CN105671529A - Preparation method for continuous fiber copper pipe - Google Patents
Preparation method for continuous fiber copper pipe Download PDFInfo
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- CN105671529A CN105671529A CN201610163247.4A CN201610163247A CN105671529A CN 105671529 A CN105671529 A CN 105671529A CN 201610163247 A CN201610163247 A CN 201610163247A CN 105671529 A CN105671529 A CN 105671529A
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- fiber
- copper
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Classifications
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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
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/062—Fibrous particles
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
- C23C18/18—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
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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
- C23C18/18—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
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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
- C23C18/18—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
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
-
- 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
- C23C28/023—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 only coatings of metal elements only
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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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
Abstract
The invention discloses a preparation method for preparing a continuous fiber copper pipe. According to the specific technical scheme, the preparation method comprises the steps that surface treatment of polypropylene continuous fibers is carried out; a sodium hydroxide solution is adopted for chemical oil removal, a chromic anhydride and sulfuric acid solution is used for surface roughening treatment, an acidic tin saline solution is used for fiber sensitization, a silver nitrate and ammonia water solution is used for fiber surface activation, and a formaldehyde solution is used for fiber reduction; then fiber chemical copper plating and fiber copper plating are carried out, and bivalent copper salt is adopted as main electroplating salt; the polypropylene fibers are removed under the oxidizing atmosphere; and the fiber copper pipe is obtained through reduction.
Description
Technical field
The present invention relates to functional metal fiber pipe preparing technical field, especially relate to the preparation method of a kind of macrofiber copper pipe.
Background technology
Steel fiber, compared with organic and inorganic fiber, has high elasticity, high wear resistance, good air permeability, electroconductibility, magnetic diffusivity, thermal conductivity and self lubricity and coking property, and range of application is wide, and prospect is noticeable. It is mainly used at present: clutch coupling, brake block friction material, conductive plastics, microwave protection clothes, high-voltage hot-line work clothes, automotive muffler, heat exchanger etc. And the steel fiber pipe with hollow structure is when using as radio-radar absorber, can show better electromagnetic wave attenuation effect and lower density. At present, the production method of steel fiber pipe mainly contains method of electrostatic spinning (Wang Meice etc., a kind of method [P] preparing metal nano fiber pipe based on single passage electrical spinning method, Chinese invention patent, application number: 201310525512.5,2013-10-30), and electrostatic spinning and metal gas phase precipitation technology combine method (Jin Yishui. the manufacture of high functionality metal nano fiber and Performance Evaluation thereof. external chemical fibre technology, 2011,40 (10), 47-49.). This type of method all cannot prepare continuity steel fiber pipe, and is difficult to make metal evenly be coated on fiber surface.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of macrofiber copper pipe, continuity polypropylene fibre surface treatment (alligatoring, activation, sensitization), change plating and plating are made continuity conjugated fibre, conjugated fibre through decomposition, cracking, burning, reduces and form macrofiber copper pipe.
The technical solution adopted for the present invention to solve the technical problems, comprises the following steps:
(1) surface treatment of polypropylene continuity fiber: adopt the sodium hydroxide solution of 10 ~ 20%wt to carry out electrochemical deoiling, chromium acid anhydride and sulphuric acid soln is adopted to carry out the alligatoring of fiber surface, acid tin-salt solution is adopted to carry out the sensitization of fiber, the cleaning of fiber after sensitization, adopting Silver Nitrate and ammonia soln to carry out the activation of fiber surface, the fiber after activation reduces through formaldehyde solution;
(2) electroless copper of fiber, its solution composition is: Seignette salt 10~20g/L, sodium hydroxide 2~5g/L, copper sulfate 2~4g/L, nickelous chloride, 0.2 ~ 1g/L, formaldehyde 1~3g/L, and the electroless plating time is 2-8min;
(3) fiber copper facing, electroplates main salt and adopts copper sulfate;
(4) removal of polypropylene fibre, conjugated fibre is oxidized 1-3h under 400~500 DEG C of oxidizing atmospheres;
(5) reduction of copper fiber pipe, under the protection of reducing atmosphere, 200~500 DEG C of insulation 0.2-1.5h, naturally cool to room temperature, obtain fiber copper pipe.
It is an advantage of the invention that:
(1) select the polypropylene fibre of different diameter or special crosssection, the continuity fiber copper pipe of different rule chromium and section form can be prepared;
(2) due to the decomposition of polypropylene fibre, cracking, burning not thorough, carbon residue has been retained in pipe, on the one hand for copper oxide is reduced into metal carrying for suitable reductive agent, improve speed of response, on the other hand, when fiber copper pipe uses as radio-radar absorber, the reflection of the interior carbon residue of pipe and sorption (XieW, ChengHF, ChuZYetal.EffectofFSSonmicrowaveabsorbingpropertiesofhollow-porouscarbonfibercomposites.MaterialsandDesign,2009,30(4):1201 1204.), the attenuating of hertzian wave will be strengthened;
(3) by the composition of the adjustment main salt of plating and the simple adjustment of technique, the continuity fiber pipe with different metal composition can be obtained;
(4) length of fiber copper pipe is not by process technology limit, only depends on the length of former polypropylene fibre.
Embodiment:
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:φ0.0The forming technology of 1mm fiber copper pipe
(1) polypropylene continuity Fibre diameter isφ0.006mm, first adopts 10%wt sodium hydroxide solution to carry out electrochemical deoiling 5min; The aqueous solution proportioning of alligatoring is 80g/L chromium acid anhydride, 300ml/L sulfuric acid, and roughening treatment temperature is 60 DEG C, roughening treatment time 20min; Sensitizing solution consists of tin chloride 8g/L, hydrochloric acid 40ml/L, sensitized treatment time 3min; Adopting Silver Nitrate and ammonia soln to carry out the activation of fiber surface, the fiber after activation reduces through formaldehyde solution;
(2) electroless copper of fiber, its solution composition is: Seignette salt 10g/L, sodium hydroxide 2.5g/L, copper sulfate 2g/L, nickelous chloride 0.2g/L, formaldehyde 1.2g/L, and the electroless plating time is 3min;
(3) fiber copper facing, electroplate liquid consists of, copper sulfate 120g/L, sulfuric acid 30ml/L, potassium aluminium sulfate 10g/L, electroplating time 20min;
(4) removal of polypropylene fibre, conjugated fibre is oxidized 1.5h under 450 DEG C of air atmospheres;
(5) reduction of copper fiber pipe, in a hydrogen atmosphere, 300 DEG C of insulation 0.5h, naturally cool to room temperature, obtainφ0.01mm continuity fiber copper pipe.
Claims (1)
1. prepare the preparation method of continuity fiber copper pipe for one kind, it is characterised in that, preparation process is:
(1) surface treatment of polypropylene continuity fiber: adopt the sodium hydroxide solution of 10 ~ 20%wt to carry out electrochemical deoiling, chromium acid anhydride and sulphuric acid soln is adopted to carry out the alligatoring of fiber surface, acid tin-salt solution is adopted to carry out the sensitization of fiber, the cleaning of fiber after sensitization, adopting Silver Nitrate and ammonia soln to carry out the activation of fiber surface, the fiber after activation reduces through formaldehyde solution;
(2) electroless copper of fiber, its solution composition is: Seignette salt 10~20g/L, sodium hydroxide 2~5g/L, copper sulfate 2~4g/L, nickelous chloride, 0.2 ~ 1g/L, formaldehyde 1~3g/L, and the electroless plating time is 2-8min;
(3) fiber copper facing;
(4) removal of polypropylene fibre, conjugated fibre is oxidized 1-3h under 400~500 DEG C of oxidizing atmospheres;
(5) reduction of copper fiber pipe, under the protection of reducing atmosphere, 200~500 DEG C of insulation 0.2-1.5h, naturally cool to room temperature, obtain fiber copper pipe.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201610163247.4A CN105671529A (en) | 2016-03-22 | 2016-03-22 | Preparation method for continuous fiber copper pipe |
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CN201610163247.4A CN105671529A (en) | 2016-03-22 | 2016-03-22 | Preparation method for continuous fiber copper pipe |
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CN105671529A true CN105671529A (en) | 2016-06-15 |
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CN201610163247.4A Pending CN105671529A (en) | 2016-03-22 | 2016-03-22 | Preparation method for continuous fiber copper pipe |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
CN109126656A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy catalytic reactor production method |
CN109136895A (en) * | 2017-06-18 | 2019-01-04 | 刘志红 | A kind of cobalt-nickel-phosphor magnetic coupling fiber and preparation method |
CN109930188A (en) * | 2019-01-31 | 2019-06-25 | 山东金宝电子股份有限公司 | A method of holey copper is prepared based on conductive fiber |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1306118A (en) * | 2001-02-27 | 2001-08-01 | 湘潭大学 | Process for preparing electrically conductive polyester fibres |
CN103805972A (en) * | 2014-01-17 | 2014-05-21 | 北京航空航天大学 | Ultra-light hollow pipe microarray metal material built by adopting template method and preparation method thereof |
-
2016
- 2016-03-22 CN CN201610163247.4A patent/CN105671529A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1306118A (en) * | 2001-02-27 | 2001-08-01 | 湘潭大学 | Process for preparing electrically conductive polyester fibres |
CN103805972A (en) * | 2014-01-17 | 2014-05-21 | 北京航空航天大学 | Ultra-light hollow pipe microarray metal material built by adopting template method and preparation method thereof |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109136895A (en) * | 2017-06-18 | 2019-01-04 | 刘志红 | A kind of cobalt-nickel-phosphor magnetic coupling fiber and preparation method |
CN109136889A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of cobalt-nickel-phosphor catalytic reactor and production method |
CN109126656A (en) * | 2017-06-27 | 2019-01-04 | 罗奕兵 | A kind of Ni-Fe-phosphorus non-crystalline alloy catalytic reactor production method |
CN109930188A (en) * | 2019-01-31 | 2019-06-25 | 山东金宝电子股份有限公司 | A method of holey copper is prepared based on conductive fiber |
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