CN108145148A - A kind of production technology based on brush nickel plating alloy amorphous powder - Google Patents

A kind of production technology based on brush nickel plating alloy amorphous powder Download PDF

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Publication number
CN108145148A
CN108145148A CN201711464598.XA CN201711464598A CN108145148A CN 108145148 A CN108145148 A CN 108145148A CN 201711464598 A CN201711464598 A CN 201711464598A CN 108145148 A CN108145148 A CN 108145148A
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amorphous
nickel
powder
mol
plating
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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
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/0003Metallic powders per se; Mixtures of metallic powders; Metallic powders mixed with a lubricating or binding agent
    • 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

Abstract

A kind of ingredient based on brush nickel plating alloy amorphous powder is 40 82 wt% of nickel, and 8 30 wt% of cobalt, 5 15 wt% of iron, 5 15 wt% of phosphorus, powder is amorphous structure.Production technology it is characterized by comprising the following steps:(1)Metal substrate selects and is plated the derusting on surface, ungrease treatment;(2)The preparation of nickel alloy amorphous deposit:Nickel alloy amorphous deposit 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 75 DEG C;(3)Amorphous deposit is made to come off from metallic substrate surfaces using milling method;(4)The amorphous deposit to come off is crushed using modes such as ball mill, particle breakers;(5)The nickel alloy amorphous powder of different thicknesses is sieved into using sieve.

Description

A kind of production technology based on brush nickel plating alloy amorphous powder
Technical field
The present invention relates to a kind of amorphous powdered alloy, more particularly, to a kind of based on brush nickel plating alloy amorphous powder Production technology.
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 scope of application.It is non- Structure of the crystal structure with longrange disorder, shortrange order, makes powder 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 leading to 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 It is 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, does not need to coating bath, easy to carry, suitable for field and field repair.Particularly with large-scale, precision equipment Scene do not disintegrate repair it is more with practical value;
2nd, simple for process, operation is flexible, does not need to the position of plating and 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.
Invention content
In view of the above-mentioned problems, provide a kind of production technology based on brush nickel plating alloy amorphous powder.
The ingredient of the nickel alloy amorphous powder of the present invention is nickel 40-82 wt %, cobalt 8-30 wt%, iron 5-15 wt%, phosphorus 5-15 wt%。
The production technology of nickel alloy amorphous powder of the present invention.Include 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, cobaltous sulfate or cobalt chloride 0.4-2.5 mol/L, ferrous sulfate or frerrous chloride 0.3-2 mol/L, phosphorous acid 0.2-1.5 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 tartaric acid and the mixture of neopelex;
4 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 nickel alloy amorphous deposit:Nickel alloy amorphous deposit is prepared using brush electroplating method, anode 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 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 40-75 DEG C,;
(4)Amorphous deposit is made to come off from metallic substrate surfaces using milling method, rolling reduction ratio is 4-10%;
(5)The amorphous deposit to come off is crushed using modes such as ball mill, particle breakers.When broken, ball mill, particle are broken Broken machine should use and force the type of cooling or interval work mode, to prevent amorphous particle from generating larger Wen Sheng when broken, generation Crystallization change;
(6)The nickel alloy amorphous 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 produce 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, it is electroplated Liquid is also flow regime, therefore, the concentration polarization problem of generation is not electroplated, and 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, so as to be more easy to carry out amorphous alloy coating rolling pressure stripping;
6. this method can match 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 1 Ni 74Co12Fe7P7 amorphous powdered alloys of embodiment
Its preparation process, includes the following steps:
(1)The pretreatment of metallic substrate surfaces:Metal substrate selects 08F steel plates, plate thickness 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, 0.65 mol/L of cobalt chloride, frerrous chloride 0.5 Mol/L, 0.5 mol/L of phosphorous acid, additive 3g/L, 15 g/L of potassium chloride, 4 g/L of reducing agent, excess water;
Above-mentioned additive is tartaric acid and neopelex mass ratio is 2:1 mixture;
Above-mentioned reducing agent is ascorbic acid;
(4)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, plating temperature is 65 DEG C, and titration hydrochloric acid makes electroplate liquid Ph values be 2;
(5)Amorphous alloy coating is removed using rolling reductions method, rolling reduction ratio is 8%;
(6)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 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;
(7)It is sieved into the Ni74Co12Fe7P7 amorphous powdered alloys of different thicknesses.
The preparation of 2 Ni 61Co22Fe9P8 amorphous powdered alloys of embodiment
Its preparation process, includes the following steps:
(1)The pretreatment of metallic substrate surfaces:Metal substrate selects brass sheet, and plate thickness 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 cobaltous sulfate, ferrous sulfate 0.55mol/L, 0.5 mol/L of phosphorous acid, additive 3g/L, 22 g/L of potassium sulfate, 3 g/L of reducing agent, excess water;
Above-mentioned additive is tartaric acid and neopelex mass ratio is 1:1 mixture;
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 2 A/mm2, plating temperature is 65 DEG C, and titration hydrochloric acid makes electroplate liquid Ph values be 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 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)It is sieved into the Ni 61Co22Fe9P8 amorphous powdered alloys of different thicknesses.

Claims (5)

1. a kind of production technology based on brush nickel plating alloy amorphous powder, the ingredient of powder is nickel 40-82 wt %, cobalt 8- 30 wt%, iron 5-15 wt%, phosphorus 5-15 wt%, powder is amorphous structure.
2. the production technology of nickel alloy amorphous powder, which is characterized in that include 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, cobaltous sulfate or cobalt chloride 0.4-2.5 mol/L, ferrous sulfate or frerrous chloride 0.3-2 mol/L, phosphorous acid 0.2-1.5 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 nickel alloy amorphous deposit:Nickel alloy amorphous deposit is prepared using brush electroplating method, anode 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 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 40-75 DEG C,;
(4)Amorphous deposit is made to come off from metallic substrate surfaces using milling method, rolling reduction ratio is 4-10%;
(5)The amorphous deposit to come off is crushed using modes such as ball mill, particle breakers, and when crushing, ball mill, particle are broken Broken machine should use and force the type of cooling or interval work mode;
(6)The nickel alloy amorphous powder of different thicknesses is sieved into using sieve.
3. additive described in claim 2 is tartaric acid and the mixture of neopelex.
4. 4 kinds of salt use homo-ion in electric brush plating liquor described in claim 2, that is, it is soluble sulphate or chlorate.
5. reducing agent is water-soluble described in claim 2.
CN201711464598.XA 2017-12-28 2017-12-28 A kind of production technology based on brush nickel plating alloy amorphous powder Pending CN108145148A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100034687A1 (en) * 2005-12-28 2010-02-11 Zhichao Lu Compound magnetic powder and magnetic powder cores, and methods for making them thereof
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
CN106893953A (en) * 2017-03-21 2017-06-27 长沙理工大学 A kind of cobalt base amorphous alloy powder and production method
CN106893954A (en) * 2017-03-21 2017-06-27 长沙理工大学 A kind of Co based amorphous alloy powders and its preparation technology
CN107267892A (en) * 2017-06-19 2017-10-20 长沙理工大学 A kind of ni-based amorphous alloy catalysis electrode and production method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100034687A1 (en) * 2005-12-28 2010-02-11 Zhichao Lu Compound magnetic powder and magnetic powder cores, and methods for making them thereof
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
CN106893953A (en) * 2017-03-21 2017-06-27 长沙理工大学 A kind of cobalt base amorphous alloy powder and production method
CN106893954A (en) * 2017-03-21 2017-06-27 长沙理工大学 A kind of Co based amorphous alloy powders and its preparation technology
CN107267892A (en) * 2017-06-19 2017-10-20 长沙理工大学 A kind of ni-based amorphous alloy catalysis electrode and production method

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