CN108439457A - A kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material - Google Patents

A kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material Download PDF

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CN108439457A
CN108439457A CN201810393069.3A CN201810393069A CN108439457A CN 108439457 A CN108439457 A CN 108439457A CN 201810393069 A CN201810393069 A CN 201810393069A CN 108439457 A CN108439457 A CN 108439457A
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carbon cloth
solution
hydro
zinc oxide
friction material
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CN108439457B (en
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费杰
张立洁
黄剑锋
段笑
屈蒙
谷岳峰
罗丹
张超
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Shaanxi University of Science and Technology
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/02—Oxides; Hydroxides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
    • D06M15/41—Phenol-aldehyde or phenol-ketone resins
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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  • Textile Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a kind of methods that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material, EtOH Sonicate processing carbon cloth is used to remove its surface impurity first, then carbon cloth is cleaned with acetone using soxhlet extraction, remove its surface organic matter and sizing agent, further use diene synthesis in the lossless grafting oxygen-containing functional group of carbon cloth surfaces, then one layer of zinc oxide crystal seed layer is inoculated in carbon cloth surfaces, using hydro-thermal electrophoresis in carbon cloth surfaces homoepitaxial ZnO nanorod, it is last hot-forming to the phenol resin solution that carbon cloth vacuum impregnation after processing is modified.Present invention fast-growth zinc oxide nano rod on carbon cloth using the method for hydro-thermal electrophoresis builds multi-scale reinforcing body to improve the performance of friction material.

Description

A kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material
Technical field
The invention belongs to friction material fields, and in particular to a kind of hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth and rubs The method for wiping material.
Background technology
As high tech equipment, rail traffic and vehicle develop to high-speed overload direction, to the peace of wet type biography/braking system Full property and stability propose harsh requirement.As an important component in wet type biography/braking system, Wet-type friction material It is main to play a part of generating torque, transmit load, directly determine the safety and stability of biography/braking system.Carbon cloth increases Strong resin-matrix friction material is widely used in work because of its low-density, Gao Biqiang, the excellent properties such as antifatigue, designability is strong In journey friction material.However, carbon fiber is poor with resin infiltration, interface resin unsticking seriously constrains the friction of such material Stability and service life.Based on this, processing is modified to carbon cloth fiber surface, enhances its interface cohesion with resin matrix Intensity further expands its application in friction field.
The present invention, in carbon cloth surfaces growing ZnO nanorod, forms abundant network branches structure using hydro-thermal electrophoretic techniques, Improve the performance perpendicular to fiber axial direction.The advantages of this process set hydrothermal growth process and electrochemical deposition method, growth temperature It spends low, rapidly and efficiently, can get pattern is uniform, draw ratio is moderate ZnO nanorod, new think of is provided to construct multi-scale reinforcing body Road.
A kind of Chinese patent " carbon fiber sheet friction for wet clutch of 1 Publication No. CN102343679A of document Material preparation method and application " discloses a kind of applied to wet clutch, the friction and wear behavior of raising wet type carbon fiber sheet Method, the friction material of gained in the case where its is thinning, still have good wear resistance.However it is prepared The complex process of friction material, equipment requirement is high, needs to prepare under high temperature and certain pressure condition.And hydro-thermal electrophoresis In carbon fiber surface growing zinc oxide nanorod, the chemical bonding between fiber and resin and mechanical engagement not only may be implemented, Enhance the friction and wear behavior of friction material.And it is simple for process, growth temperature is low, and equipment requirement is low.2 Publication No. of document The Chinese patent " preparation method of growing zinc oxide nanorod reinforced resin base frication material on carbon cloth " of CN106147117A, Disclose it is a kind of using immersion method in the method for carbon cloth surfaces growing zinc oxide nanorod, friction material is enhanced by developing zinc oxide The friction and wear behavior of material.However growth period is long, zinc oxide is unevenly distributed on carbon fiber, sparse.
Invention content
The purpose of the present invention is to provide the sides that a kind of hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material Method, to overcome the problems of the above-mentioned prior art, present invention fast-growth oxygen on carbon cloth using the method for hydro-thermal electrophoresis Change zinc nanometer rods, builds multi-scale reinforcing body to improve the performance of friction material.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material, includes the following steps：
Step 1：After handling carbon cloth with EtOH Sonicate, carbon cloth is cleaned；
Step 2：It is lossless using the carbon cloth surfaces of diene synthesis after cleaning using methacrylic acid as grafted monomers It is grafted oxygen-containing functional group；
Step 3：Zinc acetate dihydrate and sodium hydroxide are dissolved in ethanol solution respectively, stirs evenly and respectively obtains two water Zinc acetate solution and sodium hydroxide solution, are denoted as solution B and solution C respectively, and into solution B, addition ethanol solution dilutes to obtain molten Liquid D, into solution C, addition ethanol solution dilutes to obtain solution E, and E solution is added drop-wise to after stirring is stood in solution D and obtains zinc source Seed layer colloidal sol；
Step 4：The carbon cloth that step 2 obtains is impregnated in the seed layer colloidal sol of zinc source, is then dried, repeated impregnations and baking After doing several times, the carbon cloth that seed layer is contained on surface is obtained；
Step 5：By zinc source and alkali source with 1：1 molar ratio mixing is added in ultra-pure water, obtains growth-promoting media；
Step 6：The carbon cloth that seed layer is contained on surface is placed in growth-promoting media, is given birth in carbon cloth surfaces using hydro-thermal electrophoresis Long ZnO nanorod；
Step 7：The carbon cloth surfaces obtained in step 6 using vacuum pressure impregnating method impregnate phenol-formaldehyde resin modified, then It is dry, it is finally hot-forming to obtain zinc oxide nano rod/carbon cloth friction material.
Further, cleaning is specially in step 1：Carbon cloth after supersound process deionized water is rinsed 3-5 times, is connect It and extracts the carbon cloth after flushing 2-3 hours at 60-80 DEG C using soxhlet extraction acetone soln, then rinsed with deionized water 10min。
Further, zinc acetate dihydrate and sodium hydroxide are dissolved in ethanol solution respectively in step 3, are stirred evenly point Do not obtain that molar concentration is 0.0125mol/L acetate dihydrates zinc solution and molar concentration is 0.025mol/L sodium hydroxide solutions, It is denoted as solution B and solution C respectively, ethanol solution is added into solution B and dilutes to obtain the solution D of a concentration of 0.0014mol/L, to Ethanol solution is added in solution C to dilute to obtain the solution E of a concentration of 0.0071mol/L.
Further, dip time is 15-30min in step 4, and drying temperature is 100-150 DEG C, repeated impregnations and baking It is 3-5 times dry.
Further, zinc source is zinc nitrate hexahydrate in step 5；Alkali source is hexa, ammonium fluoride or chlorination Ammonium.
Further, the molar concentration in zinc source is 0.025mol/L in the growth-promoting media that step 5 obtains.
Further, anode is made with graphite cake when hydro-thermal electrophoresis in step 6, carbon cloth makees cathode, electrophoresis time 15- 60min, electrophoretic current 0.15-0.2A, voltage 0.3-0.35V.
Further, the mass fraction that post-modification phenolic resin is impregnated in step 7 is 30-40%.
Further, drying temperature is room temperature in step 7, and drying time is 24 hours.
Compared with prior art, the present invention has technique effect beneficial below：
Present invention fast-growth zinc oxide nano rod on carbon cloth using the method for hydro-thermal electrophoresis, builds multi-scale enhancement Body improves the performance of friction material.It uses methacrylic acid to carry out activation process to carbon cloth first, carbon cloth surfaces is made not damage Increase active function groups in the case of hindering fibre strength, and simple for process, it is low for equipment requirements the features such as, secondly in carbon cloth surfaces It is inoculated with one layer of zinc oxide crystal seed layer, is later stage surface to provide buffer transition layer in carbon cloth surfaces growing zinc oxide nanorod Developing zinc oxide is laid a good foundation, while also enhancing the Interface Adhesion between carbon cloth and resin, then in carbon cloth table just growth of oxygen Change zinc nanometer rods, form nanometer pinning layer, gives full play to each layer, form the gradient transition of the Nomenclature Composition and Structure of Complexes between two layers, ensure The high strength bond of pinning layer and buffer layer gives full play to the synergistic effect of each layer chemical bonding and mechanical engagement, synchronizes and carry Rise the intensity, toughness and friction stability of composite material.
Description of the drawings
Fig. 1 is the schematic diagram using hydro-thermal electrophoresis growing zinc oxide nanorod in carbon cloth surfaces growth；
Fig. 2 is unmodified carbon fiber and hydro-thermal electrophoresis growing zinc oxide nanorod/carbon cloth SEM photograph comparison diagram, wherein (a) It is (b) microscopic appearance of growing zinc oxide nanorod/carbon cloth for untreated carbon fiber surface microscopic appearance；
Fig. 3 is the coefficient of kinetic friction figure of untreated carbon cloth and carbon cloth after the growth of hydro-thermal electrophoresis, and wherein CP-1 is indicated Untreated carbon cloth, CP-2 indicate carbon cloth after the growth of hydro-thermal electrophoresis.
Specific implementation mode
Embodiments of the present invention are described in further detail below：
A kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material, includes the following steps：
1) carbon cloth is cut to 5 × 8 rectangles first, the carbon cloth of lock seaming is ultrasonically treated 24 by surrounding lock seaming in ethanol Hour, carbon cloth taking-up deionized water is rinsed 3-5 times, then the soxhlet extraction acetone soln of the carbon cloth after cleaning exists 60-80 DEG C extracts 2-3 hours, and 10min is rinsed with deionized water；
2) using methacrylic acid as grafted monomers, using diene synthesis in the lossless oxygen-containing function of grafting of carbon cloth surfaces Group.
3) zinc acetate dihydrate and sodium hydroxide are dissolved in respectively in ethanol solution, being uniformly mixing to obtain molar concentration is Sodium hydroxide solution (the note that the acetate dihydrate zinc solution (being denoted as solution B) and molar concentration of 0.0125mol/L is 0.025mol/L For solution C), into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, is added into solution C Ethanol solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped to after stirring is stood in solution D and is obtained To zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 15-30min in the seed layer colloidal sol of zinc source, is dried with 100-150 DEG C, repeat to obtain for 3-5 times Contain the carbon cloth of seed layer in surface；
5) by zinc source and alkali source with 1：1 molar ratio mixing is added in ultra-pure water, obtains growth-promoting media, and zinc source is six hydration nitre Sour zinc；Alkali source is hexamethylene tetraammonia, ammonium fluoride or ammonium chloride, and the molar concentration in zinc source is 0.025mol/L in growth-promoting media.
6) carbon cloth that seed layer is contained on surface is placed in growth-promoting media, ZnO is grown in carbon cloth surfaces using hydro-thermal electrophoresis Nanometer rods, graphite cake make anode, and carbon cloth makees cathode.Electrophoresis time is 15-60min, electrophoretic current 0.15-0.2A, voltage 0.3-0.35V。
7) phenolic resin that the carbon cloth surfaces dipping that vacuum pressure impregnating method is obtained in step 6) is modified is used, its resin is made Quality accounts for the 30-40% of composite material, is dried at room temperature for 24 hours, then under vulcanizer hot pressing can be obtained zinc oxide Nanometer rods/carbon cloth friction material.
The present invention uses hydro-thermal electrophoresis in carbon fiber surface growing zinc oxide nanorod, using hydrothermal synthesis technology as base Plinth couples electrophoretic deposition technique, makes full use of the postcritical hyperbaric environment of hydro-thermal and the efficient feature of electric field, surface is made to charge Nucleus orientated deposition to carbon fiber surface, then surface is efficient, uniform growth in situ zinc oxide, zinc oxide as fiber with Bridge joint between resin, chemical bonding and mechanical engagement effect effectively enhance the knot of the interface between fiber and resin matrix It closes, and then improves the microcosmic abrasional behaviors such as three-dimensional carbon fiber attrition in actuation process, matrix peeling and third body abrasive grain, substantially Degree improves tribological property and mechanical performance.The hydro-thermal electrophoresis speed of growth is fast, simple process and low cost, adapts to industrialization Batch production, be with a wide range of applications.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) it is that surrounding is lockstitched a border with line after carbon cloth is cut into 5cm × 8cm rectangles, the carbon cloth on side will be locked in ethanol solution It is ultrasonically treated for 24 hours, carbon cloth taking-up deionized water is rinsed 3 times, dried in 60 DEG C of baking ovens.Soxhlet extraction is used again Carbon cloth being cleaned at 80 DEG C with acetone soln 2 hours, 10min being rinsed with deionized water, at 60 DEG C, drying is for 24 hours；
2) using methacrylic acid as grafted monomers, (80 DEG C, 3h) are lossless in carbon cloth surfaces diene synthesis under the conditions of oil bath It is grafted oxygen-containing functional group.
3) zinc acetate dihydrate and sodium hydroxide are stirred to be dissolved in respectively in ethanol solution at 60 DEG C and obtains molar concentration and is The sodium hydroxide solution that the acetate dihydrate zinc solution of 0.0125mol/L is denoted as solution B and molar concentration is 0.025mol/L is denoted as Solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, and ethyl alcohol is added into solution C Solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped in solution D at 60 DEG C and stirs standing After obtain zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 15min in the seed layer colloidal sol of zinc source, is dried with 150 DEG C, be repeated 4 times to obtain surface and contain crystalline substance The carbon cloth of kind layer；
5) zinc nitrate hexahydrate and hexa are pressed 1：It is obtained in the deionized water that 1 molar ratio is mixed to join Zinc source molar concentration is 0.025mol/L zinc source growth-promoting media；
6) carbon cloth that seed layer is contained on surface is placed in hydro-thermal electrophoretic apparatus, waits for being heated to grow in hydro-thermal electrophoresis apparatus After 90 DEG C of temperature, using graphite cake as anode, carbon cloth keeps electric current in 0.2A, voltage is in 0.35V, hydro-thermal electricity as cathode Swim developing zinc oxide 30min.
7) vacuum pressure impregnating method is used, carbon cloth is immersed into phenolic resin, ensures that the quality of the content of resin accounts for composite wood The 35% of material, makes it dry for 24 hours at room temperature.It it is then 150 DEG C in hot pressing temperature, hot pressing pressure is hot pressing 10min under 10MPa Obtain zinc oxide nano rod/carbon cloth reinforced resin friction material.
Embodiment 2
1) it is that surrounding is lockstitched a border with line after carbon cloth is cut into 5cm × 8cm rectangles, the carbon cloth of lock seaming is surpassed in ethanol solution For 24 hours, carbon cloth taking-up deionized water 4 times is dried in 60 DEG C of baking ovens for sonication.Soxhlet extraction acetone is used again Solution cleans carbon cloth at 70 DEG C 1 hour, and 5min is rinsed with deionized water, is dried for 24 hours at 60 DEG C；
2) using methacrylic acid as grafted monomers, (80 DEG C, 3h) are lossless in carbon cloth surfaces diene synthesis under the conditions of oil bath It is grafted oxygen-containing functional group.
3) zinc acetate dihydrate and sodium hydroxide are stirred to be dissolved in respectively in ethanol solution at 60 DEG C and obtains molar concentration and is The sodium hydroxide solution that the acetate dihydrate zinc solution of 0.0125mol/L is denoted as solution B and molar concentration is 0.025mol/L is denoted as Solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, and ethyl alcohol is added into solution C Solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped in solution D at 60 DEG C and stirs standing After obtain zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 30min in the seed layer colloidal sol of zinc source, is dried with 100 DEG C, be repeated 3 times to obtain surface and contain crystalline substance The carbon cloth of kind layer；
5) zinc nitrate hexahydrate and ammonium fluoride are pressed 1：Zinc source is obtained in the deionized water that 1 molar ratio is mixed to join to rub A concentration of 0.025mol/L zinc of that source growth-promoting media；
6) carbon cloth that seed layer is contained on surface is placed in hydro-thermal electrophoretic apparatus, waits for being heated to grow in hydro-thermal electrophoresis apparatus After 90 DEG C of temperature, using graphite cake as anode, carbon cloth keeps electric current in 0.15A, voltage is in 0.3V, hydro-thermal electricity as cathode Swim developing zinc oxide 45min.
7) vacuum pressure impregnating method is used, carbon cloth is immersed into phenolic resin, ensures that the quality of the content of resin accounts for composite wood The 30% of material, makes it dry for 24 hours at room temperature.It it is then 170 DEG C in hot pressing temperature, hot pressing pressure is hot pressing 15min under 10MPa Obtain zinc oxide nano rod/carbon cloth reinforced resin friction material.
Embodiment 3
1) it is that surrounding is lockstitched a border with line after carbon cloth is cut into 5cm × 8cm rectangles, the carbon cloth on side will be locked in ethanol solution It is ultrasonically treated for 24 hours, carbon cloth taking-up deionized water 4 times is dried in 60 DEG C of baking ovens.Used soxhlet extraction with third again Ketone solution cleans carbon cloth at 60 DEG C 3 hours, and 15min is rinsed with deionized water, is dried for 24 hours at 60 DEG C；
2) using methacrylic acid as grafted monomers, (80 DEG C, 3h) are lossless in carbon cloth surfaces diene synthesis under the conditions of oil bath It is grafted oxygen-containing functional group.
3) zinc acetate dihydrate and sodium hydroxide are stirred to be dissolved in respectively in ethanol solution at 60 DEG C and obtains molar concentration and is The sodium hydroxide solution that the acetate dihydrate zinc solution of 0.0125mol/L is denoted as solution B and molar concentration is 0.025mol/L is denoted as Solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, and ethyl alcohol is added into solution C Solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped in solution D at 60 DEG C and stirs standing After obtain zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 120min in the seed layer colloidal sol of zinc source, is dried with 120 DEG C, be repeated 5 times to obtain surface and contain The carbon cloth of seed layer；
5) zinc nitrate hexahydrate and ammonium chloride are pressed 1：Zinc source mole is obtained in the deionized water that 1 molar ratio is mixed to join A concentration of 0.025mol/L zinc source growth-promoting media；
6) carbon cloth that seed layer is contained on surface is placed in hydro-thermal electrophoretic apparatus, waits for being heated to grow in hydro-thermal electrophoresis apparatus After 90 DEG C of temperature, using graphite cake as anode, carbon cloth keeps electric current in 0.18A, voltage is in 0.3V, hydro-thermal electricity as cathode Swim developing zinc oxide 60min.
7) vacuum pressure impregnating method is used, carbon cloth is immersed into phenolic resin, ensures that the quality of the content of resin accounts for composite wood The 40% of material, makes it dry for 24 hours at room temperature.It it is then 170 DEG C in hot pressing temperature, hot pressing pressure is hot pressing 10min under 10MPa Obtain zinc oxide nano rod/carbon cloth reinforced resin friction material.
Embodiment 4
1) it is that surrounding is lockstitched a border with line after carbon cloth is cut into 5cm × 8cm rectangles, the carbon cloth on side will be locked in ethanol solution It is ultrasonically treated for 24 hours, carbon cloth taking-up deionized water 3 times is dried in 60 DEG C of baking ovens.Used soxhlet extraction with third again Ketone solution cleans carbon cloth at 80 DEG C 2 hours, and 10min is rinsed with deionized water, is dried for 24 hours at 60 DEG C；
2) using methacrylic acid as grafted monomers, (80 DEG C, 3h) are lossless in carbon cloth surfaces diene synthesis under the conditions of oil bath It is grafted oxygen-containing functional group.
3) zinc acetate dihydrate and sodium hydroxide are stirred to be dissolved in respectively in ethanol solution at 60 DEG C and obtains molar concentration and is The sodium hydroxide solution that the acetate dihydrate zinc solution of 0.0125mol/L is denoted as solution B and molar concentration is 0.025mol/L is denoted as Solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, and ethyl alcohol is added into solution C Solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped in solution D at 60 DEG C and stirs standing After obtain zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 25min in the seed layer colloidal sol of zinc source, is dried with 100 DEG C, be repeated 3 times to obtain surface and contain crystalline substance The carbon cloth of kind layer；
5) zinc nitrate hexahydrate and ammonium fluoride are pressed 1：Zinc source mole is obtained in the deionized water that 1 molar ratio is mixed to join A concentration of 0.025mol/L zinc source growth-promoting media；
6) carbon cloth that seed layer is contained on surface is placed in hydro-thermal electrophoretic apparatus, waits for being heated to grow in hydro-thermal electrophoresis apparatus After 90 DEG C of temperature, using graphite cake as anode, carbon cloth keeps electric current in 0.2A, voltage is in 0.3V, hydro-thermal electrophoresis as cathode Developing zinc oxide 15min.
7) vacuum pressure impregnating method is used, carbon cloth is immersed into phenolic resin, ensures that the quality of the content of resin accounts for composite wood The 30% of material, makes it dry for 24 hours at room temperature.It it is then 150 DEG C in hot pressing temperature, hot pressing pressure is hot pressing 15min under 10MPa Obtain zinc oxide nano rod/carbon cloth reinforced resin friction material.
Embodiment 5
1) it is that surrounding is lockstitched a border with line after carbon cloth is cut into 5cm × 8cm rectangles, the carbon cloth on side will be locked in ethanol solution It is ultrasonically treated for 24 hours, carbon cloth taking-up deionized water 5 times is dried in 60 DEG C of baking ovens.Used soxhlet extraction with third again Ketone solution cleans carbon cloth at 70 DEG C 2 hours, and 15min is rinsed with deionized water, is dried for 24 hours at 60 DEG C；
2) using methacrylic acid as grafted monomers, (80 DEG C, 3h) are lossless in carbon cloth surfaces diene synthesis under the conditions of oil bath It is grafted oxygen-containing functional group.
3) zinc acetate dihydrate and sodium hydroxide are stirred to be dissolved in respectively in ethanol solution at 60 DEG C and obtains molar concentration and is The sodium hydroxide solution that the acetate dihydrate zinc solution of 0.0125mol/L is denoted as solution B and molar concentration is 0.025mol/L is denoted as Solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, and ethyl alcohol is added into solution C Solution dilutes to obtain the solution E of a concentration of 0.0071mol/L, and E solution is slowly dropped in solution D at 60 DEG C and stirs standing After obtain zinc source seed layer colloidal sol；
4) carbon cloth is immersed in 200min in the seed layer colloidal sol of zinc source, is dried with 100 DEG C, be repeated 4 times to obtain surface and contain The carbon cloth of seed layer；
5) zinc nitrate hexahydrate and ammonium chloride are pressed 1：Zinc source mole is obtained in the deionized water that 1 molar ratio is mixed to join A concentration of 0.025mol/L zinc source growth-promoting media；
6) carbon cloth that seed layer is contained on surface is placed in hydro-thermal electrophoretic apparatus, waits for being heated to grow in hydro-thermal electrophoresis apparatus After 90 DEG C of temperature, using graphite cake as anode, carbon cloth keeps electric current in 0.15A, voltage is in 0.3V, hydro-thermal electricity as cathode Swim developing zinc oxide 30min.
7) vacuum pressure impregnating method is used, carbon cloth is immersed into phenolic resin, ensures that the quality of the content of resin accounts for composite wood The 30% of material, makes it dry for 24 hours at room temperature.It it is then 150 DEG C in hot pressing temperature, hot pressing pressure is hot pressing 10min under 10MPa Obtain zinc oxide nano rod/carbon cloth reinforced resin friction material.
Fig. 1 be hydro-thermal electrophoresis in the schematic diagram of carbon cloth surfaces growth in situ ZnO nanorod, make full use of hydro-thermal overcritical Hyperbaric environment and the efficient feature of electric field, make surface charge nucleus orientated deposition to carbon fiber surface, then on surface Efficiently, uniform growth in situ.Nano-oxide is as the bridge joint between fiber and resin, chemical bonding and mechanical engagement effect The interface cohesion between fiber and resin matrix is effectively enhanced, is the result figure of embodiment 1 from Fig. 2, compares original carbon fiber Fiber after being grown with hydro-thermal electrophoresis illustrates that successfully oxidation can be grown on the surface of carbon fiber using preparation method of the present invention Zinc nanometer rods, Fig. 3 are the result figure of embodiment 1, and paired observation is it is found that pass through the company of carbon cloth composite material after present invention processing Continuous friction coefficient is more stable, and its coefficient of kinetic friction is higher than original untreated carbon cloth composite material, illustrates its frictional property It can stablize, frictional behaviour is good.

Claims (9)

1. a kind of method that hydro-thermal electrophoresis prepares zinc oxide nano rod/carbon cloth friction material, which is characterized in that including following step Suddenly：
Step 1：After handling carbon cloth with EtOH Sonicate, carbon cloth is cleaned；
Step 2：Using methacrylic acid as grafted monomers, using the lossless grafting of the carbon cloth surfaces of diene synthesis after cleaning Oxygen-containing functional group；
Step 3：Zinc acetate dihydrate and sodium hydroxide are dissolved in ethanol solution respectively, stirs evenly and respectively obtains acetate dihydrate Zinc solution and sodium hydroxide solution, are denoted as solution B and solution C respectively, and ethanol solution is added into solution B and dilutes to obtain solution D, Ethanol solution is added into solution C to dilute to obtain solution E, E solution is added drop-wise to after stirring is stood in solution D and obtains zinc source crystal seed Layer colloidal sol；
Step 4：The carbon cloth that step 2 obtains is impregnated in the seed layer colloidal sol of zinc source, is then dried, if repeated impregnations and drying After dry time, the carbon cloth that seed layer is contained on surface is obtained；
Step 5：By zinc source and alkali source with 1：1 molar ratio mixing is added in ultra-pure water, obtains growth-promoting media；
Step 6：The carbon cloth that seed layer is contained on surface is placed in growth-promoting media, ZnO is grown in carbon cloth surfaces using hydro-thermal electrophoresis Nanometer rods；
Step 7：The carbon cloth surfaces obtained in step 6 using vacuum pressure impregnating method impregnate phenol-formaldehyde resin modified, then dry, It is finally hot-forming to obtain zinc oxide nano rod/carbon cloth friction material.
2. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, Be characterized in that, in step 1 cleaning be specially：Carbon cloth after supersound process deionized water is rinsed 3-5 times, will then be rinsed Carbon cloth afterwards is extracted 2-3 hours using soxhlet extraction acetone soln at 60-80 DEG C, then rinses 10min with deionized water.
3. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, is dissolved in zinc acetate dihydrate and sodium hydroxide in ethanol solution respectively in step 3, stir evenly to respectively obtain and rub A concentration of 0.0125mol/L acetate dihydrates zinc solution of that and molar concentration are 0.025mol/L sodium hydroxide solutions, are denoted as respectively Solution B and solution C, into solution B, addition ethanol solution dilutes to obtain the solution D of a concentration of 0.0014mol/L, into solution C Ethanol solution is added to dilute to obtain the solution E of a concentration of 0.0071mol/L.
4. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, Be characterized in that, in step 4 dip time be 15-30min, drying temperature be 100-150 DEG C, repeated impregnations and drying 3-5 times.
5. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, zinc source is zinc nitrate hexahydrate in step 5；Alkali source is hexa, ammonium fluoride or ammonium chloride.
6. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, the molar concentration in zinc source is 0.025mol/L in the growth-promoting media that step 5 obtains.
7. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, make anode when hydro-thermal electrophoresis with graphite cake in step 6, carbon cloth makees cathode, electrophoresis time 15-60min, electricity Swimming electric current is 0.15-0.2A, voltage 0.3-0.35V.
8. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, the mass fraction that post-modification phenolic resin is impregnated in step 7 is 30-40%.
9. the method that a kind of hydro-thermal electrophoresis according to claim 1 prepares zinc oxide nano rod/carbon cloth friction material, It is characterized in that, drying temperature is room temperature in step 7, and drying time is 24 hours.
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