CN106119817A - A kind of method of W fiber surface chemical deposition morphology controllable nickel dam - Google Patents

A kind of method of W fiber surface chemical deposition morphology controllable nickel dam Download PDF

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CN106119817A
CN106119817A CN201610488700.9A CN201610488700A CN106119817A CN 106119817 A CN106119817 A CN 106119817A CN 201610488700 A CN201610488700 A CN 201610488700A CN 106119817 A CN106119817 A CN 106119817A
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fiber
chemical deposition
nickel dam
distilled water
fiber surface
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CN106119817B (en
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梁淑华
原张晓
张乔
卓龙超
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Xian University of Technology
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Xian University of Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1635—Composition of the substrate
    • C23C18/1637—Composition of the substrate metallic substrate
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • 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
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
    • C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
    • C23C18/1837—Multistep pretreatment

Abstract

A kind of method that the invention discloses W fiber surface chemical deposition morphology controllable nickel dam, first by W fiber through surface clean and roughening treatment, it is then placed in the chemical sinking effusion added with activation nickel foil carrying out chemical deposition, is dried to obtain with deionized water and alcohol washes final vacuum the most successively.The method of W fiber surface chemical deposition morphology controllable nickel dam of the present invention uses activation nickel sheet to replace noble metal to activate W fiber, reduces production cost, selects CuSO simultaneously4As controlling agent, lactic acid as chelating agent, advantageously formed the nickel coating of various pattern by composition regulation and control.Therefore, the W fiber of the controlled nickel dam of surface chemistry deposition morphology, as a kind of reinforcement, can meet the demand of various types of materials strengthening, thus improve the various aspects of performance of material.

Description

A kind of method of W fiber surface chemical deposition morphology controllable nickel dam
Technical field
The invention belongs to material surface chemical treatment method field, be specifically related to a kind of W fiber surface chemical deposition pattern The method of controlled nickel dam.
Background technology
W fiber can also present good toughness because of it while ensureing higher-strength, thus is widely used as reinforcement Material, strengthens non-crystaline amorphous metal, high-temperature composite material and refractory metal material.But owing to its surface is oxidizable, at high temperature with Matrix material is difficult to be formed preferable interface fine structure, therefore need to be formed one layer on its surface had by chemical surface treatment The transition zone of activation, to improve the interfacial combined function of W fiber and matrix material.Nickel is as a kind of active element, generally It is added in tungsten-bast alloy and improves its activity, be considered as therefore a kind of potential material surface in field of material surface treatment Process active layer.Strengthen different matrix materials, the pattern of W fiber surface sedimentary be it is also proposed different requirements.Conventional Deposition requires smooth surface, but some special dimension requires that sedimentary presents different pattern (such as graininess, born of the same parents' shape, netted Deng), in order to meet these demands, need to propose a kind of simple possible, economical and practical surface treatment method, it is possible at W fiber Surface forms the nickel coating of morphology controllable.
Summary of the invention
A kind of method that it is an object of the invention to provide W fiber surface chemical deposition morphology controllable nickel dam, the method is fine at W The nickel dam morphology controllable of dimension table face deposition, it is possible to meet some special dimension requirement.
The technical solution adopted in the present invention is, a kind of method of W fiber surface chemical deposition morphology controllable nickel dam, first By W fiber through surface clean and roughening treatment, it is then placed in the chemical sinking effusion added with activation nickel foil carrying out chemical deposition, Finally it is dried with deionized water and alcohol washes final vacuum successively, obtains the W fiber of surface deposited nickel layer.
The feature of the present invention also resides in,
Surface process be by W fiber in the alkali wash water that pH value is 10～11 in 50～100 DEG C of saponifications 10～60min Oil removing and decontamination, then clean 3～5 times with deionized water ultrasonic vibration 30～60min.
Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP-10 emulsifying agent composition, wherein 1L Distilled water adds 5～20g Na respectively3PO4·12H2O, 20～40g Na2SiO3, 10～20g Na2CO3Granule and 1～5g OP-10 emulsifying agent.
Roughening treatment be the W fiber after surface is processed put in the HF acid of concentration 40% in 30～60 DEG C of roughening 15～ 45min, then cleans with deionized water.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Form with citric acid, wherein 1L distilled water adds 30 respectively ～60g NiSO4, 30～40g NaH2PO2With 20～40g citric acids.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2With lactic acid form, wherein 1L distilled water adds respectively 30～ 60g NiSO4, 30～40g NaH2PO2With 1～10g lactic acid.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2、CuSO4Form with lactic acid, wherein 1L distilled water adds respectively Add 30～60g NiSO4, 30～40g NaH2PO2, 1～10g CuSO4With 10～30g lactic acid.
Chemical deposition is chemical deposition 10～60min at 60～120 DEG C.
Clean and use deionized water and ethanol ultrasonic vibration 30～60min respectively to clean 3～5 times.
Vacuum drying is to be dried 2～8h at 50～100 DEG C.
The invention has the beneficial effects as follows, the method for W fiber surface chemical deposition morphology controllable nickel dam of the present invention, by W Fiber surface cleans, roughening treatment so that W fiber surface roughness increases, and selects CuSO subsequently4As controlling agent, lactic acid is made For chelating agent, activation nickel sheet replaces precious metal activation W fiber surface, deposits nickel by chemical deposition at W fiber surface, to obtain final product The nickel plating W fiber that surface topography is controlled.On the one hand the W fiber of chemical deposition nickel dam has the advantage of morphology controllable, wherein porous The nickel dam of structure is well combined with W fiber, without obscission, the most beneficially W fiber as during reinforcement with matrix material it Between interface cohesion；On the other hand, use activation nickel sheet to replace noble metal to activate W fiber, reduce production cost, select simultaneously Use CuSO4As controlling agent, lactic acid as chelating agent, advantageously formed the nickel coating of various pattern by composition regulation and control.Therefore, The W fiber of the controlled nickel dam of surface chemistry deposition morphology, as a kind of reinforcement, can meet the demand of various types of materials strengthening, thus Improve the various aspects of performance of material.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 obtains the SEM figure of smooth surface nickel dam in W fiber surface chemical deposition；
Fig. 2 is that the embodiment of the present invention 2 obtains the SEM figure of born of the same parents' shape nickel granule in W fiber surface chemical deposition；
Fig. 3 is that the embodiment of the present invention 3 obtains the SEM figure of loose structure nickel dam in W fiber surface chemical deposition.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
The method of W fiber surface chemical deposition morphology controllable nickel dam of the present invention, implements the most according to the following steps:
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 50～100 DEG C of saponifications 10～60min oil removing and go Dirt, then cleans 3～5 times with deionized water ultrasonic vibration 30～60min；Alkali wash water is by distilled water, Na3PO4·12H2O、 Na2SiO3、Na2CO3Granule and OP-10 emulsifying agent composition, wherein 1L distilled water adds 5～20g Na respectively3PO4·12H2O、20 ～40g Na2SiO3, 10～20g Na2CO3Granule and 1～5g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 15～45min in 30～60 DEG C, then use Deionized water cleans；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 10～60min at 60～120 DEG C, use deionized water and ethanol ultrasonic vibration 30～60min respectively to clean 3～5 It is vacuum dried 2～8h at 50～100 DEG C after secondary, obtains the W fiber of surface deposited nickel layer.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Form with citric acid, wherein 1L distilled water adds 30 respectively ～60g NiSO4, 30～40g NaH2PO2With 20～40g citric acids, deposition obtains the nickel plating W fiber that surface is smooth.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2With lactic acid form, wherein 1L distilled water adds respectively 30～ 60g NiSO4, 30～40g NaH2PO2With 1～10g lactic acid, deposition obtains the nickel plating W fiber that surface is born of the same parents' shape.
Chemical sinking effusion is by distilled water, NiSO4、NaH2PO2、CuSO4Form with lactic acid, wherein 1L distilled water adds respectively Add 30～60g NiSO4, 30～40g NaH2PO2, 1～10g CuSO4With 10～30g lactic acid, it is cellular that deposition obtains surface Nickel plating W fiber.
To the cleaning of W fiber surface, roughening treatment in the present invention so that W fiber surface roughness increases, and then utilizes chemistry Sedimentation when W fiber surface deposited nickel layer, the combination that beneficially nickel dam is good with W fiber, be not susceptible to obscission.
The present invention selects CuSO4As controlling agent, lactic acid, as chelating agent, is regulated and controled by solution composition, changes Ni2+With Cu2+Reduction potential, it is achieved the controlled preparation of deposited nickel layer pattern, can meet W fiber as during reinforcement material at all kinds of materials Application in material.
Embodiment 1
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 50 DEG C of saponification 30min oil removings and decontamination, then spend Ionized water ultrasonic vibration 30min cleans 3 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 10g Na respectively3PO4·12H2O、30g Na2SiO3、15g Na2CO3Granule and 2g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 15min in 30 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 10min at 60 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Forming with citric acid, wherein 1L steams Distilled water is added 30g NiSO respectively4、35g NaH2PO2With 30g citric acid, use deionized water and ethanol ultrasonic vibration respectively 30min is vacuum dried 2h at 50 DEG C after cleaning 3 times, obtains the nickel plating W fiber that surface is smooth.
Embodiment 2
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 50 DEG C of saponification 30min oil removings and decontamination, then spend Ionized water ultrasonic vibration 30min cleans 3 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 10g Na respectively3PO4·12H2O、30g Na2SiO3、15g Na2CO3Granule and 2g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 15min in 30 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 60min at 60 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Form with lactic acid, wherein 1L distillation Water adds 30g NiSO respectively4、35g NaH2PO2With 10g lactic acid, use deionized water and ethanol ultrasonic vibration 30min respectively It is vacuum dried 2h at 50 DEG C after cleaning 3 times, obtains the nickel plating W fiber that surface is born of the same parents' shape.
Embodiment 3
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 70 DEG C of saponification 30min oil removings and decontamination, then spend Ionized water ultrasonic vibration 30min cleans 3 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 10g Na respectively3PO4·12H2O、30g Na2SiO3、15g Na2CO3Granule and 2g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 15min in 30 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 40min at 90 DEG C, chemical sinking effusion is by distilled water, NiSO4、NaH2PO2、CuSO4Forming with lactic acid, wherein 1L steams Distilled water is added 37g NiSO respectively4、35g NaH2PO2、1g CuSO4With 20g lactic acid, deionized water and ethanol is used to surpass respectively Acoustic shock is swung after 30min cleans 3 times and is vacuum dried 2h at 50 DEG C, and obtaining surface is cavernous nickel plating W fiber.
Fig. 1～3 respectively embodiment of the present invention 1～3 obtains the SEM of different-shape nickel dam in W fiber surface chemical deposition Figure.It will be seen that relative to traditional chemical deposited nickel layer, chemical deposition of the present invention obtains W fiber surface nickel dam morphology controllable. By adding different chelating agent or controlling agent and adjusting each concentration of component in chemical sinking effusion, it is possible to achieve deposited nickel layer pattern Controlled preparation, the nickel dam of this morphology controllable be conducive to W fiber as during reinforcement surface activity raising and strengthen not With specific demand during material.
Embodiment 4
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 80 DEG C of saponification 60min oil removings and decontamination, then spend Ionized water ultrasonic vibration 45min cleans 5 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 20g Na respectively3PO4·12H2O、40g Na2SiO3、10g Na2CO3Granule and 5g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 30min in 60 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 30min at 90 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Forming with citric acid, wherein 1L steams Distilled water is added 60g NiSO respectively4、30g NaH2PO2With 20g citric acid, use deionized water and ethanol ultrasonic vibration respectively 60min is vacuum dried 5h at 100 DEG C after cleaning 4 times, obtains the nickel plating W fiber that surface is smooth.
Embodiment 5
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 100 DEG C of saponification 10min oil removings and decontamination, then use Deionized water ultrasonic vibration 60min cleans 4 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP-10 emulsifying agent forms, and wherein 1L distilled water adds 5g Na respectively3PO4·12H2O、20g Na2SiO3、20g Na2CO3Granule With 1g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 45min in 45 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 60min at 120 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Forming with citric acid, wherein 1L steams Distilled water is added 45g NiSO respectively4、40g NaH2PO2With 40g citric acid, use deionized water and ethanol ultrasonic vibration respectively 45min is vacuum dried 8h at 75 DEG C after cleaning 5 times, obtains the nickel plating W fiber that surface is smooth.
Embodiment 6
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 60 DEG C of saponification 50min oil removings and decontamination, then spend Ionized water ultrasonic vibration 40min cleans 5 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 15g Na respectively3PO4·12H2O、25g Na2SiO3、10g Na2CO3Granule and 3g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 30min in 40 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 40min at 80 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Form with lactic acid, wherein 1L distillation Water adds 40g NiSO respectively4、30g NaH2PO2With 5g lactic acid, use deionized water and ethanol ultrasonic vibration 50min respectively It is vacuum dried 6h at 60 DEG C after cleaning 3 times, obtains the nickel plating W fiber that surface is born of the same parents' shape.
Embodiment 7
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 70 DEG C of saponification 20min oil removings and decontamination, then spend Ionized water ultrasonic vibration 50min cleans 4 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 20g Na respectively3PO4·12H2O、35g Na2SiO3、15g Na2CO3Granule and 4g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 25min in 50 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 20min at 100 DEG C, wherein chemical sinking effusion is by distilled water, NiSO4、NaH2PO2Form with lactic acid, wherein 1L distillation Water adds 50g NiSO respectively4、40g NaH2PO2With 1g lactic acid, use deionized water and ethanol ultrasonic vibration 40min respectively It is vacuum dried 4h at 90 DEG C after cleaning 4 times, obtains the nickel plating W fiber that surface is born of the same parents' shape.
Embodiment 8
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 90 DEG C of saponification 40min oil removings and decontamination, then spend Ionized water ultrasonic vibration 40min cleans 4 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 15g Na respectively3PO4·12H2O、20g Na2SiO3、10g Na2CO3Granule and 3g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 20min in 35 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 50min at 70 DEG C, chemical sinking effusion is by distilled water, NiSO4、NaH2PO2、CuSO4Forming with lactic acid, wherein 1L steams Distilled water is added 45g NiSO respectively4、40g NaH2PO2、10g CuSO4With 10g lactic acid, use deionized water and ethanol respectively Ultrasonic vibration 35min is vacuum dried 7h at 80 DEG C after cleaning 4 times, and obtaining surface is cavernous nickel plating W fiber.
Embodiment 9
Step 1, W fiber surface cleans
By W fiber in the alkali wash water that pH value is 10～11 in 80 DEG C of saponification 60min oil removings and decontamination, then spend Ionized water ultrasonic vibration 60min cleans 5 times；Alkali wash water is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP- 10 emulsifying agent compositions, wherein 1L distilled water adds 20g Na respectively3PO4·12H2O、30g Na2SiO3、10g Na2CO3Granule and 5g OP-10 emulsifying agent；
Step 2, roughening treatment
W fiber after the process of surface is put in the HF acid of concentration 40% and be roughened 15min in 60 DEG C, then use deionized water Ultrasonic vibration 30min cleans 3 times；
Step 3, the W fiber after roughening put in the chemical sinking effusion (regulation pH value be 9～10) added with activation nickel foil Chemical deposition 50min at 60 DEG C, chemical sinking effusion is by distilled water, NiSO4、NaH2PO2、CuSO4Forming with lactic acid, wherein 1L steams Distilled water is added 60g NiSO respectively4、30g NaH2PO2、5g CuSO4With 30g lactic acid, deionized water and ethanol is used to surpass respectively Acoustic shock is swung after 50min cleans 5 times and is vacuum dried 8h at 90 DEG C, and obtaining surface is cavernous nickel plating W fiber.

Claims (10)

1. the method for a W fiber surface chemical deposition morphology controllable nickel dam, it is characterised in that first by W fiber through surface Clean and roughening treatment, be then placed in added with activation nickel foil chemical sinking effusion in carry out chemical deposition, spend the most successively from Sub-water and alcohol washes final vacuum are dried, and obtain the W fiber of surface deposited nickel layer.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that surface Process be by W fiber in the alkali wash water that pH value is 10～11 in 50～100 DEG C of saponifications 10～60min oil removing and decontamination, Then clean 3～5 times with deionized water ultrasonic vibration 30～60min.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 2, it is characterised in that alkali cleaning Liquid is by distilled water, Na3PO4·12H2O、Na2SiO3、Na2CO3Granule and OP-10 emulsifying agent composition, wherein 1L distilled water adds respectively Add 5～20g Na3PO4·12H2O, 20～40g Na2SiO3, 10～20g Na2CO3Granule and 1～5g OP-10 emulsifying agent.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that roughening Process is that the W fiber after being processed on surface is put in the HF acid of concentration 40% and is roughened 15～45min in 30～60 DEG C, then spends Ionized water cleans.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that chemistry Deposition liquid is by distilled water, NiSO4、NaH2PO2Form with citric acid, 1L distilled water wherein adds 30～60g NiSO respectively4、 30～40g NaH2PO2With 20～40g citric acids.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that chemistry Deposition liquid is by distilled water, NiSO4、NaH2PO2Form with lactic acid, 1L distilled water wherein adds 30～60g NiSO respectively4、30 ～40g NaH2PO2With 1～10g lactic acid.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that chemistry Deposition liquid is by distilled water, NiSO4、NaH2PO2、CuSO4Form with lactic acid, wherein 1L distilled water adds 30～60g respectively NiSO4, 30～40g NaH2PO2, 1～10g CuSO4With 10～30g lactic acid.
8., according to the method for the arbitrary described W fiber surface chemical deposition morphology controllable nickel dam of claim 5～7, its feature exists In, chemical deposition is chemical deposition 10～60min at 60～120 DEG C.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that clean Deionized water and ethanol ultrasonic vibration 30～60min respectively is used to clean 3～5 times.
The method of W fiber surface chemical deposition morphology controllable nickel dam the most according to claim 1, it is characterised in that vacuum Be dried is to be dried 2～8h at 50～100 DEG C.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973171A (en) * 2021-03-31 2021-06-18 西安建筑科技大学 Method for removing calcium and magnesium ions in sulfate solution by mineral wool induction
CN115161567A (en) * 2022-07-20 2022-10-11 内蒙古科技大学 Preparation method of interface control tungsten filament bundle reinforced copper-based composite material and composite material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215693A (en) * 2008-01-11 2008-07-09 江苏奈特纳米科技有限公司 Method for preparing high-performance conductive fiber
CN101285180A (en) * 2008-01-11 2008-10-15 西北工业大学 Process for preparing micro-coiled carbon fiber/Ni composite material by chemical nickel plating
CN101319325A (en) * 2008-07-03 2008-12-10 西北工业大学 Method of manufacturing fine helical nickel-carbon alloy material
CN101760734A (en) * 2010-02-01 2010-06-30 成都理工大学 Tin-nickel chemical plating prescription and process on surface of glass fiber
CN102086517A (en) * 2009-12-08 2011-06-08 沈阳临德陶瓷研发有限公司 Chemical nickel-plating method for carbon fiber

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215693A (en) * 2008-01-11 2008-07-09 江苏奈特纳米科技有限公司 Method for preparing high-performance conductive fiber
CN101285180A (en) * 2008-01-11 2008-10-15 西北工业大学 Process for preparing micro-coiled carbon fiber/Ni composite material by chemical nickel plating
CN101319325A (en) * 2008-07-03 2008-12-10 西北工业大学 Method of manufacturing fine helical nickel-carbon alloy material
CN102086517A (en) * 2009-12-08 2011-06-08 沈阳临德陶瓷研发有限公司 Chemical nickel-plating method for carbon fiber
CN101760734A (en) * 2010-02-01 2010-06-30 成都理工大学 Tin-nickel chemical plating prescription and process on surface of glass fiber

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973171A (en) * 2021-03-31 2021-06-18 西安建筑科技大学 Method for removing calcium and magnesium ions in sulfate solution by mineral wool induction
CN112973171B (en) * 2021-03-31 2023-02-21 西安建筑科技大学 Method for removing calcium and magnesium ions in sulfate solution by mineral wool induction
CN115161567A (en) * 2022-07-20 2022-10-11 内蒙古科技大学 Preparation method of interface control tungsten filament bundle reinforced copper-based composite material and composite material

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