CN109136891A - A kind of nickel-phosphor amorphous alloy composite fibre and preparation method - Google Patents
A kind of nickel-phosphor amorphous alloy composite fibre and preparation method Download PDFInfo
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- CN109136891A CN109136891A CN201710461047.1A CN201710461047A CN109136891A CN 109136891 A CN109136891 A CN 109136891A CN 201710461047 A CN201710461047 A CN 201710461047A CN 109136891 A CN109136891 A CN 109136891A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/22—Roughening, e.g. by etching
- C23C18/24—Roughening, e.g. by etching using acid aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/285—Sensitising or activating with tin based compound or composition
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
-
- 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 nickel-phosphor amorphous alloy composite fibre length can be continuous, and section is the shapes such as circle, abnormity, and the outer diameter of composite fibre is 0.01-0.2mm, and composite fibre core filaments diameter is 0.005-0.08mm;The clad of composite fibre is nickel-phosphor amorphous alloy, and specific ingredient is that Ni is 80-94%, and P 6-20%, the core filaments material of composite fibre is polymer.The step of preparation method are as follows: (1) use alkaline solution, oil removing degreasing is carried out to polymer fiber;(2) roughening of fiber surface is carried out using chromic anhydride and sulfuric acid solution;(3) sensitization of fiber is carried out using acid tin-salt solution;(4) activation of fiber surface is carried out using silver nitrate and ammonia spirit;(5) chemical plating nickel-phosphorus of fiber;(6) fiber brush nickel plating-phosphorus non-crystalline alloy.
Description
Technical field
The present invention relates to the production fields of metal composite fiber, more particularly, to a kind of compound fibre of nickel-phosphor amorphous alloy
Dimension and preparation method.
Background technique
The function of soft magnetic materials is mainly the conversion and transmission of magnetic conduction, electromagnetic energy.Currently, being applied to soft magnetic materials substantially
On can be divided into four classes: alloy thin band or thin slice;Amorphous alloy ribbon;Magnetic medium powder is coated and is bonded through electric insulating medium
Compression moulding as required afterwards;Ferrite.There is excellent soft magnetism with the amorphous alloy that transition metal (iron, cobalt, nickel) is matrix,
Saturation induction density height and A.C.power loss are low, can be widely applied to high and low frequency transformer and (partially close instead of silicon steel sheet and perm
Gold), Magnetic Sensor, write head, magnetic shielding material etc..With the rapid development of electronic engineering technology, advanced soft magnetic materials
Develop and develop a hot spot for being increasingly becoming the field.Use transition metal (iron, cobalt, nickel) for the amorphous powdered alloy of matrix
Or fiber prepares magnetic medium powder body material, is remarkably improved the soft magnet performance of device.
These methods can roughly be divided by the preparation method of amorphous alloy material according to the difference of material reset condition:
Liquid phase method, vapor phase method and solid phase method.The thought of liquid phase method is first to melt master alloy with uniformly, then uses the side of purification with rapid cooling
Formula makes aluminium alloy, and chilling shapes in a short time, and the major advantage of such method is to prepare that easy, the period is short, but prepared alloy
Size largely limited by alloy amorphous Forming ability.Such methods mainly have: water quenching, copper mold casting method,
High pressure diecasting method, suction casting method, casting die etc..Vapor phase method includes the methods of vacuum evaporation, sputtering, glow discharge and CVD, is obtained
It is film-form amorphous material.Such methods are suitable for preparationα- Ge andαThe compound amorphous state of the other four degree of coordinations of-Si is partly led
Body.Solid phase method includes thermally decomposing, neutron exposure, impact etc., such as prepares vitreous carbon using solid-bed break-up.Preparing film material
When material, it is easier to obtain amorphous structure.This is because method for manufacturing thin film can relatively easily cause to be formed it is non-
The external condition of crystal structure, i.e., higher degree of supercooling and low atom diffusivity.
The present invention is in view of the above problems, propose a kind of nickel-phosphor amorphous alloy composite fibre and preparation method thereof.This fiber can
It is widely used in magnetic medium powder, catalyst, radio-radar absorber etc..
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of nickel-phosphor amorphous alloy composite fibres, and composite fibre length can
Continuously, section is the shapes such as circle, abnormity, and the outer diameter of composite fibre is 0.01-0.2mm, and composite fibre core filaments diameter is
0.005-0.08mm;The clad of composite fibre is nickel-phosphor amorphous alloy, and specific ingredient is that Ni is 40-85%, Fe 10-
20%, P 6-20%, the core filaments material of composite fibre are polymer.
A kind of preparation method of nickel-phosphor amorphous alloy composite fibre, the technological process of production are as follows: polymer fiber is carried out
It is surface-treated (oil removing degreasing, roughening, sensitization, activation), the chemical plating nickel-phosphorus of polymer fiber, electronickelling-phosphorus non-crystalline alloy plating
Composite fibre is made in layer.
The present invention solves scheme used by its technical problem, specific steps are as follows:
(1) alkaline solution is used, oil removing degreasing is carried out to polymer fiber;
(2) roughening of fiber surface is carried out using chromic anhydride and sulfuric acid solution;Coarsening solution group becomes chromic anhydride 30-100g/L, 200-
400ml/L sulfuric acid:
(3) sensitization of fiber is carried out using acid tin-salt solution;Sensitizing solution group becomes stannic chloride 5-15g/L, hydrochloric acid 20-
50ml/L:
(4) activation of fiber surface is carried out using silver nitrate and ammonia spirit;
(5) chemical plating nickel-phosphorus of fiber, solution composition are as follows: nickel sulfate and nickel acetate 0.05-0.5mol/L, sodium hypophosphite 0.1-
0.5mol/L, complexing agent 0.2-1 mol/L, titration ammonia spirit Ph value are 8-10, and solution temperature is 15-40 DEG C when chemical plating,
Electroless plating time is 0.5-2min;
Above-mentioned complexing agent is citrate, tartaric acid;
(6) fiber brush nickel plating-phosphorus non-crystalline alloy,
Brush Plating solution composition: the preferred 2-3.5mol/L of soluble nickel salt 1-4.5mol/L(), acid 0.2-1mol/L, hypophosphorous acid
0.3-1.2mol/L, complexing agent 0.5-5g/L, excess water;
Above-mentioned acid includes the polynary middle strong acid such as boric acid, phosphoric acid, carboxylic acid;
Above-mentioned complexing agent includes tartaric acid, citrate, carboxylate etc.;
Preparation technology parameter are as follows: anode uses graphite plate, and the current density of electrode is 0.05-0.5A/mm2, brush plated fiber, electricity
Pole speed of related movement is the preferred 10-15m/min of 5-20m/min(), titration strong acid solution makes plating solution Ph value 1-3, plating temperature
It is 30-80 DEG C.
The invention has the advantages that
(1) polypropylene fibre for selecting different-diameter or odd-shaped cross section can prepare the continuous nickel-phosphor of different rule chromium and section configuration
Amorphous alloy covered composite yarn fiber;
(2) the nickel-phosphor composite fibre constituted with different proportion can be can get by adjusting the time of electroplating technology;
(3) compared with traditional preparation methods, the nickel-phosphor composite fibre of overlength can be prepared, fibre length is not by this process conditions
Limitation, is only dependent upon the length of original copolymer fiber;
(4) when preparing radio-radar absorber using complex structure of filament, be conducive to the weight of lightening material, and due to compound interface
Out-of-flatness caused by reflection and scattering, further enhance the absorbing property of composite material;
(5) composite fibre is wound in can back and forth on shelf and serves as liquid and gaseous reactive catalyst, both increased anti-
Answer area, in turn ensure the flowing of reactive material with exchange, catalytic efficiency can be greatly improved.
Specific embodiment:
The invention will be further described with reference to embodiments:
Embodiment 1: the forming technology of nickel-phosphor composite fibre
(1) it the surface treatment of fiber: usesφ0.01The polypropylene fibre of mm carries out electrochemical deoiling using sodium hydroxide solution
Degreasing;
(2) the aqueous solution proportion being roughened is 80g/L chromic anhydride, 300ml/L sulfuric acid, and roughening treatment temperature is 60 DEG C, roughening treatment
Time 20min;
(3) sensitization of fiber, sensitizing solution group become stannic chloride 8g/L, hydrochloric acid 40ml/L, sensitized treatment time 3min;
(4) activation of fiber surface is carried out using silver nitrate and ammonia spirit, the fiber after activation is restored through formalin;
(5) chemical plating of fiber, solution composition are as follows: nickel chloride 0.45mol/L, tartaric acid 0.3mol/L, hypophosphorous acid after handling
0.2mol/L, titration ammonia spirit Ph value are 8.5, and electroless plating time is 20 s;
(6) Brush Plating nickel-phosphor amorphous alloy
Electroplate liquid composition: 2.5 mol/L of nickel sulfate, boric acid 0.4mol/L, phosphorous acid 0.6mol/L, sodium citrate 1.2g/L, remaining
Measure water;
Preparation technology parameter are as follows: anode uses graphite plate, and the current density of electrode is 0.05A/mm2, brush plated fiber, electrode phase
It is 15m/min to movement velocity, titration strong acid solution makes plating solution Ph value 2, and plating temperature is 40 DEG C.
Embodiment 2: Ni-Fe-phosphorus composite fibre forming technology
(1) it the surface treatment of fiber: usesφ0.015The polypropylene fibre of mm carries out electrochemical deoiling using sodium hydroxide solution
Degreasing;
(2) the aqueous solution proportion being roughened is 65g/L chromic anhydride, 250ml/L sulfuric acid, and roughening treatment temperature is 60 DEG C, roughening treatment
Time 30min;
(3) sensitization of fiber, sensitizing solution group become stannic chloride 6.5g/L, hydrochloric acid 30ml/L, sensitized treatment time 2min;
(4) activation of fiber surface is carried out using silver nitrate and ammonia spirit, the fiber after activation is restored through formalin;
(5) chemical plating of fiber, solution composition are as follows: nickel sulfate 0.4mol/L, 0.35 mol/L of tartaric acid, hypophosphorous acid after handling
Sodium 0.3mol/L, titration ammonia spirit Ph value are 8.5, electroless plating time 0.5min;
(6) Brush Plating nickel-phosphor amorphous alloy
Electroplate liquid composition: nickel chloride 3mol/L, boric acid 0.5mol/L, sodium hypophosphite 0.7 mol/L, sodium citrate 1.2g/L, remaining
Measure water;
Preparation technology parameter are as follows: anode uses graphite plate, and the current density of electrode is 0.05A/mm2, brush plated fiber, electrode phase
It is 10m/min to movement velocity, titration strong acid solution makes plating solution Ph value 2, and plating temperature is 30 DEG C.
Claims (4)
1. a kind of nickel-phosphor amorphous alloy composite fibre, which is characterized in that fibre length can be continuous, and section is the shapes such as circle, abnormity
Shape, the outer diameter of composite fibre are 0.01-0.2mm, and composite fibre core filaments diameter is 0.005-0.08mm;The clad of composite fibre
For nickel-phosphor amorphous alloy, specific ingredient is that Ni is 80-94%, and P 6-20%, the core filaments material of composite fibre is polymer.
2. a kind of preparation method of nickel-phosphor amorphous alloy composite fibre, which is characterized in that production stage are as follows: (1) using alkalinity
Solution carries out oil removing degreasing to polymer fiber;(2) roughening of fiber surface is carried out using chromic anhydride and sulfuric acid solution;(3) it adopts
The sensitization of fiber is carried out with acid tin-salt solution;(4) activation of fiber surface is carried out using silver nitrate and ammonia spirit;(5)
The chemical plating nickel-phosphorus of fiber;(6) fiber brush nickel plating-phosphorus non-crystalline alloy.
3. described in claim 2, its plating solution of chemical plating nickel-phosphorus composition are as follows: nickel sulfate and nickel acetate 0.05-0.5mol/L, secondary phosphorus
Sour sodium 0.1-0.5mol/L, complexing agent 0.2-1 mol/L, titration ammonia spirit Ph value are 8-10, and solution temperature is when chemical plating
15-40 DEG C, electroless plating time 0.5-2min;
Above-mentioned complexing agent is citrate, tartaric acid.
4. described in claim 2, Brush Plating prepares nickel phosphorus non-crystal alloy layer, solution composition: soluble nickel salt 1-4.5mol/
The preferred 2-3.5mol/L of L(), acid 0.2-1mol/L, hypophosphorous acid 0.3-1.2mol/L, complexing agent 0.5-5g/L, excess water;
Above-mentioned acid includes the polynary middle strong acid such as boric acid, phosphoric acid, carboxylic acid;
Above-mentioned complexing agent includes tartaric acid, citrate, carboxylate etc.;
Its preparation technology parameter are as follows: anode uses graphite plate, and the current density of electrode is 0.05-0.5A/mm2, in routing planes two
Side brush plated fiber, electrode speed of related movement are the preferred 10-15m/min of 5-20m/min(), titration strong acid solution makes plating solution Ph
Value 1-3, plating temperature are 30-80 DEG C.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1546726A (en) * | 2003-12-09 | 2004-11-17 | 南开大学 | Method for chemical plating nickel phosphor alloy |
US20130243974A1 (en) * | 2012-03-15 | 2013-09-19 | Dh Holdings Co., Ltd. | Method of preparing nickel-coated nanocarbon |
CN104561951A (en) * | 2014-07-04 | 2015-04-29 | 广东丹邦科技有限公司 | Method and plating solution for chemical plating of nickel phosphorus alloy, and nickel phosphorus alloy layer |
CN105926012A (en) * | 2016-05-31 | 2016-09-07 | 长沙理工大学 | Preparation method for iron-nickel-copper oxysome long fiber pipe |
-
2017
- 2017-06-18 CN CN201710461047.1A patent/CN109136891A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1546726A (en) * | 2003-12-09 | 2004-11-17 | 南开大学 | Method for chemical plating nickel phosphor alloy |
US20130243974A1 (en) * | 2012-03-15 | 2013-09-19 | Dh Holdings Co., Ltd. | Method of preparing nickel-coated nanocarbon |
CN104561951A (en) * | 2014-07-04 | 2015-04-29 | 广东丹邦科技有限公司 | Method and plating solution for chemical plating of nickel phosphorus alloy, and nickel phosphorus alloy layer |
CN105926012A (en) * | 2016-05-31 | 2016-09-07 | 长沙理工大学 | Preparation method for iron-nickel-copper oxysome long fiber pipe |
Non-Patent Citations (2)
Title |
---|
崔玉顺等: "镍磷合金电刷镀工艺", 《腐蚀与防护》 * |
徐滨士等: "《材料表面工程技术》", 31 December 2014, 哈尔滨工业大学出版社 * |
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