CN108203793A - A kind of Ni bases amorphous powder and preparation method - Google Patents
A kind of Ni bases amorphous powder and preparation method Download PDFInfo
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- CN108203793A CN108203793A CN201611169977.1A CN201611169977A CN108203793A CN 108203793 A CN108203793 A CN 108203793A CN 201611169977 A CN201611169977 A CN 201611169977A CN 108203793 A CN108203793 A CN 108203793A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/04—Electroplating with moving electrodes
- C25D5/06—Brush or pad plating
Abstract
A kind of base amorphous powder of Ni and its preparation process, powdered ingredients are 40 95 wt % of Ni, other alloying elements for can together with Ni electro-deposition element, such as a kind of or multielement combination in P, Fe, Cr, Co, Mo, W, Re.The preparation process of powder is：（1）Metal substrate is plated the pretreatment on surface：（2）The preparation of electroplate liquid；（3）The preparation of amorphous alloy coating：（4）The stripping of amorphous alloy coating；（5）The ball milling of Amorphous Alloy Grain；（6）The screening of amorphous powdered alloy.
Description
Technical field
The present invention relates to a kind of amorphous powdered alloy, more particularly, to a kind of Ni bases amorphous powder and preparation 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. is unable to meet demand, using being restricted.It is mainly manifested in：(1) amorphous band iron core is in high frequency
Work
When inductive loop cause loss it is very big, limit its application in high frequency field；(2) soft magnetic ferrite high-frequency loss is low, but
It is that saturation induction density and magnetic conductivity are low, it is impossible to meet the growth requirement of miniaturization and high current；(3) metal magnetic powder core is deposited
High-frequency loss is high, DC superposition characteristic difference or it is expensive the problems such as, limit its scope of application.Amorphous Magnaglo
Due to its excellent soft magnet performance, various electronic component stabilisations, miniaturization, high frequency, high current, high power can be met
Demand, the development of the hi-tech industries such as automobile, electronics, aerospace field can be greatly facilitated.
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.This rear two classes method is required for material to have stronger amorphous formation ability.
Invention content
Based on the above problem, the present invention provides a kind of Ni bases amorphous powders and preparation method thereof, and this method can be prepared
The wider array of Ni bases amorphous powder of composition and ratio range of choice of amorphous alloy material constituent element.
Ni bases amorphous/powder of the present invention, specific alloying component are Ni 40-95 wt %, and alloying element is can be with Ni
The element of electro-deposition together, such as in P, Fe, Cr, Co, Mo, W, Re one or more elements combination.
The preparation process of Ni based amorphous alloy powders of the present invention, includes the following steps：
（1）Nickel or nickel alloy wire or wire rod are chosen, chemistry or electrochemical method derusting, degreasing can be used in silk or wire surface；
（2）Winding displacement：In the same surface wiring of fixed frame, it is 0-5mm to make nickel wire or wire rod spacing distance；
（3）In winding displacement plane both sides Brush Plating amorphous deposit；
The electroplate liquid forms：Nickel salt（The mixture of nickel sulfate, nickel chloride or both）1-4mol/L（It is preferred that 2-3.5mol/
L）, acid 0.2-1mol/L, complexing agent 0.5-5g/L, alloying element additive 0.2-2mol/L, excess water；
In the upper alloying element additive, iron is with ferrous sulfate or frerrous chloride（Need to be furnished with reducing agent）, chromium with chromic anhydride, molybdenum with
Sodium molybdate, cobalt by cobaltous sulfate, tungsten adds by sodium tungstate, phosphorus by phosphorous acid or soluble hypophosphites, Re in the form of Re soluble salts
Add；
Above-mentioned acid includes boric acid, phosphoric acid, carboxylic acid etc.；
Above-mentioned complexing agent includes tartaric acid, neopelex, lauryl sodium sulfate, citrate etc.；
The technique of brush plating parameter is：Amorphous alloy coating is prepared using brush electroplating method, anode uses graphite, the electricity of electrode
Current density is 0.4-1.5A/mm2（It is preferred that 0.6-1 A/mm2）, electrode speed of related movement is 5-20m/min（It is preferred that 10-15m/
min）, titrating strong acid solution makes plating solution Ph values no more than 1, and plating temperature is 30-60 DEG C；
（4）The non-crystaline amorphous metal composite filament or wire rod plated using unlubricated drawing, drawing mould cross-sectional area is chooses nickel or nickel
The 80-95% of B alloy wire or wire rod cross-sectional area, drawing mould are disposed vertically, compound nickel wire or wire rod drawing from lower to upper, drawing
When mold generate vibration；
（5）The amorphous particle of peeling is carried out ball milling by the ball milling of Amorphous Alloy Grain under the conditions of vacuum or inert gas shielding,
Ball mill, planetary ball mill etc., Ball-milling Time 2-24h, ratio of grinding media to material 3-10 can be used in ball milling:1；
（6）It is sieved into the Ni base amorphous powders of different thicknesses.
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. for conventional 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 remove to amorphous alloy coating；
4. 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, and since nickel or nickel alloy wire are since plastic deformation ability is much larger than amorphous alloy coating, wire rod deformation
Greatly, non-crystaline amorphous metal deformation it is small, and due to using unlubricated drawing cause the additional tensile stress generated in amorphous alloy coating into
One step increases, this additional tensile stress, which will make to generate between amorphous alloy coating meeting and matrix, to be detached and be allowed to broken, is shortened and is prepared
The Ball-milling Time of amorphous powdered alloy, improves production efficiency；
5. this method can match without considering the amorphous formation ability to material by adjusting the concentration of each main component of electroplate liquid
Than differently composed and ratio amorphous powdered alloy can be obtained, and therefore, the applicability of this method is more extensive, and operability is more
By force, the performance requirement of different occasions can be met；
6. using the multi-thread method arranged in parallel of plane, thus board-like Brush Plating can be used and be electroplated in winding displacement plane both sides, carry
High production efficiency；
7. composite filament drawing from lower to upper, and the vibration of drawing mould, fall convenient for the amorphous alloy coating of peeling, not in mold
Import is assembled, and improves the collection efficiency of powder.
Specific embodiment
The invention will be further described with reference to embodiments.
The preparation of 1 Ni-P amorphous powdered alloys of embodiment
The 91.8wt% of the present embodiment amorphous powdered alloy Ni contents, P content are the 8.2wt% of composite deposite.
Its preparation process, includes the following steps：
（1）Selectionφ2mm nickel wires first using alkalilye degreasing, are removed by acid solution and are aoxidized as base material, silk material；
（2）Winding displacement：The spacing of nickel wire is 1mm；
（3）Electroplate liquid forms：Nickel sulfate 2.5mol/L, boric acid 0.5mol/L, tartaric acid 1.2g/L, phosphorous acid 0.4mol/L,
Excess water；
Technique of brush plating parameter is：Amorphous alloy coating is prepared using brush electroplating method, anode uses graphite cake, the electric current of electrode
Density is 0.6A/mm2, electrode speed of related movement is 10m/min, and titration strong acid solution makes plating solution Ph values be 1, and plating temperature is
50℃；
（4）Usingφ1.9mm drawing moulds, the composite filament that unlubricated drawing has been plated, the drawing from lower to upper of compound nickel wire, drawing speed
It spends for 0.1m/s, the vibration frequency 150Hz of drawing mould；
（5）The ball milling of Amorphous Alloy Grain, using planetary ball mill ball milling, amorphous powdered alloy argon filling gas shielded, ball milling 5h, ball
Material is than being 5:1；
（6）The screening of amorphous powdered alloy, using 200 mesh and 400 mesh sieve sub-sieves, wherein more than 200 mesh powder proportions
It is 39% for 42%, 200-400 mesh powder proportion, is 29% less than 400 mesh powder proportions.
The preparation of 2 Ni-Fe-P amorphous powdered alloys of embodiment
The preparation of the present embodiment Ni-Fe-P amorphous powdered alloys, powder Ni contents 79.2wt%, Fe content be 14.6wt%, P content
For 6.2wt%.
Its preparation process, includes the following steps：
（1）Selectionφ2mm nickel wires first using alkalilye degreasing, are removed by acid solution and are aoxidized as base material, silk material；
（2）Winding displacement：The spacing 2mm of nickel wire；
（3）Electroplate liquid forms：2. mol/L of nickel sulfate, ferrous sulfate 0.6mol/L, boric acid 0.4mol/L, tartaric acid 1g/L,
Phosphorous acid 0.3mol/L, potassium iodide 1g/L, excess water；
Technique of brush plating parameter is：Amorphous alloy coating is prepared using brush electroplating method, anode uses graphite cake, the electric current of electrode
Density is 0.8A/mm2, electrode speed of related movement is 10m/min, and titration strong acid solution makes plating solution Ph values be 0.5, plating temperature
It is 50 DEG C；
（4）Usingφ1.9mm drawing moulds, the composite filament that unlubricated drawing has been plated, compound nickel wire or wire rod drawing from lower to upper,
Drawing speed is 0.1m/s, the vibration frequency 150Hz of drawing mould；
（5）The ball milling of Amorphous Alloy Grain, using planetary ball mill ball milling, amorphous powdered alloy argon filling gas shielded ball milling 3h, ball
Material is than being 3:1；
（6）The screening of amorphous powdered alloy, using 200 mesh and 400 mesh sieve sub-sieves, wherein more than 200 mesh powder proportions
It is 33% for 42%, 200-400 mesh powder proportion, is 25% less than 400 mesh powder proportions.
Claims (2)
1. a kind of Ni bases amorphous powder and preparation method, which is characterized in that powder organization is amorphous/state, and ingredient is Ni 40-95
Wt %, other alloying elements for can together with Ni electro-deposition element, such as in P, Fe, Cr, Co, Mo, W, Re it is a kind of or more
The combination of kind element.
The preparation method of 2.Ni base amorphous powders, it is characterised in that：Include the following steps：
（1）Choose nickel or nickel alloy wire or wire rod derusting, degreasing；
（2）Winding displacement：
（3）In winding displacement plane both sides Brush Plating amorphous deposit；
The electroplate liquid forms：Nickel salt（The mixture of nickel sulfate, nickel chloride or both）1-4mol/L（It is preferred that 2-3.5mol/
L）, acid 0.2-1mol/L, complexing agent 0.5-5g/L, alloying element additive 0.2-2mol/L, excess water；
In the upper alloying element additive, iron is with ferrous sulfate or frerrous chloride（Need to be furnished with reducing agent）, chromium with chromic anhydride, molybdenum with
Sodium molybdate, cobalt by cobaltous sulfate, tungsten adds by sodium tungstate, phosphorus by phosphorous acid or soluble hypophosphites, Re in the form of Re soluble salts
Add；
Above-mentioned acid includes boric acid, phosphoric acid, carboxylic acid etc.；
Above-mentioned complexing agent includes tartaric acid, neopelex, lauryl sodium sulfate, citrate etc.；
The technique of brush plating parameter is：Amorphous alloy coating is prepared using brush electroplating method, anode uses graphite, the electricity of electrode
Current density is 0.4-1.5A/mm2（It is preferred that 0.6-1 A/mm2）, electrode speed of related movement is 5-20m/min（It is preferred that 10-15m/
min）, titrating strong acid solution makes plating solution Ph values no more than 1, and plating temperature is 30-60 DEG C；
（4）The amorphous composite filament or wire rod plated using unlubricated drawing, drawing mould cross-sectional area is chooses nickel or nickel alloy
The 80-95% of silk or wire rod cross-sectional area, drawing mould is disposed vertically, compound nickel wire or wire rod drawing from lower to upper, and when drawing makes
Mold generates vibration；
（5）The ball milling of Amorphous Alloy Grain；
（6）It is sieved into the Ni base amorphous powders of different thicknesses.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970819A (en) * | 2006-11-04 | 2007-05-30 | 燕山大学 | Binary NiP amorphous alloy bulk and method for preparing same |
| CN101532153A (en) * | 2009-03-13 | 2009-09-16 | 甘军 | Amorphous nano-alloy plating layer of electrodeposition nickel-based series, electroplating liquid and electroplating process |
| CN102703840A (en) * | 2012-05-25 | 2012-10-03 | 燕山大学 | Block ternary nickel-tungsten-phosphorus amorphous alloy and preparation method thereof |
| CN103060725A (en) * | 2013-01-22 | 2013-04-24 | 上海交通大学 | Nickel-base amorphous alloy powder as well as nickel-base amorphous composite coating and preparation method thereof |
| CN103469119A (en) * | 2013-08-15 | 2013-12-25 | 华南理工大学 | Amorphous composite materials, and preparation method and applications thereof |
| CN108193146A (en) * | 2016-12-08 | 2018-06-22 | 刘志红 | A kind of ni-based amorphous alloy powder and production method |
| CN108220825A (en) * | 2016-12-14 | 2018-06-29 | 刘志红 | A kind of Ni based amorphous alloy powders and its preparation process |
-
2016
- 2016-12-16 CN CN201611169977.1A patent/CN108203793A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970819A (en) * | 2006-11-04 | 2007-05-30 | 燕山大学 | Binary NiP amorphous alloy bulk and method for preparing same |
| CN101532153A (en) * | 2009-03-13 | 2009-09-16 | 甘军 | Amorphous nano-alloy plating layer of electrodeposition nickel-based series, electroplating liquid and electroplating process |
| CN102703840A (en) * | 2012-05-25 | 2012-10-03 | 燕山大学 | Block ternary nickel-tungsten-phosphorus amorphous alloy and preparation method thereof |
| CN103060725A (en) * | 2013-01-22 | 2013-04-24 | 上海交通大学 | Nickel-base amorphous alloy powder as well as nickel-base amorphous composite coating and preparation method thereof |
| CN103469119A (en) * | 2013-08-15 | 2013-12-25 | 华南理工大学 | Amorphous composite materials, and preparation method and applications thereof |
| CN108193146A (en) * | 2016-12-08 | 2018-06-22 | 刘志红 | A kind of ni-based amorphous alloy powder and production method |
| CN108220825A (en) * | 2016-12-14 | 2018-06-29 | 刘志红 | A kind of Ni based amorphous alloy powders and its preparation process |
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