CN104790000B - A kind of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid and preparation method thereof - Google Patents
A kind of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid and preparation method thereof Download PDFInfo
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- CN104790000B CN104790000B CN201410750588.2A CN201410750588A CN104790000B CN 104790000 B CN104790000 B CN 104790000B CN 201410750588 A CN201410750588 A CN 201410750588A CN 104790000 B CN104790000 B CN 104790000B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/24—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates from liquids
- H01F41/26—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates from liquids using electric currents, e.g. electroplating
Abstract
Manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid and preparation method thereof belongs to coat of metal electro-deposition preparation field.The manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of the present invention contains frerrous chloride, manganese chloride, bismuth chloride ingredient and suitable water;Boric acid, sodium hypophosphite, sodium citrate and ascorbic acid are also added in the formula;The parts by weight of each ingredient are in plating solution:35~45 parts of boric acid, 30~45 parts of sodium hypophosphite, 5~15 parts of frerrous chloride, 55~65 parts of manganese chloride, 4~10 parts of bismuth chloride, 35~45 parts of sodium citrate, 1~5 part of ascorbic acid.The present invention also provides the preparation methods of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, using workpiece to be electroplated as cathode, to be electroplated in this electroplate liquid using Pt pieces as anode, and the temperature of electroplate liquid is 20~40 DEG C, and voltage when plating is 2.0 ~ 5.0V.The electroplate liquid of the present invention has chemical stability height, of low cost, environment friendly and pollution-free.There is this preparation method simple controllable, obtained manganese bismuth iron phosphorus permanent-magnet alloy coating to have corrosion resistance strong, and magnetic property is good, is mainly used for the fields such as the surface finishing and magnetic material of miscellaneous hardware etc..
Description
Technical field
The present invention relates to manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquids and preparation method thereof, belong to coat of metal electro-deposition and prepare neck
Domain.
Background technology
Plating have it is of low cost, it is simple for process, it is easy to operate the advantages that, it we live in application it is very extensive,
Closely bound up with the various aspects of life, plating is one of most efficient method in process for treating surface.Past is mainly electroplated
Monometallic, far from meet modernization to surface property the needs of.Therefore, rapid hair of the plating alloy at nearly more than 20 years
Exhibition, it can not only obtain the surface of property, but also type is various, and application range is more extensive, has been applied at present
The industries such as magnetic material.MnBi alloys with magnetic performance just receive significant attention after being found from nineteen forty-three, each prosperity state
Family all gives very big support to the research of the material.MnBi alloys have good magneto-optical property at high temperature, can be used for magnetic
Light-memory medium, people are more in preparation method, magneto-optical property, alloying etc. to the MnBi alloy films by MnBi composition of alloy
The research that a aspect is concentrated.So far, scientist mainly uses vacuum vapour deposition and sputtering method to prepare MnBi
Alloy film, the MnBi alloy films obtained have good coercivity and a temperature characterisitic, but that there are equipment is complicated due to these methods,
It is expensive, of high cost, be not easy to mass produce, to limit its application.According to literature survey, so far, only B.
Benfedda seminars report one about successfully obtaining MnBi alloys using electro-deposition techniques and have studied its electro-deposition machine
Reason, then has not been reported.Therefore, it develops a kind of environmental type electrolyte and prepares the manganese bismuth iron phosphorus with magnetic performance with this
Permanent-magnet alloy coating is of great significance.Through retrieving Chinese patent, in relation to electroplate liquid in terms of invention it is very much, but without of the invention
The technology being related to.
Invention content
The present invention provides manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, which is free of corrosive goods
Matter, safety and environmental protection, chemical stability is high, and preparation process is simply controllable.The present invention also provides a kind of manganese bismuth iron phosphorus permanent-magnet alloy electricity
The preparation method of plating solution, has that preparation process is easy to operate, of low cost, corrosion resistance is strong, safety and environmental protection.The electroplate liquid is mainly used
In the surface finishing of miscellaneous hardware etc. and the manganese bismuth iron phosphorus permanent-magnet alloy of magnetic material.
The present invention particular technique content be:
A kind of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid should containing frerrous chloride, manganese chloride, bismuth chloride ingredient and suitable quantity of water
Also contain boric acid, sodium hypophosphite, sodium citrate and ascorbic acid in formula;The parts by weight of each ingredient therein are respectively:
35~45 parts of boric acid, 30~45 parts of sodium hypophosphite, 5~15 parts of frerrous chloride, 55~65 parts of manganese chloride, bismuth chloride 2~10
Part, 35~45 parts of sodium citrate, 1~5 part of ascorbic acid;It is formulated each component in the manganese bismuth iron phosphorus permanent-magnet alloy of preparation from the above mentioned
Mass percent be manganese 2%~27%, bismuth 3%~20%, iron 50%~75%, phosphorus 10%~21%.
The parts by weight of a kind of above-mentioned manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, optimum formula are 40 parts of boric acid, secondary Asia
40 parts of sodium phosphate, 12 parts of frerrous chloride, 60 parts of manganese chloride, 6 parts of bismuth chloride, 40 parts of sodium citrate, 3 parts of ascorbic acid and appropriate
Water;The mass percent of each component is in manganese bismuth iron phosphorus permanent-magnet alloy in the manganese bismuth iron phosphorus permanent-magnet alloy prepared by upper optimum formula
The mass percent of each component is manganese 15%, bismuth 20%, iron 50%, phosphorus 15%.
Another manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of the present invention, contains frerrous chloride, manganese chloride, bismuth chloride ingredient
And suitable quantity of water, it is characterised in that:Also contain boric acid, sodium hypophosphite, sodium citrate and ascorbic acid in the formula;It is therein each
The parts by weight of ingredient are respectively:38~42 parts of boric acid, 35~42 parts of sodium hypophosphite, 8~13 parts of frerrous chloride, manganese chloride
58~62 parts, 4~7 parts of bismuth chloride, 38~42 parts of sodium citrate, 2~4 parts of ascorbic acid.
The parts by weight of above-mentioned manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, one optimum formula are 40 parts of boric acid, secondary phosphorous
40 parts of sour sodium, 10 parts of frerrous chloride, 60 parts of manganese chloride, 6 parts of bismuth chloride, 40 parts of sodium citrate, 3 parts of ascorbic acid.
The present invention also provides a kind of preparation methods of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, are above-mentioned any one to prepare
The method of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid described in, including first boric acid is dissolved in the warm water of total volume 1/2, it stirs
When be added sodium hypophosphite, sodium citrate, obtain solution A after dissolving;The pH value for further including adjustment solution A is 2, is then added successively
Enter frerrous chloride, manganese chloride, bismuth chloride and ascorbic acid, and suitable water is added, electricity can be carried out after being sufficiently stirred 2 hours
Plating.
The preparation method of the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, using Pt pieces as anode, using workpiece to be electroplated as cathode,
The temperature being electroplated in electroplate liquid is 20~35 DEG C, and voltage when plating is 2.0~5.0V.The manganese bismuth iron phosphorus electroplate liquid
Optimum temperature be 28 DEG C.
Since temperature of electroplating solution raising can accelerate the movement velocity of particle in plating solution, to reduce the time of plating, but temperature
Height is spent, can make occur a large amount of bubble in plating solution, lead to the degradation of coating, it is described to make coating surface even uniform
Plating when manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid temperature be preferably also 25 DEG C~32 DEG C, manganese bismuth iron phosphorus permanent-magnet alloy electricity
The optimum temperature of the preparation method of plating solution, the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid is 28 DEG C.
Plating power supply used preferably uses DC power supply, be electroplated the thickness of manganese bismuth iron phosphorus permanent-magnet alloy coating obtained by
Electroplating time determines.
Compared with prior art, the present invention has technique effect beneficial below:
Manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of the present invention, due to the protection that need not ventilate, plating solution standing time is long, and chemistry is steady
Qualitative height;It is of low cost since without additive, selected material itself price, low, electroplating device is again simple;Plating solution
In be free of corrosive substance, it is environmentally friendly without discharge of steam during plating;Manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of the present invention
The manganese bismuth iron phosphorus permanent-magnet alloy coating surface that preparation method is obtained is more smooth, can be applied in actual production, and traditional
MnBi alloys membrane preparation method such as vacuum evaporation, sputtering method etc. is compared, and has unique advantage.Prepared manganese bismuth iron phosphorus permanent magnetism
Due to the content of phosphorus height in each component in alloy layer, which has strong corrosion resistance, while alloy stability is good, peace
Loopful is protected, and compared with traditional MnBi alloy films, performance is more superior;Meanwhile iron has very strong ferromagnetism, and have good
Plasticity and thermal conductivity, manganese bismuth alloy also have magnetic property.The manganese bismuth iron phosphorus permanent-magnet alloy prepared by the present invention is mainly used for day
With the surface finishing and magnetic material of hardware etc., future application will more extensively.
Description of the drawings
Fig. 1 is the electron spectrum of the manganese bismuth iron phosphorus permanent-magnet alloy coating of the present invention(EDS)Implementation illustration.
With reference to the accompanying drawings shown in 1, abscissa is ENERGY E nergy/keV, and ordinate is can spectral intensity Intensitv/a.u.;
The spectral peak of Mn, Bi, Fe, P and Cu are shown in figure.
Fig. 2 is the scanning electron microscope of the manganese bismuth iron phosphorus permanent-magnet alloy coating of Fig. 1(SEM)Figure.
Specific implementation mode
It is clear in order to make the purpose of the present invention, technical solution and advantageous effects be more clear, below in conjunction with attached drawing into
One step detailed description of the present invention technology contents and specific implementation mode.It should be understood that described in this specification specific
Embodiment is not intended to limit the present invention just for the sake of explaining the present invention.
Embodiment 1
40g boric acid is dissolved in the warm water of 0.5L, 40g sodium hypophosphites, 40g sodium citrates are sequentially added under stirring,
It is sufficiently stirred, obtains solution A after mixing;The pH value that solution A is adjusted with the HCl of 1.0mol/L is 2, under stiring, successively
10g frerrous chlorides, 60g manganese chlorides, 6g bismuth chlorides and 3g ascorbic acid is added, after being sufficiently stirred 2 hours, adds appropriate water-soluble to 1L
Obtain manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid.
Using Pt pieces as anode, using copper foil as cathode, it is electroplated in the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of above-mentioned acquisition,
Electroplating voltage is 3.0V, and the temperature of electroplate liquid is 28 DEG C, electroplating time 10 minutes, after plating, coating use successively ethyl alcohol and
Water cleans, and is dried up after cleaning up and obtains manganese bismuth iron phosphorus permanent-magnet alloy coating.
Manganese bismuth iron phosphorus permanent-magnet alloy coating manufactured in the present embodiment, scanning electron microscope(SEM)As shown in Fig. 1,
Superficial layer spheroidal, coating surface have a little crack, but whole still more smooth.Coating composition after tested, EDS results
(Fig. 2)It has been shown that, Cu are substrate peak, and after normalization, the mass percentage content of each component is in the alloy:Manganese is 15%, and bismuth is
20%, iron is 50% and phosphorus is 15%.Pass through vibrating specimen magnetometer(VSM)The magnetic property of manganese bismuth iron phosphorus permanent-magnet alloy is detected
Know that its coercivity is 520 Oe, there is preferable permanent magnetism performance.
Embodiment 2
35g boric acid is dissolved in the warm water of 0.5L, 45g sodium hypophosphites, 35g sodium citrates are sequentially added under stirring,
It is sufficiently stirred, obtains solution A after mixing;The pH value that solution A is adjusted with the HCl of 1.0mol/L is 2, under stiring, successively
5g frerrous chlorides, 55g manganese chlorides, 2g bismuth chlorides and 1g ascorbic acid is added adds suitable quantity of water to be settled to after being sufficiently stirred 2 hours
1L obtains manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid.
Using Pt pieces as anode, using copper foil as cathode, it is electroplated in the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of above-mentioned acquisition,
Electroplating voltage is 2.0V, and the temperature of electroplate liquid is 20 DEG C, electroplating time 15 minutes, after plating, coating use successively ethyl alcohol and
Water cleans, and is dried up after cleaning up and obtains manganese bismuth iron phosphorus permanent-magnet alloy coating.
Manganese bismuth iron phosphorus permanent-magnet alloy coating manufactured in the present embodiment is rougher, and crackle is smaller.Coating composition after tested, EDS
The results show that Cu is substrate peak, after normalization, the mass percentage content manganese of each component is 27% in the alloy, bismuth 7%, iron
It is 11% for 55 % and phosphorus.Pass through vibrating specimen magnetometer(VSM)It, which is rectified, is learnt to the magnetic property detection of manganese bismuth iron phosphorus permanent-magnet alloy
Stupid power is 360 Oe, shows permanent magnetism performance.
Embodiment 3
45g boric acid is dissolved in the warm water of 0.5L, 30g sodium hypophosphites, 42g sodium citrates are sequentially added under stirring,
It is sufficiently stirred, obtains solution A after mixing;The pH value that solution A is adjusted with the HCl of 1.0mol/L is 2, under stiring, successively
15g frerrous chlorides, 65g manganese chlorides, 10g bismuth chlorides and 5g ascorbic acid is added, after being sufficiently stirred 2 hours, adds suitable quantity of water constant volume
Manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid is obtained to 1L.
Using Pt pieces as anode, using copper foil as cathode, it is electroplated in the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of above-mentioned acquisition,
Electroplating voltage is 5.0V, and the temperature of electroplate liquid is 35 DEG C, electroplating time 20 minutes, after plating, coating use successively ethyl alcohol and
Water cleans, and is dried up after cleaning up and obtains manganese bismuth iron phosphorus permanent-magnet alloy coating.
Manganese bismuth iron phosphorus permanent-magnet alloy coating manufactured in the present embodiment, surface is more coarse, partly has and falls off.Coating after tested
Ingredient, EDS is the results show that Cu is substrate peak, and after normalization, the mass percentage content manganese of each component is 2% in the alloy, bismuth
It is 16%, iron is 61% and phosphorus is 21%.Pass through vibrating specimen magnetometer(VSM)Magnetic property detection to manganese bismuth iron phosphorus permanent-magnet alloy
It learns that its coercivity is 255 Oe, shows as permanent magnetism performance.
Embodiment 4
38g boric acid is dissolved in the warm water of 0.5L, 35g sodium hypophosphites, 45g sodium citrates are sequentially added under stirring,
It is sufficiently stirred, obtains solution A after mixing;The pH value that solution A is adjusted with the HCl of 1.0mol/L is 2, under stiring, successively
8g frerrous chlorides, 62g manganese chlorides, 4g bismuth chlorides and 2g ascorbic acid is added adds suitable quantity of water to be settled to after being sufficiently stirred 2 hours
1L obtains manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid.
Using Pt pieces as anode, using copper foil as cathode, it is electroplated in the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of above-mentioned acquisition,
Electroplating voltage is 4.0V, and the temperature of electroplate liquid is 30 DEG C, and electroplating time 5 minutes, after plating, coating uses second alcohol and water successively
Cleaning dries up after cleaning up and obtains manganese bismuth iron phosphorus permanent-magnet alloy coating.
Manganese bismuth iron phosphorus permanent-magnet alloy coating manufactured in the present embodiment, coating surface have a little crack.Coating composition after tested,
EDS is the results show that Cu is substrate peak, and after normalization, the mass percentage content manganese of each component is 12% in the alloy, bismuth 3%,
Iron is 75% and phosphorus is 10%.Pass through vibrating specimen magnetometer(VSM)It is learnt to the magnetic property detection of manganese bismuth iron phosphorus permanent-magnet alloy
Coercivity is 186 Oe, shows as permanent magnetism performance.
Embodiment 5
42g boric acid is dissolved in the warm water of 0.5L, 42g sodium hypophosphites, 38g sodium citrates are sequentially added under stirring,
It is sufficiently stirred, obtains solution A after mixing;The pH value that solution A is adjusted with the HCl of 1.0mol/L is 2, under stiring, successively
13g frerrous chlorides, 58g manganese chlorides, 7g bismuth chlorides and 4g ascorbic acid is added adds suitable quantity of water to be settled to after being sufficiently stirred 2 hours
1L obtains manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid.
Using Pt pieces as anode, using copper foil as cathode, it is electroplated in the manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid of above-mentioned acquisition,
Electroplating voltage is 3.0V, and the temperature of electroplate liquid is 32 DEG C, electroplating time 30 minutes, after plating, coating use successively ethyl alcohol and
Water cleans, and is dried up after cleaning up and obtains manganese bismuth iron phosphorus permanent-magnet alloy coating.
Manganese bismuth iron phosphorus permanent-magnet alloy coating manufactured in the present embodiment, surface has a little crack, structure smooth.Coating after tested
Ingredient, EDS is the results show that Cu is substrate peak, and after normalization, the mass percentage content manganese of each component is 16% in the alloy, bismuth
It is 18%, iron is 52% and phosphorus is 14%.Pass through vibrating specimen magnetometer(VSM)Magnetic property detection to manganese bismuth iron phosphorus permanent-magnet alloy
It learns that its coercivity is 455 Oe, shows as permanent magnetism performance.
The object of the invention and positive technique effect are realized by said program.
Claims (4)
1. a kind of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid, special containing frerrous chloride, manganese chloride, bismuth chloride ingredient and suitable quantity of water
Sign is:Also contain boric acid, sodium hypophosphite, sodium citrate and ascorbic acid in the formula;The parts by weight of each ingredient therein
Number is respectively:40 parts of boric acid, 40 parts of sodium hypophosphite, 10 parts of frerrous chloride, 60 parts of manganese chloride, 6 parts of bismuth chloride, sodium citrate 40
Part, 3 parts of ascorbic acid.
2. a kind of preparation method of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid according to claim 1, it is characterised in that:Including
First boric acid is dissolved in the warm water of total volume 1/2, sodium hypophosphite, sodium citrate are added when stirring, solution is obtained after dissolving
A;The pH value for further including adjustment solution A is 2, then sequentially adds frerrous chloride, manganese chloride, bismuth chloride and ascorbic acid, is added
Suitable water can be electroplated after being sufficiently stirred 2 hours.
3. a kind of preparation method of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid as claimed in claim 2, it is characterised in that:It is with Pt pieces
Anode, using workpiece to be electroplated as cathode, the temperature that is electroplated in electroplate liquid is 20~35 DEG C, and voltage when plating is 2.0
~5.0V.
4. the preparation method of manganese bismuth iron phosphorus permanent-magnet alloy electroplate liquid as claimed in claim 2, it is characterised in that:The manganese bismuth iron phosphorus
The optimum temperature of electroplate liquid is 28 DEG C.
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CN105951140B (en) * | 2016-06-08 | 2018-08-17 | 中国计量大学 | Rare earth-free manganese-based permanent magnet electroplating solution and preparation method thereof |
CN105951125B (en) * | 2016-06-08 | 2018-08-17 | 中国计量大学 | A kind of manganese base magnetism electroplate liquid and preparation method thereof |
CN105970257B (en) * | 2016-06-30 | 2018-12-25 | 中国计量大学 | A kind of iron-manganese-phosphorus magnetic alloy electroplate liquid and preparation method thereof |
CN109440149B (en) * | 2018-11-23 | 2021-06-08 | 云南师范大学 | Electroplating liquid composition and process for electroplating high-iron-low-tin alloy |
CN113241247A (en) * | 2021-05-10 | 2021-08-10 | 东莞市众旺永磁科技有限公司 | Manufacturing process of hollow magnetic product |
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