CN102002748A - Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition - Google Patents
Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition Download PDFInfo
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Abstract
The invention relates to a method for preparing a composite material, which comprises the following steps of: putting a basal body subjected to pretreatment into a conventional electroplating bath, and applying an electric field and an ultrasonic field on the plating bath with an ultrasonic generator and a pulsing power source. The process of pulse-ultrasound electrodeposition generally comprises the following steps of: 1, elecroplating pretreatment comprising pretreatment of the basal body and preparation of electroplate liquid; 2, electrodeposition process: putting the basal body which is pretreated in the step one into the prepared electroplate liquid for electrodeposition; and3, post treatment of plating parts, mainly comprising the working procedures of ultrasonic cleaning for the plating parts which are deposited in the step two and anhydrous alcohol cleaning. In the invention, in the electroplate liquid containing nickel and iron ions and insoluble nanoparticles, the nanoparticles are uniformly distributed in the liquid by using ultrasonic stirring, the nanoparticles and substrate metal ions are simultaneously deposited to obtain the ferromagnetic nano composite material composed of substrate metal nickel-iron and the nanoparticles under the condition that positive and negative pulse current or voltage are applied.
Description
Technical field
The method of pulse of the present invention-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material relates to composite material and preparation method thereof, specifically relates to the impulse ultrasound electro-deposition method of ferromagnetic nano matrix material.
Background technology
Present develop rapidly along with modern science and technology, industrial circle has proposed various new requirements to the surface property of material, single-material is difficult to satisfy this demand, and the matrix material that therefore has novel texture and multiple specific function has obtained increasingly extensive concern and application.Matrix material is the differing materials by two or more, a kind of novel material that they is combined with each other and forms by appropriate means.Its performance is better than forming any material of matrix material.Matrix material is because its excellent comprehensive performances, particularly the designability of its performance is widely used in fields such as aerospace, national defence, traffic, physical culture, nano composite material then is wherein the most attractive part, development in recent years is very fast, and the strategy of world developed country new material development all is put into important position to the development of nano composite material.
Nano magnetic material is a kind of novel magnetic material that occurs the eighties in 20th century.When particle size is nano level, because of the feature physical length relevant with magnetic is in nanometer scale just, its multiple electromagnetic property or physical property is changed, and then make the characteristic of nano magnetic material be different from conventional material.Therefore research and develop the extensive concern that the novel nano magneticsubstance has caused countries in the world.Materials science holds an important position in current new technology development.Various top layers functional materials and metal matrix sandwich with the impulse ultrasound electro-deposition method is produced not only can satisfy the special requirement of various occasions, and can also simplify production technique, save valuable starting material and reduce cost.The amorphous alloy of prepared by electrodeposition, ferromagnetic nano level multilayer film and function-graded material etc. also all have very wide development prospect.At existing problem in the above-mentioned prior art, the method for a kind of novel pulse-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material of research and design, existing problem is very necessary in the prior art thereby overcome.
Summary of the invention
In view of existing problem in the above-mentioned prior art, the method that the objective of the invention is a kind of novel pulse-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material of research and design, thereby solve the requirement of industrial circle to the surface property of material, single-material is difficult to satisfy the demands, the development of the matrix material of multiple specific function and application problem.The method of pulse of the present invention-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is that matrix is inserted in the conventional plating tank through after the pre-treatment, is that coating bath applies electric field and ultrasonic field by the ultra-sonic generator and the pulse power; The process of impulse ultrasound galvanic deposit generally is made up of following steps:
The first step: pre-electroplating treatment: comprise a) the pre-treatment b of matrix) preparation of electroplate liquid;
Second step: electrodeposition process: the first step is put into the electroplate liquid that is configured through the matrix of pre-treatment carry out galvanic deposit;
The 3rd step: the aftertreatment of plating piece: comprise that mainly the plating piece that the second step deposition is finished carries out ultrasonic cleaning, the dehydrated alcohol matting.
Matrix pre-treatment of the present invention is: matrix is carried out oil removing, rust cleaning, electropolishing and reactivation process successively.
Each component of solution that matrix is carried out oil removing of the present invention is:
NaOH 80～100g/l
Na3PO4 50～60g/l
Temperature 60～80
Deruster prescription: H2SO4 150～200g/l
HCl 50～60g/l
OP emulsifying agent 3～5g/l
Thiocarbamide 4g/l
Sodium lauryl sulphate 0.02～0.05g/l
Temperature (℃) normal temperature
Electropolishing solution formula and processing parameter:
H3PO4 72％
Chromic acid 23%
Current density 20～100A/dm2
Temperature (℃) 65～75
Activation: carry out under the dilute hydrochloric acid with 10%, normal temperature, the time is 30～60S.
Consisting of of electroplate liquid of the present invention:
Single nickel salt (NiSO
46H
2O) 200g/l～350g/l
Nickelous chloride (NiCl
26H
2O) 40g/l～60g/l
Ferrous sulfate (FeSO
47H
2O) 10g/l～30g/l
Boric acid (H
3BO
3) 30g/l～50g/l
Asccharin 3g/l～5g/l
Nano particle 2g/l～8g/l
Sodium lauryl sulphate 0.1g/l～1g/l.
Nano particle of the present invention is nano particles such as titanium nitride TiN, silicon carbide SiC, titanium carbide TiC, and the particle diameter of nanoparticle is 20nm～100nm; The nano particle of selling on the market should be inserted and be cleaned in the container and dispersion treatment, and amount adds in the solution that will dispose in accordance with regulations then.
Positive negative pulse stuffing power supply and the ultra-sonic generator of when galvanic deposit, using of the present invention, the processing parameter that is adopted is:
(1) ultrasonic wave
Wave direction X, Y, X+Y
Power 0～360W
(2) pulsed current
Pulse width 0～200ms
Pulse interval 0～1000ms
Pulse duty factor 0.20～1
Pulse-repetition 5～5000Hz
The pulse waveform rectangle
(3) supporting electrode Ni plate
(4) interpole gap 20～40mm
(5)PH 2～4
(6) temperature is 50 ℃～70 ℃
(7) depositing time 30～90min.
Aftertreatment to sedimentary plating piece of the present invention mainly comprises ultrasonic cleaning, the dehydrated alcohol matting.
The objective of the invention is to propose a kind of pulsed current and ultrasonic wave turbulent compound action of utilizing, in the tap a blast furnace processing method of magnetic nanometer composite material of steel metal parts surface preparation.The used major equipment of impulse ultrasound electro-deposition method that the present invention proposes has positive negative pulse stuffing power supply, ultrasonic generator, suitable coating bath, electric wire etc.Nano level metal compound of the present invention is nano particles such as titanium nitride TiN, silicon carbide SiC.Can select wherein one or more composition according to the needs of matrix material.Before the electroplate liquid preparation, the nano particle of selling on the market should be inserted and be cleaned in the container and dispersion treatment, and amount adds in the solution that will dispose in accordance with regulations then.
The concrete steps of pulse-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material are as follows:
The first step: the pre-treatment of matrix: oil removing, rust cleaning, electropolishing and activation.
Second step: will put into electroplate liquid through the matrix of the first step pre-treatment and carry out galvanic deposit.Control PH 2～4,50 ℃～70 ℃ of temperature, supporting electrode Ni plate, interpole gap 20mm～40mm, current density 4～8A/dm in the deposition process
2
After at first electrolytic solution configuration is finished, to stir evenly processing to solution usually, solution is placed on carry out ultrasonic stirring evenly 4 hours in the ultra-sonic generator, make nano particle full and uniform dispersion in the solution in solution.Open ultrasonic generator, utilize temperature control system that electroplate liquid is heated, open the positive negative pulse stuffing power supply then and plating piece is placed in the coating bath, then connection line, the galvanic deposit of beginning impulse ultrasound.
The 3rd step: the aftertreatment of plating piece mainly comprises ultrasonic cleaning, operations such as dehydrated alcohol cleaning.
The method of pulse of the present invention-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is simple, cost is low, the good mechanical properties of matrix material and have good magnetic properties, be particularly suitable for the various electron devices of working in the surface strengthening of mechanical component and the high-frequency alternating magnetic field environment with etc. the field.
Description of drawings
The present invention has two width of cloth accompanying drawings, wherein:
Fig. 1 is an experimental installation synoptic diagram of the present invention;
Fig. 2 is the current waveform figure that the present invention exports.
Among the figure: 1, negative electrode (sample) 2, anode (nickel plate) 3, power supply 4, plating bath 5, coating bath 6, supporting network 7, water 8, ultrasonic generator.
Embodiment
Specific embodiments of the invention as shown in drawings, the concrete implementation step of described pulse-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is:
1, exemplar is carried out mechanical pretreatment: with the sand paper corase grind, foreign matters such as the burr on removal exemplar surface, oxide compound reduce surfaceness.
2, exemplar is carried out pre-treatment: oil removing, rust cleaning, electropolishing and activation.Each component of solution of matrix being carried out oil removing is: sodium hydroxide 90g/l, sodium phosphate 60g/l, washing powder 4g/l, 60 ℃ of temperature, time 8min.
The deruster prescription: sulfuric acid 180g/l, hydrochloric acid 55g/l, OP emulsifying agent 4g/l, thiocarbamide 4g/l, sodium lauryl sulphate 0.04g/l, temperature are normal temperature, time 8min.
Electropolishing solution formula and processing parameter: phosphoric acid 72%, chromic acid 23%, water 5%, current density 60A/dm2,60 ℃ of temperature, time 6min.
Activation: carry out under the dilute hydrochloric acid with 10%, normal temperature, the time is 45s.
3, will put into electroplate liquid through the matrix of previous step pre-treatment and carry out galvanic deposit.Wherein the composition of electroplate liquid is: single nickel salt (NiSO
46H
2O) 250g/l, nickelous chloride (NiCl6H
2O) 50g/l, iron protochloride (FeCl
24H
2O) 20g/l, boric acid (H
3BO
3) 40g/l, asccharin 4g/l, nano particle 6g/l, sodium lauryl sulphate 0.2g/l.Control PH 3.2,60 ℃ of temperature, supporting electrode Ni plate, interpole gap 30mm, current density 8A/dm in the deposition process
2
The experimental installation that when galvanic deposit, adopts as shown in Figure 1, the experimental installation of being formed by negative electrode (sample) 1, anode (nickel plate) 2, power supply 3, plating bath 4, coating bath 5, supporting network 6, water 7, ultrasonic generator 8.The current waveform of the positive negative pulse stuffing power supply output of using as shown in Figure 2.Above-mentioned electroplate liquid is put into coating bath after ultrasonic agitation, matrix is after a series of pre-treatment processes such as rust cleaning, oil removing and activation then, and putting into coating bath carries out galvanic deposit, and its interpole gap is 30mm, and the startup temperature control system makes bath temperature be controlled at 60 ℃.The ultrasonic power that adopts is 300W, and the current parameters of employing has: pulse duty factor 30%, pulse-repetition 1000Hz, current density 8A/dm
2With electroplating time be 90min.The surfacing light of resulting ferromagnetic nano composite deposite, surfaceness is very little, and has premium propertiess such as very high microhardness and magnetic property.
Claims (7)
1. the method for pulse-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that matrix is inserted in the conventional plating tank through after the pre-treatment, is that coating bath applies electric field and ultrasonic field by the ultra-sonic generator and the pulse power; The process of impulse ultrasound galvanic deposit generally is made up of following steps:
The first step: pre-electroplating treatment: comprise a) the pre-treatment b of matrix) preparation of electroplate liquid;
Second step: electrodeposition process: the first step is put into the electroplate liquid that is configured through the matrix of pre-treatment carry out galvanic deposit;
The 3rd step: the aftertreatment of plating piece: comprise that mainly the plating piece that the second step deposition is finished carries out ultrasonic cleaning, the dehydrated alcohol matting.
2. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that described matrix pre-treatment is: matrix is carried out oil removing, rust cleaning, electropolishing and reactivation process successively.
3. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that described each component of solution that matrix is carried out oil removing is:
NaOH 80～100g/l
Na3PO4 50～60g/l
Washing powder 3～5g/l
Temperature 60～80
Time 5～10min
Deruster prescription: H2SO4 150～200g/l
HCl 50～60g/l
OP emulsifying agent 3～5g/l
Thiocarbamide 4g/l
Sodium lauryl sulphate 0.02～0.05g/l
Temperature (℃) normal temperature
Time 5～10min
Electropolishing solution formula and processing parameter:
H3PO4 72％
Chromic acid 23%
Water 5%
Current density 20～100A/dm2
Temperature (℃) 65～75
Time 3～5min
Activation: carry out under the dilute hydrochloric acid with 10%, normal temperature, the time is 30～60S.
4. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that consisting of of described electroplate liquid:
Single nickel salt (NiSO
46H
2O) 200g/l～350g/l
Nickelous chloride (NiCl
26H
2O) 40g/l～60g/l
Ferrous sulfate (FeSO
47H
2O) 10g/l～30g/l
Boric acid (H
3BO
3) 30g/l～50g/l
Asccharin 3g/l～5g/l
Nano particle 2g/l～8g/l
Sodium lauryl sulphate 0.1g/l～1g/l.
5. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material, it is characterized in that described nano particle is nano particles such as titanium nitride TiN, silicon carbide SiC, titanium carbide TiC, the particle diameter of nanoparticle is 20nm～100nm; The nano particle of selling on the market should be inserted and be cleaned in the container and dispersion treatment, and amount adds in the solution that will dispose in accordance with regulations then.
6. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that described positive negative pulse stuffing power supply and the ultra-sonic generator of using when galvanic deposit, the processing parameter that is adopted is:
(1) ultrasonic wave
Wave direction X, Y, X+Y
Power 0～360W
(2) pulsed current
Current density 4～8A/dm
2
Pulse width 0～200ms
Pulse interval 0～1000ms
Pulse duty factor 0.20～1
Pulse-repetition 5～5000Hz
The pulse waveform rectangle
(3) supporting electrode Ni plate
(4) interpole gap 20～40mm
(5)PH 2～4
(6) temperature is 50 ℃～70 ℃
(7) depositing time 30～90min.
7. the method for pulse according to claim 1-ultrasonic prepared by electrodeposition ferromagnetic nano matrix material is characterized in that described aftertreatment to sedimentary plating piece, mainly comprises ultrasonic cleaning, dehydrated alcohol matting.
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|---|---|---|---|
| CN 201010580000 CN102002748A (en) | 2010-12-09 | 2010-12-09 | Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition |
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|---|---|---|---|
| CN 201010580000 CN102002748A (en) | 2010-12-09 | 2010-12-09 | Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition |
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Family
ID=43810444
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|---|---|---|---|
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677137A (en) * | 2011-12-24 | 2012-09-19 | 河南科技大学 | Metal electrodeposition device |
| CN103205631A (en) * | 2012-01-16 | 2013-07-17 | 昆山允升吉光电科技有限公司 | A nickel-iron alloy material and a preparation method thereof |
| CN103977885A (en) * | 2014-04-14 | 2014-08-13 | 霍州煤电集团有限责任公司 | Coal dressing magnetic dense medium powder magnetism strengthening device |
| CN104046989A (en) * | 2014-06-06 | 2014-09-17 | 扬州虹扬科技发展有限公司 | Novel method for preprocessing electrotinned glue-filled product |
| CN104928729A (en) * | 2015-05-14 | 2015-09-23 | 大连大学 | Electrodeposition-laser remelting strengthening process of Ni-nanometer TiN composite layer on surface of nickel base superalloy |
| CN105780068A (en) * | 2014-12-16 | 2016-07-20 | 北京有色金属研究总院 | Single-pulse electrodeposition method for Ni-Fe alloy magnetic coatings |
| CN106702466A (en) * | 2017-03-10 | 2017-05-24 | 武汉科技大学 | High-magnetism high-silicon electrical steel and preparing method thereof |
| CN108286064A (en) * | 2018-01-30 | 2018-07-17 | 西南石油大学 | A kind of pulse electrodeposition Ni-W/B4C nano composite deposite preparation method |
| CN109331820A (en) * | 2018-10-29 | 2019-02-15 | 大连理工大学 | A kind of method that pulse electrodeposition prepares Pt base catalyst under ultrasound condition |
| CN110246685A (en) * | 2019-07-17 | 2019-09-17 | 徐靖才 | A kind of preparation method of samarium ferromagnetic phase |
| CN110512245A (en) * | 2019-09-19 | 2019-11-29 | 昆明理工大学 | A method of improving composite material corrosive nature |
| CN113215631A (en) * | 2021-05-08 | 2021-08-06 | 遵义智通金属表面技术处理有限公司 | Inner hole deposition technology for fine micropores with large depth-diameter ratio |
| CN114517326A (en) * | 2022-03-15 | 2022-05-20 | 大连大学 | Maskless localized micro electro-deposition additive manufacturing device and method based on ultrasound |
| CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
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|---|---|---|---|---|
| CN102677137B (en) * | 2011-12-24 | 2015-03-18 | 河南科技大学 | Metal electrodeposition device |
| CN102677137A (en) * | 2011-12-24 | 2012-09-19 | 河南科技大学 | Metal electrodeposition device |
| CN103205631A (en) * | 2012-01-16 | 2013-07-17 | 昆山允升吉光电科技有限公司 | A nickel-iron alloy material and a preparation method thereof |
| CN103977885A (en) * | 2014-04-14 | 2014-08-13 | 霍州煤电集团有限责任公司 | Coal dressing magnetic dense medium powder magnetism strengthening device |
| CN103977885B (en) * | 2014-04-14 | 2016-05-04 | 霍州煤电集团有限责任公司 | Coal separation magnetic dense media powder magnetic intensifying device |
| CN104046989A (en) * | 2014-06-06 | 2014-09-17 | 扬州虹扬科技发展有限公司 | Novel method for preprocessing electrotinned glue-filled product |
| CN105780068B (en) * | 2014-12-16 | 2018-02-02 | 北京有色金属研究总院 | The method of single pulse electrodpositing Ni Fe alloy magnetic coating |
| CN105780068A (en) * | 2014-12-16 | 2016-07-20 | 北京有色金属研究总院 | Single-pulse electrodeposition method for Ni-Fe alloy magnetic coatings |
| CN104928729A (en) * | 2015-05-14 | 2015-09-23 | 大连大学 | Electrodeposition-laser remelting strengthening process of Ni-nanometer TiN composite layer on surface of nickel base superalloy |
| CN106702466A (en) * | 2017-03-10 | 2017-05-24 | 武汉科技大学 | High-magnetism high-silicon electrical steel and preparing method thereof |
| CN108286064A (en) * | 2018-01-30 | 2018-07-17 | 西南石油大学 | A kind of pulse electrodeposition Ni-W/B4C nano composite deposite preparation method |
| CN109331820A (en) * | 2018-10-29 | 2019-02-15 | 大连理工大学 | A kind of method that pulse electrodeposition prepares Pt base catalyst under ultrasound condition |
| CN110246685A (en) * | 2019-07-17 | 2019-09-17 | 徐靖才 | A kind of preparation method of samarium ferromagnetic phase |
| CN110512245A (en) * | 2019-09-19 | 2019-11-29 | 昆明理工大学 | A method of improving composite material corrosive nature |
| CN113215631A (en) * | 2021-05-08 | 2021-08-06 | 遵义智通金属表面技术处理有限公司 | Inner hole deposition technology for fine micropores with large depth-diameter ratio |
| CN114517326A (en) * | 2022-03-15 | 2022-05-20 | 大连大学 | Maskless localized micro electro-deposition additive manufacturing device and method based on ultrasound |
| CN114517326B (en) * | 2022-03-15 | 2023-05-30 | 大连大学 | Maskless localized micro electro-deposition additive manufacturing device and method based on ultrasound |
| CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
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Application publication date: 20110406 |