CN104178789A - Process for depositing nickel-copper alloy on electromagnetic pure iron - Google Patents
Process for depositing nickel-copper alloy on electromagnetic pure iron Download PDFInfo
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- CN104178789A CN104178789A CN201410388753.4A CN201410388753A CN104178789A CN 104178789 A CN104178789 A CN 104178789A CN 201410388753 A CN201410388753 A CN 201410388753A CN 104178789 A CN104178789 A CN 104178789A
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- pure iron
- electromagnetic pure
- iron material
- copper alloy
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Abstract
The invention discloses a process for depositing a nickel-copper alloy on electromagnetic pure iron and relates to the technical field of metal material production. The process comprises eight technological processes, namely deoiling, water-washing, oxide removal, chemical polishing, demolding activation, nickel-copper alloy leaching, purification and drying. In the process method, a layer of compact nickel-copper alloy is plated on the surface of the electromagnetic pure iron by adopting a chemical deposition method, so that the process method is simple and easy to operate, and is easy for implementation of automatic production; an obtained nickel-copper alloy plating layer is bright, compact and firm in bonding, is more corrosion-resistant than copper elemental metal, and can be easily welded together with other metals in a vacuum furnace and a hydrogen furnace; an alloy plating layer solder is good in diffusion property; moreover, the process method disclosed by the invention is capable of effectively utilizing an electroplating nickel recovery solution, can be used for reducing the emission of harmful sewage, and is good in environmental friendliness.
Description
Technical field
The present invention relates to metallic substance production technical field, be specifically related to a kind of electromagnetic pure iron nickel deposited copper alloy technique.
Background technology
Electromagnetic pure iron belongs to the category of high magneticsaturation material, has that resistivity is low (is about 10
), particularly Bs (can reach 2.158T, only lower than 50%FeC alloy), under interchange condition, use can cause the resistance of vortex consumption, and be easy to process, the advantages such as low price, therefore it is mainly widely used in especially electrovacuum industry of electron trade, electromagnetic pure iron leaves in air oxidizable, although electronickelling is optimal selection, but electronickelling required equipment complexity and uneven coating even (change geometrical dimension), the limitation such as hydrogen embrittlement, find other coating layer of alternate functionality and protective electronickelling coating, reduce costs, become the maximum target that surface treatment worker pursues, corronel surface is after transpassivation, electropotential corrigendum, corronel coating is cathodic electrodeposition coating with respect to iron, chemistry in the past soaks copper or corronel mainly exists in conjunction with not firm, thereby the restriction iron-based chemistry promotion and application of soaking corronel.
Summary of the invention
It is simple that problem to be solved by this invention is to provide a kind of preparation technology, with low cost, simple to operate, the electromagnetic pure iron nickel deposited copper alloy technique that material use efficiency is good.
To achieve these goals, the technical scheme that the present invention takes for: a kind of electromagnetic pure iron nickel deposited copper alloy technique providing, comprises following processing step:
(1) oil removing: electromagnetic pure iron material is put in the solvent-borne type degreaser under room temperature, use ultrasonic wave oil removing, controlling the oil removing time is 3~8min, then electromagnetic pure iron material is put into temperature again and be in the mixing solutions of the hydrophilic group removers of 30~50 DEG C and sodium hydroxide, again adopt ultrasonic wave oil removing, controlling the oil removing time is 10~15min, finally, it is the sodium hydroxide of 30~50 DEG C that electromagnetic pure iron material after ultrasonic oil removing is put into temperature, in the mixing solutions of phosphoric acid sodium and sodium carbonate, pass to electric current and carry out electrolytic degreasing, control cathode oil removing and anode oil removing time are respectively 180~200s and 150~180s,
(2) washing: be that the water of 35 DEG C of hot water and 20 DEG C is clean by temperature respectively by the electromagnetic pure iron material after step (1) oil removing;
(3) except oxide compound: the electromagnetic pure iron material after step (2) washing is put in the mixing solutions of hydrochloric acid, hydrogen peroxide and ethanol, removed its surperficial oxide compound.
(4) chemical rightenning:, electromagnetic pure iron material is put in the reaction vessels that fills rumbling compound, and reaction vessels is put into thermostat container and carry out chemical reaction except after oxide compound through step (3), the temperature of controlling thermostat container is 20~40 DEG C;
(5) demoulding activation: after step (4) chemical rightenning, electromagnetic pure iron material is put in hydrochloric acid and carried out pickling, wash the oxide film that its surface has been lacked, and play certain activation, control pickling time is 3~5s;
(6) soak corronel: after the activation of step (5) demoulding, electromagnetic pure iron material is put into 5~15
copper sulfate and 100~300
single nickel salt mixing solutions in, through reaction after, plate one deck corronel at electromagnetic pure iron material surface;
(7) passivation: after electromagnetic pure iron material surface plated with nickel copper alloy, it is carried out to Passivation Treatment through step (6);
(8) dry: after step (7) passivation, electromagnetic pure iron material is put in loft drier and dried and get final product to obtain finished product, controlling bake out temperature is 30~35 DEG C, and control drying time is 20~30min.
Preferably, in the ultrasonic oil removing process of described step (1), the concentration of sodium hydroxide solution used is 10~15
, in described electrolytic degreasing process, the concentration of sodium hydroxide, tertiary sodium phosphate and sodium carbonate solution used is respectively 20~35
, 30~50
with 20~35
.
Preferably, in described step (4), rumbling compound used is the mixing solutions of phosphoric acid, sulfuric acid, water, inhibiter and brightening agent, and its massfraction is respectively 30%, 10%, 45%, 10% and 5%.
Preferably, in described step (7), the concrete grammar of Passivation Treatment is,
(1) electromagnetic pure iron material is immersed in rare chromic acid liquor and is processed, controlling treatment temp is 24~28 DEG C, and the control treatment time is 10~30s;
(2), after pickling, electromagnetic pure iron material is cleaned with the pure water of 20~25 DEG C.
Preferably, described rare chromic acid is 3~10
chromium trioxide solution.
Preferably, in described step (1), in the time carrying out primary ultrasonic oil removal treatment, need add the water of 30~50g.
Adopt technical scheme of the present invention, in this processing method, adopt the corronel of chemical deposition in the plated surface last layer densification of electromagnetic pure iron, processing method is simple, easy to operate, easily realize automatic production, in preparation process, by three road oil removing operations, make the greasy dirt content on electromagnetic pure iron surface extremely low, after washing, operate through deoxidation compound again, oxide on surface has obtained cleaning thoroughly, high purity, described chemical rightenning operation can be removed its surperficial oxide compound to greatest extent, improve its purity, the processing parameter of three treating processess by strict this key of control, follow-up operation can be carried out smoothly, improve the bonding force of corronel and electromagnetic pure iron, follow-up by controlling the processing parameter of Passivation Treatment parameter and baking oven well, obtain corronel coating light, fine and close, in conjunction with firm, more corrosion-resistant than copper elemental metals, easy and other metal solder in vacuum oven and hydrogen furnace, alloy layer scolder Diaspora Performance is good, and this processing method can effectively utilize electronickelling to reclaim solution, reduce harmful sewage discharge, environment friendly is good.
Embodiment
embodiment 1:
(1) oil removing: electromagnetic pure iron material is put in the solvent-borne type degreaser under room temperature, and added the water of 32g, use ultrasonic wave oil removing, controlling the oil removing time is 3min, then electromagnetic pure iron material is put into temperature again and be the hydrophilic group removers and 11 of 32 DEG C
in the mixing solutions of sodium hydroxide, again adopt ultrasonic wave oil removing, controlling the oil removing time is 11min, last, by the electromagnetic pure iron material after ultrasonic oil removing put into temperature be 31 DEG C 22
sodium hydroxide, 32
phosphoric acid sodium and 23
in the mixing solutions of sodium carbonate, pass to electric current and carry out electrolytic degreasing, control cathode oil removing and anode oil removing time are respectively 189s and 169s;
(2) washing: be that the water of 35 DEG C of hot water and 20 DEG C is clean by temperature respectively by the electromagnetic pure iron material after step (1) oil removing;
(3) except oxide compound: the electromagnetic pure iron material after step (2) washing is put in the mixing solutions of hydrochloric acid, hydrogen peroxide and ethanol, removed its surperficial oxide compound;
(4) chemical rightenning: after step (3) is removed oxide compound, electromagnetic pure iron material is put in the reaction vessels that fills rumbling compound, and reaction vessels is put into thermostat container and carry out chemical reaction, the temperature of controlling thermostat container is 21 DEG C, wherein, rumbling compound used is the mixing solutions of phosphoric acid, sulfuric acid, water, inhibiter and brightening agent, and its massfraction is respectively 30%, 10%, 45%, 10% and 5%;
(5) demoulding activation: after step (4) chemical rightenning, electromagnetic pure iron material is put in hydrochloric acid and carried out pickling, wash the oxide film that its surface has been lacked, and play certain activation, control pickling time is 3s;
(6) soak corronel: after the activation of step (5) demoulding, electromagnetic pure iron material is put into 9
copper sulfate and 145
single nickel salt mixing solutions in, through reaction after, plate one deck corronel at electromagnetic pure iron material surface;
(7) passivation: after electromagnetic pure iron material surface plated with nickel copper alloy, it is carried out to Passivation Treatment through step (6), concrete grammar is,
1) electromagnetic pure iron material is immersed in to 7
chromium trioxide solution in process, control treatment temp be 24 DEG C, the control treatment time is 12s;
2), after pickling, electromagnetic pure iron material is cleaned with the pure water of 23 DEG C.;
(8) dry: after step (7) passivation, electromagnetic pure iron material is put in loft drier and dried and get final product to obtain finished product, controlling bake out temperature is 32 DEG C, and control drying time is 21min.
embodiment 2:all the other are identical with embodiment 1, and difference is in described step (1), for the first time in ultrasonic oil removing, the water yield adding is 40g, and the oil removing time is 5min, for the second time in ultrasonic oil removing, the temperature of controlling mixing solutions is 38 DEG C, and the concentration of sodium hydroxide solution of selecting is 13
, in electrolytic degreasing, the temperature of controlling mixing solutions is 37 DEG C, sodium hydroxide, phosphoric acid sodium and the concentration of sodium carbonate selected are respectively 22
, 33
with 26
, control cathode oil removing and anode oil removing time are respectively 190s and 170s; In described step (4), the temperature of controlling thermostat container is 30 DEG C; In described step (5), control pickling time is 4s; In described step (6), the copper sulfate of selecting and the concentration of nickel sulfate solution are respectively 10
with 150
; In described step (7), the concentration of the chromium trioxide solution of selecting is 8
, controlling treatment temp is 26 DEG C, controls treatment time 20s, the temperature of controlling pure water is 24 DEG C; In described step (8), controlling bake out temperature is 34 DEG C, and control drying time is 25min.
embodiment 3:all the other are identical with embodiment 1, and difference is in described step (1), for the first time in ultrasonic oil removing, the water yield adding is 42g, and the oil removing time is 6min, for the second time in ultrasonic oil removing, the temperature of controlling mixing solutions is 39 DEG C, and the concentration of sodium hydroxide solution of selecting is 14
, in electrolytic degreasing, the temperature of controlling mixing solutions is 38 DEG C, sodium hydroxide, phosphoric acid sodium and the concentration of sodium carbonate selected are respectively 24
, 35
with 27
, control cathode oil removing and anode oil removing time are respectively 195s and 172s; In described step (4), the temperature of controlling thermostat container is 31 DEG C; In described step (5), control pickling time is 5s; In described step (6), the copper sulfate of selecting and the concentration of nickel sulfate solution are respectively 12
with 155
; In described step (7), the concentration of the chromium trioxide solution of selecting is 9
, controlling treatment temp is 27 DEG C, controls treatment time 22s, the temperature of controlling pure water is 25 DEG C; In described step (8), controlling bake out temperature is 35 DEG C, and control drying time is 27min.
After above processing step, take out electromagnetic pure iron plating piece material sample, to be measured:
。
From above data, the electromagnetic pure iron plating piece material sample luminance brightness of producing is high, and coating is combined stability with electromagnetic pure iron material excellent, difficult drop-off, and the good welding performance of material, in vacuum oven and hydrogen furnace, be easy to other metal solder, alloy layer scolder free-running property is good, and solidity to corrosion is good, and preparation technology is simple, with low cost, technology stability is good, and environment friendly is good.
Obviously specific implementation of the present invention is not subject to the restrictions described above; as long as adopted the improvement of the various unsubstantialities that method of the present invention design and technical scheme carry out; or without improving, design of the present invention and technical scheme are directly applied to other occasion, all within protection scope of the present invention.
Claims (6)
1. an electromagnetic pure iron nickel deposited copper alloy technique, comprises following processing step:
(1) oil removing: electromagnetic pure iron material is put in the solvent-borne type degreaser under room temperature, use ultrasonic wave oil removing, controlling the oil removing time is 3~8min, then electromagnetic pure iron material is put into temperature again and be in the mixing solutions of the hydrophilic group removers of 30~50 DEG C and sodium hydroxide, again adopt ultrasonic wave oil removing, controlling the oil removing time is 10~15min, finally, it is the sodium hydroxide of 30~50 DEG C that electromagnetic pure iron material after ultrasonic oil removing is put into temperature, in the mixing solutions of phosphoric acid sodium and sodium carbonate, pass to electric current and carry out electrolytic degreasing, control cathode oil removing and anode oil removing time are respectively 180~200s and 150~180s,
(2) washing: be that the water of 35 DEG C of hot water and 20 DEG C is clean by temperature respectively by the electromagnetic pure iron material after step (1) oil removing;
(3) except oxide compound: the electromagnetic pure iron material after step (2) washing is put in the mixing solutions of hydrochloric acid, hydrogen peroxide and ethanol, removed its surperficial oxide compound;
(4) chemical rightenning:, electromagnetic pure iron material is put in the reaction vessels that fills rumbling compound, and reaction vessels is put into thermostat container and carry out chemical reaction except after oxide compound through step (3), the temperature of controlling thermostat container is 20~40 DEG C;
(5) demoulding activation: after step (4) chemical rightenning, electromagnetic pure iron material is put in hydrochloric acid and carried out pickling, wash the oxide film that its surface has been lacked, and play certain activation, control pickling time is 3~5s;
(6) soak corronel: after the activation of step (5) demoulding, electromagnetic pure iron material is put into 5~15
copper sulfate and 100~300
single nickel salt mixing solutions in, through reaction after, plate one deck corronel at electromagnetic pure iron material surface;
(7) passivation: after electromagnetic pure iron material surface plated with nickel copper alloy, it is carried out to Passivation Treatment through step (6);
(8) dry: after step (7) passivation, electromagnetic pure iron material is put in loft drier and dried and get final product to obtain finished product, controlling bake out temperature is 30~35 DEG C, and control drying time is 20~30min.
2. a kind of electromagnetic pure iron nickel deposited copper alloy technique according to claim 1, is characterized in that: in the ultrasonic oil removing process of described step (1), the concentration of sodium hydroxide solution used is 10~15
, in described electrolytic degreasing process, the concentration of sodium hydroxide, tertiary sodium phosphate and sodium carbonate solution used is respectively 20~35
, 30~50
with 20~35
.
3. a kind of electromagnetic pure iron nickel deposited copper alloy technique according to claim 1, it is characterized in that: in described step (4), rumbling compound used is the mixing solutions of phosphoric acid, sulfuric acid, water, inhibiter and brightening agent, and its massfraction is respectively 30%, 10%, 45%, 10% and 5%.
4. a kind of electromagnetic pure iron nickel deposited copper alloy technique according to claim 1, is characterized in that: in described step (7), the concrete grammar of Passivation Treatment is,
(1) electromagnetic pure iron material is immersed in rare chromic acid liquor and is processed, controlling treatment temp is 24~28 DEG C, and the control treatment time is 10~30s;
(2), after pickling, electromagnetic pure iron material is cleaned with the pure water of 20~25 DEG C.
5. a kind of electromagnetic pure iron nickel deposited copper alloy technique according to claim 4, is characterized in that: described rare chromic acid is 3~10
chromium trioxide solution.
6. a kind of electromagnetic pure iron nickel deposited copper alloy technique according to claim 1, is characterized in that: in described step (1), in the time carrying out primary ultrasonic oil removal treatment, need add the water of 30~50g.
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Cited By (2)
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CN105714293A (en) * | 2014-12-04 | 2016-06-29 | 安泰科技股份有限公司 | Composite material having both high magnetic conduction and high electric conduction and preparation method thereof |
CN112030147A (en) * | 2020-07-17 | 2020-12-04 | 沈阳航天新光集团有限公司 | Electromagnetic pure iron chemical nickel and phosphorus alloy plating process |
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2014
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Patent Citations (2)
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CN101280444A (en) * | 2007-12-29 | 2008-10-08 | 横店集团东磁有限公司 | Anticorrosive electroplating method for Nd-Fe-B magnet steel |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105714293A (en) * | 2014-12-04 | 2016-06-29 | 安泰科技股份有限公司 | Composite material having both high magnetic conduction and high electric conduction and preparation method thereof |
CN105714293B (en) * | 2014-12-04 | 2018-12-21 | 安泰科技股份有限公司 | It is a kind of to have both high magnetic conduction and highly conductive composite material and preparation method |
CN112030147A (en) * | 2020-07-17 | 2020-12-04 | 沈阳航天新光集团有限公司 | Electromagnetic pure iron chemical nickel and phosphorus alloy plating process |
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