CN108103539A - A kind of Ni-Fe-phosphorus amorphous powder production method - Google Patents

A kind of Ni-Fe-phosphorus amorphous powder production method Download PDF

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Publication number
CN108103539A
CN108103539A CN201711489727.0A CN201711489727A CN108103539A CN 108103539 A CN108103539 A CN 108103539A CN 201711489727 A CN201711489727 A CN 201711489727A CN 108103539 A CN108103539 A CN 108103539A
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amorphous
phosphorus
mol
alloy coating
crystalline alloy
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刘志红
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刘志红
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/002Making metallic powder or suspensions thereof amorphous or microcrystalline
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/04Amorphous alloys with nickel or cobalt as the major constituent
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/04Electroplating with moving electrodes
    • C25D5/06Brush or pad plating
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15341Preparation processes therefor

Abstract

A kind of ingredient of ferronickel phosphorus non-crystalline alloy powder is 40 90 wt% of nickel, and 5 35 wt% of iron, 5 25 wt% of phosphorus, powder is amorphous structure.Production method is it is characterised in that it includes following steps:(1)The elongation percentage of metal substrate at normal temperatures is not less than 10%, and substrate is plated the derusting on surface, ungrease treatment;(2)The preparation of ferronickel phosphorus non-crystalline alloy coating:Ferronickel phosphorus non-crystalline alloy coating is prepared using brush electroplating method, anode uses graphite cake or stainless steel plate, and the current density of electrode is 0.5 5 A/mm2(It is preferred that 1.5 3 A/mm2), electrode speed of related movement is 5 20 m/min(It is preferred that 10 15m/min), titrating hydrochloric acid or sulfuric acid solution makes plating solution Ph values be less than 3, and plating temperature is 40 85 DEG C;(3)Using the difference of substrate and amorphous deposit plastic deformation ability, using the methods of rolling, bending, shot-peening amorphous alloy coating is made to come off;(4)The amorphous alloy coating to come off is crushed using modes such as ball mill, particle breakers, and ball mill, particle breaker should use and force the type of cooling or interval work mode.This is simple for process, workable.

Description

A kind of Ni-Fe-phosphorus amorphous powder production method
Technical field
The present invention relates to a kind of amorphous powdered alloy, more particularly, to a kind of Ni-Fe-phosphorus non-crystalline alloy powder production side 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, and powder is made to have 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 It asks, 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 performances 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 as to Prevent the problem of powder central part 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 unevenness causes strip Internal crystallization change it is uneven, and the powder particle with acute angle is easily generated 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 cathode(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 whole that metal ion reduction crystallization, the knot but plated surface each point sparks when plated pen is in contact with it occur simultaneously It is brilliant.Therefore, Brush Electroplating Technique has its unique distinction in process aspect, and feature can be summarized as follows:
1st, equipment is simple, and coating bath is not required, easy to carry, suitable for field and field repair.Particularly with large-scale, precision equipment Scene without disintegrate, repair it is more with practical value;
2nd, simple for process, operation is flexible, and the position that need not be plated not use many material protections;
3rd, in operating process, cathode has relative motion with anode, therefore allows using higher current density, it is used than slot plating Current density is several times greater to tens times;
4th, metal ion content is high in plating solution, so plating product speed is fast(It is 5 times~10 times faster than slot plating);
5th, have a plated pen of different model, and equipped with shape is different, insoluble anode not of uniform size, to various different geometries and Complicated parts can all be repaired;
6th, expense is low, and economic benefit is big.
The content of the invention
In view of the above-mentioned problems, amorphous alloy powder is made the present invention is based on Brush Plating+stripping+broken, one kind is provided Ni-Fe-phosphorus non-crystalline alloy powder production method.
The ingredient of Ni-Fe-phosphorus non-crystalline alloy powder of the present invention is nickel 40-90 wt%, iron 5-35 wt%, phosphorus 5-25 wt%。
The production method of Ni-Fe of the present invention-phosphorus non-crystalline alloy powder.Comprise the following steps:
(1)Metal substrate selects and is plated the processing on surface:The elongation percentage at normal temperatures of metal substrate is not less than 10%, is plated Mechanically or chemically derusting, degreasing can be used in surface;
(2)The composition of electric brush plating liquor:Nickel chloride or nickel sulfate 3-7.5 mol/L(It is preferred that 4-6 mol/L), phosphoric acid 0.5-1.5 Mol/L, ferrous sulfate or frerrous chloride 0.5-3.5 mol/L, phosphorous acid or hypophosphites 0.2-2 mol/L, additive 1-8g/ L, soluble sulphate or chlorate 10-50 g/L, reducing agent 1-8g/L, excess water;
Above-mentioned additive is the mixture of tartaric acid, sodium acetate or both;
3 kinds of salt use homo-ion in above-mentioned electric brush plating liquor, that is, are soluble sulphate or chlorate;
Above-mentioned reducing agent is water-soluble;
(3)The preparation of Ni-Fe-phosphorus non-crystalline alloy coating:Ni-Fe-phosphorus non-crystalline alloy coating, anode are prepared using brush electroplating method Using graphite cake or stainless steel plate, the current density of electrode is 0.5-5 A/mm2(It is preferred that 1.5-3 A/mm2), electrode relative motion Speed is 5-20 m/min(It is preferred that 10-15m/min), titrating hydrochloric acid or sulfuric acid solution makes plating solution Ph values be less than 3, and plating temperature is 40-85℃;
(4)Using the difference of substrate and amorphous deposit plastic deformation ability, close amorphous using the methods of rolling, bending, shot-peening Gold plate comes off;
(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 generates larger Wen Sheng, generation crystallization change when broken;
(6)Ni-Fe-phosphorus non-crystalline alloy powder of different thicknesses is sieved into using sieve.
Compared with prior art, the present invention has the following advantages:
1. compared with aeroponics and direct crush method, this technique has equipment investment few, simple for process, and energy is formed to non-crystaline amorphous metal The features such as power is of less demanding;
2. compared with water fog method, powder will not lead to the problem of 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 embrittlement annealing, and will not generate the powder particle with acute angle;
4. compared with galvanoplastic+crush method prepares amorphous powdered alloy method, due to having relative motion between two electrode of Brush Plating, electroplate Liquid is also flow regime, therefore, does not electroplate the concentration polarization problem of generation, can use the current density of opposite bigger, carry The production efficiency of high powder;
5. for conventional brush plating, because not requiring coating stress and surface quality, therefore the electric current of bigger can be used Density had both improved the preparation speed of amorphous alloy coating, was also beneficial to obtain amorphous more loose and with bigger internal stress Alloy layer is removed so as to be more easy to carry out amorphous alloy coating rolling pressure;
6. this method can match somebody with somebody without considering the amorphous formation ability to material by adjusting the concentration of each main component of electroplate liquid Than the amorphous powdered alloy of different constituent elements compositions and ratio can be obtained, and therefore, the applicability of this method is more extensive, operable Property is stronger, can meet requirement of the different occasions to amorphous powdered alloy performance.
Specific embodiment
The invention will be further described with reference to embodiments.
The preparation of embodiment 1Ni71Fe17P12 amorphous powdered alloys
Its preparation process, comprises the following steps:
(1)The pretreatment of metallic substrate surfaces:Metal substrate selects 08F steel plates, thickness of slab 1mm, and plated substrate surface passes through respectively Sodium hydroxide solution and hydrochloric acid solution cleaning, to remove grease and oxidation;
(2)Electric brush plating liquor forms:5 mol/L of nickel chloride, 0.8 mol/L of phosphoric acid, 1.2 mol/L of frerrous chloride, phosphorous acid 0.8 Mol/L, additive 3g/L, 15 g/L of potassium chloride, 4 g/L of reducing agent, excess water;
Above-mentioned additive is tartaric acid;
Above-mentioned reducing agent is ascorbic acid;
(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 1.5 A/mm2, electrode speed of related movement is 5 m/min, and plating temperature is 65 DEG C, and titration hydrochloric acid makes Electroplate liquid Ph values are 2;
(4)Amorphous alloy coating is removed 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 4h, ratio of grinding media to material 3:1, ball milling method uses interval work mode, and ball mill avoids non-crystalline flour per ball milling 3min, rest 10min End generates larger Wen Sheng;
(6)The screening of amorphous powdered alloy.
The preparation of 2 Ni64Fe22P14 amorphous powdered alloys of embodiment
Its 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)Electric brush plating liquor forms:4.5 mol/L of nickel sulfate, 0.5 mol/L of phosphoric acid, 1.5 mol/L of ferrous sulfate, sodium hypophosphite 0.8 mol/L, additive 3g/L, 22 g/L of potassium sulfate, 3 g/L of reducing agent, excess water;
Above-mentioned additive is tartaric acid and sodium acetate mass ratio is 1:1 mixture;
Above-mentioned reducing agent is ascorbic acid;
(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 2 A/mm2, electrode speed of related movement is 10 m/min, and plating temperature is 65 DEG C, and titration hydrochloric acid makes electricity Plating solution Ph values are 1;
(4)Amorphous alloy coating is removed using alternating bending method, bending radius is 0.2 m;
(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 ball mill avoids non-crystalline flour per ball milling 3min, rest 10min End generates larger Wen Sheng;
(6)The screening of amorphous powdered alloy.
The preparation of 3 Ni68Fe21P11 amorphous powdered alloys of embodiment
Its 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)Electric brush plating liquor forms:4.5 mol/L of nickel sulfate, 0.5 mol/L of phosphoric acid, 1.2 mol/L of ferrous sulfate, phosphorous acid 0.7 Mol/L, additive 2g/L, 22 g/L of potassium sulfate, 3 g/L of reducing agent, excess water;
Above-mentioned additive is sodium acetate;
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 3 A/mm2, electrode speed of related movement is 15 m/min, and plating temperature is 80 DEG C, and titration hydrochloric acid makes electricity Plating solution Ph values are 1;
(4)Amorphous alloy coating is removed 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 2h, ratio of grinding media to material 10:1, ball milling method uses interval work mode, and ball mill avoids amorphous per ball milling 3min, rest 10min Powder generates larger Wen Sheng;
(6)The screening of amorphous powdered alloy.

Claims (5)

1. a kind of ingredient of Ni-Fe-phosphorus non-crystalline alloy powder is nickel 40-90 wt%, iron 5-35 wt%, phosphorus 5-25 wt%, powder For amorphous structure.
2. the production method of Ni-Fe-phosphorus non-crystalline alloy powder, which is characterized in that comprise the following steps:
(1)The elongation percentage of metal substrate at normal temperatures is not less than 10%, and substrate is plated the derusting on surface, ungrease treatment;
(2)The composition of electric brush plating liquor:Nickel chloride or nickel sulfate 3-7.5 mol/L(It is preferred that 4-6 mol/L), phosphoric acid 0.5-1.5 Mol/L, ferrous sulfate or frerrous chloride 0.5-3.5 mol/L, phosphorous acid or hypophosphites 0.2-2 mol/L, additive 1-8g/ L, soluble sulphate or chlorate 10-50 g/L, reducing agent 1-8g/L, excess water;
(3)The preparation of Ni-Fe-phosphorus non-crystalline alloy coating:Ni-Fe-phosphorus non-crystalline alloy coating, anode are prepared using brush electroplating method Using graphite cake or stainless steel plate, the current density of electrode is 0.5-5 A/mm2(It is preferred that 1.5-3 A/mm2), electrode relative motion Speed is 5-20 m/min(It is preferred that 10-15m/min), titrating hydrochloric acid or sulfuric acid solution makes plating solution Ph values be less than 3, and plating temperature is 40-85℃;
(4)Using the difference of substrate and amorphous deposit plastic deformation ability, close amorphous using the methods of rolling, bending, shot-peening Gold plate comes off;
(5)The amorphous alloy coating to come off is crushed using modes such as ball mill, particle breakers, ball mill, Particle Breakage Machine should use and force the type of cooling or interval work mode;
(6)Ni-Fe-phosphorus non-crystalline alloy powder of different thicknesses is sieved into using sieve.
3. the additive described in claim 2 is the mixture of tartaric acid, sodium acetate or both.
4. 3 kinds of salt described in claim 2 are homo-ion type, that is, it is soluble sulphate or chlorate.
5. the reducing agent described in claim 2 is water-soluble.
CN201711489727.0A 2017-12-29 2017-12-29 A kind of Ni-Fe-phosphorus amorphous powder production method Pending CN108103539A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108118265A (en) * 2017-12-31 2018-06-05 罗奕兵 A kind of technique of brush plating method production iron-phosphorus amorphous powder

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106381510A (en) * 2016-12-06 2017-02-08 刘志红 Preparing technology of Ni-Fe-P alloy-based compound coating
CN106756641A (en) * 2016-12-14 2017-05-31 刘志红 A kind of Fe based amorphous alloy powders and its preparation technology

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106381510A (en) * 2016-12-06 2017-02-08 刘志红 Preparing technology of Ni-Fe-P alloy-based compound coating
CN106756641A (en) * 2016-12-14 2017-05-31 刘志红 A kind of Fe based amorphous alloy powders and its preparation technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108118265A (en) * 2017-12-31 2018-06-05 罗奕兵 A kind of technique of brush plating method production iron-phosphorus amorphous powder

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Application publication date: 20180601