode, the area ratio of anode are arranged to 1:1, adjustment Anode-cathode Distance is 3cm,
Negative electrode, anode and dc source are connected and be soaked in electric depositing solution, ultrasonic vibration is carried out and handles 10 min；It is in temperature
Under the conditions of 45 DEG C, the min of electro-deposition 5 is carried out using dc source, wherein cathode-current density is 5A/dm2, take out negative electrode and use
Deionized water rinsing, soaked in absolute ethyl alcohol cleaning, it is drying to obtain the iron-nickel alloy coating combined closely with carbon cloth surface.
Claims (4)
- A kind of 1. method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, it is characterised in that concretely comprise the following steps：（1）Carbon-based material is heat-treated, ultrasonic cleaning obtains pre-processing carbon-based material；（2）Iron-nickel alloy electric depositing solution is prepared, the wherein component of iron-nickel alloy electric depositing solution is NiSO4 0.2~0.5 mol/ L、NiCl2 0.1~0.2 mol/L、FeSO4 0.03~0.1 mol/L、H3BO3 0.2~0.5 mol/L、NaCl 0.1~0.25 Mol/L, the g/L of ascorbic acid 0.5 ~ 2,1 ~ 2.5g/L of saccharin, 0.05 ~ 0.3g/L of additive A, surplus are Deionized water；（3）With step（1）Gained pretreatment carbon-based material is negative electrode, and iron-nickel alloy plate is anode, step（2）Iron-nickel alloy electricity Deposition solution is electroplate liquid, and under the conditions of temperature is 30 ~ 50 DEG C, the min of electro-deposition 5 ~ 60 is carried out using dc source, is taken out cloudy Cleaned, be drying to obtain iron-nickel alloy coating in pole.
- 2. according to claim 1 in the method for carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, it is characterised in that：Step （1）The temperature of middle heat treatment is 150 ~ 350 DEG C, and the time of heat treatment is 10 ~ 20min, and heat-treating atmosphere is air atmosphere or contained Oxygen atmosphere.
- 3. according to claim 1 in the method for carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, it is characterised in that：Step （2）Middle additive A is adjacent sulfo group benzaldehyde, adjacent shuttle base cinnamic acid, diethyl maleic acid vinegar, 1,4- butynediols or phenyl propyne Acid.
- 4. according to claim 1 in the method for carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating, it is characterised in that：Step （3）The area ratio of middle negative electrode and anode is 1:(1 ~ 4), Anode-cathode Distance are 3 ~ 15cm；Cathode-current density during electro-deposition is 2 ~5 A/dm2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710644747.4A CN107541758A (en) | 2017-08-01 | 2017-08-01 | A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating |
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| CN108441909A (en) * | 2018-03-22 | 2018-08-24 | 无锡神意模具新材料有限公司 | A kind of graphite powder plating nickel on surface method |
| CN110344078A (en) * | 2019-07-03 | 2019-10-18 | 湖北大学 | A kind of nickel foam@cobalt molybdenum phosphide/ferronickel double-hydroxide electrode and the preparation method and application thereof |
| CN112701306A (en) * | 2021-01-30 | 2021-04-23 | 江西理工大学 | Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof |
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| CN112701306A (en) * | 2021-01-30 | 2021-04-23 | 江西理工大学 | Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof |
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