CN107937946A - A kind of production method electroplated amorphous and prepare Fe Ni P powder - Google Patents
A kind of production method electroplated amorphous and prepare Fe Ni P powder Download PDFInfo
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- CN107937946A CN107937946A CN201711494734.XA CN201711494734A CN107937946A CN 107937946 A CN107937946 A CN 107937946A CN 201711494734 A CN201711494734 A CN 201711494734A CN 107937946 A CN107937946 A CN 107937946A
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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
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
Amorphous powdered alloy is made for plating+stripping+broken in a kind of production method of Co Fe Ni P powder, technological principle, it is characterised in that comprises the following steps：（1）Metal substrate selects and is plated the processing on surface；（2）Cobalt ferronickel phosphorus non-crystalline alloy coating is prepared using electro-plating method, anode uses graphite cake or stainless steel plate, and the current density of electrode is 0.05 0.5 A/mm2, titrating hydrochloric acid solution makes plating solution Ph values be less than 3, and plating temperature is 40 85 DEG C；（3）Amorphous alloy coating is set to come off from metallic substrate surfaces using the methods of rolling, bending, shot-peening；（4）The amorphous alloy coating to come off is crushed using modes such as ball mill, particle breakers；When broken, ball mill, particle breaker should use and force the type of cooling or interval work mode；（5）It is sieved into the Co Fe Ni P amorphous powdered alloys of different thicknesses.
Description
Technical field
The present invention relates to a kind of amorphous powdered alloy, more particularly, to a kind of life electroplated amorphous and prepare Fe-Ni-P powder
Production method.
Background technology
With the development of electron electric power, communication industry, electronic component is sent out to miniaturization, high frequency and high current direction
Exhibition, and the requirement to the Electro Magnetic Compatibility of electronic equipment is also higher and higher, traditional amorphous band iron core, soft magnet
Oxysome
And metal magnetic powder core etc. has been unable to meet demand.Common magnetic material performance deficiency is mainly manifested in：(1) amorphous band
Iron core inductive loop in high-frequency work causes loss very big, limits its application in high frequency field；(2) soft magnetic ferrite is high
Frequency is lost low, but saturation induction density and magnetic conductivity are low, it is impossible to meet the growth requirement of miniaturization and high current；(3) it is golden
Belong to powder core there is the problems such as high-frequency loss is high, DC superposition characteristic is poor or expensive, limit its application range.It is non-
Crystal structure has longrange disorder, the structure of shortrange order, powder is had many unique performances.Amorphous Magnaglo is due to it
Excellent soft magnet performance, can meet various electronic component stabilisations, miniaturization, high frequency, high current, high-power need
Ask, the development of the hi-tech industries such as automobile, electronics, aerospace field can be greatly facilitated.And cobalt base amorphous alloy powder removes
With excellent magnetic property, also with the performance such as high temperature resistant, resistance to exhaust gas corrosion, wear-resisting, anti-corrosion, closed in electronics, coating and hard
It is used widely in gold.
Up to the present, the preparation process of amorphous powdered alloy mainly has water fog method, aeroponics and using amorphous thin ribbon
The technique for crushing powder processed.Water fog method has big cooldown rate, can meet the requirement for preparing amorphous powder.However, in water mist
During change, the powder obtained easily forms oxide, and oxygen content is high, furthermore upon solidification of the molten metal, the vapor of generation
The surface of molten metal can be covered in, the presence of the vapor film reduces the core metal intensity of cooling for causing melting, so that
Prevent the problem of powder core is from obtaining amorphous structure, influence device performance.Aeroponics are since intensity of cooling is limited, only
The strong amorphous powdered alloy of amorphous formation ability can be prepared, and production cost is high.The advantages of direct crush method, is to material
Selectivity is not strong, and stock utilization is high, but brittle annealing need to be carried out to amorphous thin ribbon, it is easy to since annealing inequality causes strip
Internal crystallization change it is uneven, and the powder particle with acute angle is easily produced after broken, is the following process of powder
Bring difficulty.
And compared with liquisol quenching method, sputtering method prepare amorphous alloy material, galvanoplastic are more economical, and application range is also more
To be wide.The formation of Resisting Property of Brush Electroplating Coating plating of inherently making peace is identical, is all the metal ion in solution in anode（Workpiece）
The process of upper electric discharge crystallization.But compared with plating, plated pen and workpiece have relative motion in Brush Plating, thus plated surface is not
It is overall that metal ion reduction crystallization, the knot but plated surface each point sparks when plated pen is in contact with it occur at the same time
It is brilliant.Therefore, electroplating technology has its unique distinction in process aspect, its feature can be summarized as follows：
1st, equipment is simple, technique is simple, and operation is flexible；
2nd, expense is low, and economic benefit is big；
3rd, the controllable scope of powder metallurgy component ratio is big.
The content of the invention
In view of the above-mentioned problems, principle of the present invention based on plating amorphous, there is provided one kind plating amorphous prepares Fe-Ni-P powder
The production method at end.
The component of the Fe-Ni- P amorphous powders of the present invention is Fe 40-89 wt %, Ni 5-35 wt%, P 6-25
wt%；Its powder is amorphous structure.
The production method of Fe-Ni- P powder of the present invention.Comprise the following steps：
（1）Its elongation percentage is not less than 10% to the selection of metal substrate material at normal temperatures, is plated derusting, the ungrease treatment on surface；
（2）The composition of electroplate liquid：Soluble ferrite 1-4 mol/L（It is preferred that 1.5-2.5 mol/L）, soluble nickel salt 0.2-
1.2 mol/L, phosphorous acid or hypophosphites 0.1-0.6 mol/L, phosphoric acid 0.5-1.5 mol/L, additive 1-8g/L, solubility
Strong acid salt 10-50 g/L, reducing agent 2-5 g/L, excess water；
Above-mentioned additive is sodium citrate, lauryl sodium sulfate, neopelex；
Above-mentioned reducing agent is water-soluble；
（3）Fe-Ni- P non-crystalline coatings are prepared using electro-plating method, anode uses graphite cake or stainless steel plate, the electric current of electrode
Density is 0.05-0.5 A/mm2, titrating strong acid solution makes plating solution Ph values be less than 3, and plating temperature is 50-90 DEG C；
（4）Amorphous alloy coating is set to come off from metallic substrate surfaces using the methods of rolling, bending, shot-peening；
（5）Amorphous Alloy Grain crushes, and the amorphous alloy coating to come off is broken using modes such as ball mill, particle breakers
It is broken；When broken, ball mill, particle breaker should use and force the type of cooling or interval work mode, to prevent non-crystaline amorphous metal
Grain produces larger temperature rise, generation crystallization change when broken.
Compared with prior art, the present invention has the following advantages：
1. compared with aeroponics and direct crush method, this technique has that equipment investment is few, technique is simple, and energy is formed to non-crystaline amorphous metal
The features such as power is of less demanding；
2. compared with water fog method, the problem of powder will not produce oxidation and partial amorphization；
3. compared with direct crush method, due to depositing under the conditions of using pH value smaller, cause to generate larger planted agent in coating
Power and compared with concrete dynamic modulus, coating is i.e. tear-away with broken without brittle annealing, and will not produce the powder particle with acute angle；
4. compared with preparing galvanization coating, the present invention does not require coating stress and surface quality, therefore can use bigger
Current density, had both improved the preparation speed of amorphous alloy coating, was also beneficial to obtain more loose and with bigger internal stress
Amorphous alloy coating, so as to be more easy to peel off amorphous alloy coating and come off；
6. compared with chilling method prepares amorphous powdered alloy, the present invention need not consider the amorphous formation ability of material, can pass through tune
The concentration proportioning of whole each main component of electroplate liquid, can obtain the amorphous powdered alloy of different constituent elements compositions and ratio, therefore, we
The applicability of method is more extensive, and operability is stronger, can meet requirement of the different occasions to amorphous powdered alloy performance.
Embodiment
The invention will be further described with reference to embodiments.
The preparation of 1 Fe74Ni 18P8 amorphous powdered alloys of embodiment
Preparation process, comprises the following steps：
（1）The pretreatment of metallic substrate surfaces：Metal substrate selects 08F steel plates, and it is molten through sodium hydroxide respectively to be plated substrate surface
Liquid and hydrochloric acid solution cleaning, to remove grease and oxidation；
（2）Electroplate liquid forms：1.8 mol/L of frerrous chloride, 0.3 mol/L of phosphoric acid, 0.45 mol/L of nickel chloride, phosphorous acid
0.25mol/L, 1.5 g/L of additive, 15 g/L of soluble chlorine salt dissolving, 1.5 g/L of reducing agent, excess water；
Above-mentioned additive is sodium citrate and lauryl sodium sulfate mass ratio is 1:1 mixture；
Above-mentioned soluble chlorine salt dissolving is potassium chloride；
Above-mentioned reducing agent is ascorbic acid；
（3）The preparation of amorphous alloy coating：Pretreated metallic plate accesses cathode, and anode uses graphite cake, stirs electroplate liquid,
The current density of electrode is 0.05 A/mm2, plating temperature is 65 DEG C, and titration hydrochloric acid makes electroplate liquid Ph values be 1；
（4）Amorphous alloy coating is peeled off using bending method, bending radius is 0.2 m；
（5）Amorphous Alloy Grain crushes, and Amorphous Alloy Grain is crushed under argon gas protection using planetary ball mill, ball milling
2h, ratio of grinding media to material 5:1, ball milling method uses interval work mode, and for ball mill per ball milling 3min, rest 10min, avoids non-crystalline flour
End produces larger temperature rise.
The preparation of 2 Fe62 Ni of embodiment, 26 P12 amorphous powdered alloys
Preparation process, comprises the following steps：
（1）The pretreatment of metallic substrate surfaces：Metal substrate selects brass sheet, and thickness of slab 1mm, is plated substrate surface respectively through hydrogen
Sodium hydroxide solution and hydrochloric acid solution cleaning, to remove grease and oxidation；
（2）Electroplate liquid forms：1.8 mol/L of ferrous sulfate, 0.7 mol/L of phosphoric acid, 0.3 mol/L of nickel sulfate, sodium hypophosphite
0.3mol/L, additive 3g/L, 20 g/L of soluble sulphate, 3 g/L of reducing agent, excess water；
Above-mentioned additive is neopelex；
Above-mentioned soluble chlorine salt dissolving is sodium sulphate；
Above-mentioned reducing agent is potassium iodide；
（3）The preparation of amorphous alloy coating：Pretreated plating piece accesses cathode, and anode uses graphite cake, stirs electroplate liquid, electricity
The current density of pole is 0.1 A/mm2, plating temperature is 75 DEG C, and titration hydrochloric acid makes electroplate liquid Ph values be 2；
（4）Amorphous alloy coating is peeled off using rolling reductions method, rolling reduction ratio is 8%；
（5）Amorphous Alloy Grain crushes, and using planetary ball mill crusher machine, Amorphous Alloy Grain is broken in argon gas protection, ball milling
3h, ratio of grinding media to material 5:1, ball milling method uses interval work mode, and for ball mill per ball milling 3min, rest 10min, avoids non-crystalline flour
End produces larger temperature rise.
Claims (4)
1. a kind of production method electroplated amorphous and prepare Fe-Ni- P powder, it is characterised in that powdered ingredients are Co 53-82
Wt %, Fe 5-25 wt%, Ni 5-20 wt%, P 3-18 wt%；Powder is non crystalline structure.
2. amorphous powdered alloy is made for plating+stripping+broken in the production method technological principle of powder, it is characterised in that including
Following steps：
（1）Metal substrate selects and is plated the processing on surface；
（2）The composition of electroplate liquid：1.8 mol/L of frerrous chloride, 0.3 mol/L of phosphoric acid, 0.45 mol/L of nickel chloride, phosphorous acid
0.25mol/L, 1.5 g/L of additive, 15 g/L of soluble chlorine salt dissolving, 1.5 g/L of reducing agent, excess water；
（3）Co-Ni-Fe-phosphorus non-crystalline alloy coating is prepared using electro-plating method, anode uses graphite cake or stainless steel plate, electrode
Current density be 0.05-0.5 A/mm2, titrating hydrochloric acid solution makes plating solution Ph values be less than 3, and plating temperature is 50-90 DEG C；
（4）Amorphous alloy coating is set to come off from metallic substrate surfaces using the methods of rolling, bending, shot-peening；
（5）The amorphous alloy coating to come off is crushed using ball mill, particle breaker etc.；When broken, ball mill, particle are broken
Broken machine should be by the way of cooling or interval work be forced.
3. the additive described in claim 2 is sodium citrate, lauryl sodium sulfate, neopelex.
4. the reducing agent described in claim 2 is water-soluble.
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| CN106756641A (en) * | 2016-12-14 | 2017-05-31 | 刘志红 | A kind of Fe based amorphous alloy powders and its preparation technology |
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| CN106756641A (en) * | 2016-12-14 | 2017-05-31 | 刘志红 | A kind of Fe based amorphous alloy powders and its preparation technology |
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Application publication date: 20180420 |