CN106637912A - Ferrous alloy composite fiber and preparation method thereof - Google Patents
Ferrous alloy composite fiber and preparation method thereof Download PDFInfo
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- CN106637912A CN106637912A CN201611224451.9A CN201611224451A CN106637912A CN 106637912 A CN106637912 A CN 106637912A CN 201611224451 A CN201611224451 A CN 201611224451A CN 106637912 A CN106637912 A CN 106637912A
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- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
Abstract
The invention discloses a ferrous alloy composite fiber and a preparation method thereof. A graphene layer having the effects of conducting electricity, conducting heat and sealing is used for coating a ferrous alloy fiber for the first time, so that the ferrous alloy fiber not only has good electricity conducting capacity but also has good anticorrosion capacity. The invention also provides a preparation method of a graphene layer coated ferrous alloy fiber, the microwave technology of rapid heating, the microwave absorption characteristics of a graphene derivative and microwave vortex heating characteristics of the surface of the ferrous alloy fiber are combined, so that a graphene derivative layer is coated on the surface of the ferrous alloy fiber to form a composite fiber, then, in a set atmosphere, the composite fiber moves at a set speed to pass through a microwave heating region, the graphene derivative layer on the surface of the composite fiber is processed by microwave heating in a set time to be converted into a graphene layer, then the composite fiber leaves the microwave heating region and is cooled, and finally extruding treatment is performed on the composite fiber, so that the composite ferrous alloy fiber having good electricity conducting capacity and good anticorrosion capacity can be obtained.
Description
Technical field
The invention belongs to Material Field, is related to a kind of ferrous alloy composite fibre and preparation method thereof, particularly will have
The Graphene of good conductive ability and sealing process be used for coat ferrous alloy fiber so that ferrous alloy fiber have it is good
Conductive capability well and anti-corrosion capability.
Background technology
With society development, including the ferrous alloy including iron, steel, stainless steel etc. fiber due to possessing good machine
The many merits such as tool performance, cheap price and obtaining extensively application including the wide spectrum such as engineering construction, electromagnetic protection.So
And the presence for some problems such as needing to be improved including etching problem, electric conductivity of ferrous alloy fiber itself limits it and enters
The popularization and application of one step.Therefore the coating decoration of ferrous alloy fiber is paid high attention to by people, and including high score attached bag
Cover, coatings, ferrous alloy are compound etc., and aspect obtains fast development.And still further aspect, Graphene leads as a kind of two dimension
Electric material, its excellent mechanical property (Young's modulus is up to 1.0TPa), (electron mobility is up to 10 to electrical properties6cm2.v-1s-1), (thermal conductivity coefficient is up to 5000w.m to thermal property-1.k-1), (visible absorption of single-layer graphene only has optical property
2.3% and excellent locked mode characteristic), the theoretical specific surface area (2630m of super large2.g-1) cause it to modify field in metal surface
Application potential paid high attention to by people.The research of people shows the graphite that copper wire surface is prepared by CVD method
Alkene layer coated copper wire not only has good anti-corrosion capability but also its conductive capability is also very excellent.Because Graphene gas phase is sunk
The catalysis characteristics that product needs, is confined to a few metals material such as copper, nickel by the metal material of vapor deposition growth Graphene at present
Material.Additionally, people also developed the graphene oxide or its reduzate redox graphene produced based on graphite.Oxidation
Graphene or redox graphene solution can be layering coating in the Graphene basal plane mode parallel with coating substrate
Film forming, but its conductive capability is not good enough and Graphene basal plane on because there is the aperture that oxidation is formed certain material to pass through energy
Power affects it to widely use larger range of.And be based on high temperature reduction by graphene oxide prepare with high reducing degree
Although graphene powder electric conductivity improve, because its dispersive property is not good enough, current people can only pass through powder electrostatic
The mode of painting is coated on material surface.But electrostatic powder spraying is difficult to so that Graphene basal plane because graphene powder is reunited
Uniform covering material is sprawled, therefore it can not play the superior function of grapheme material.Also developed for this people and with the addition of
Prevent including the Graphene of the graphene-based material including graphene oxide powder, redox graphene powder and graphene powder
Rotten coating.But what one side anticorrosive paint added can affect Graphene to include leading including the other materials including macromolecular material
Electricity, the performance of the capacity of heat transmission, and the basal plane hole that still further aspect graphene oxide and redox graphene are present is to anti-corrosion
The impact of ability and graphene powder are difficult to dispersed and coating characteristic so that it is anti-that the coating of Graphene anticorrosive paint is obtained
The performance of rotten coating also needs to further improve by exploitation.So people can be effectively in the urgent need to developing new technology
Graphene layer is coated on into material surface.For this purpose, the present invention proposes first for graphene layer to be coated on ferrous alloy in the world
Fiber surface and obtain the composite iron-base alloy fiber with good conductive ability and antiseptic power.The present invention proposes system simultaneously
Standby graphene layer coats the preparation method of ferrous alloy composite fibre, i.e., derivative by Graphene first on ferrous alloy fiber
Thing solution coating and obtain Graphene derivative layer cladding ferrous alloy composite fibre, then setting atmospheric condition under be combined
Fiber with setting speed motion by heating using microwave area, using the microwave absorption capacity of Graphene microcell in Graphene derivative and
The metal swirl heat characteristic of ferrous alloy fiber surface a few micrometers depth causes Graphene derivative layer or the graphite for aoxidizing
Alkene edge derivative layer and ferrous alloy superficial layer be rapidly heated due to microwave action and reduction-oxidation Graphene derivative
Or de- graphene edge derivative edge functional group and Graphene derivative layer is converted into into graphene layer.Because solution is applied
The Graphene derivative layer of cloth is coated on layer by layer on ferrous alloy fiber, and now at high temperature with the form that Graphene basal plane is sprawled
Graphene layer that reason is obtained due also to interaction between different graphene film interlayer pi-electron cloud and can keep preferably leading
Electricity, heat conduction and mechanical performance.On the other hand, composite fibre not only can be controlled accurately with setting speed motion by heating using microwave area
The heat time of made composite fiber, the microwave-oven-heating time as is set with multiple class that 30 seconds is unit, but tests
Show that a whole shelves are heated under protective atmosphere may be occurred to cause the Graphene derivative layer being coated with due to heating up too fast
It is at random or even come off, though accurate micro-wave oven can set microwave pulse length, but be also difficult to set may optimum heating when
Between such as 1.2 seconds, and composite fibre then can easily be obtained by heating using microwave area with setting speed according to heating using microwave area size
The accurate optimal heat time.Composite fibre can also avoid heating using microwave area not same district with setting speed by heating using microwave area
The heating that domain heating effect different band is come is uneven.In fact, composite fibre is placed on into heating a period of time in micro-wave oven, take out
Can be clearly felt that the composite fibre heating effect for being placed on different heating region is different afterwards, in this and micro-wave oven thermoelectricity is added
The uniformity of field is relevant, although can improve microwave-oven-heating uniformity, but its by designing such as curve antenna structure mode
Also there is certain limit.And composite fibre with setting speed by whole heating using microwave area then because all composite fibres are by whole
The individual thermal treatment zone and obtain consistent heating effect.Certainly composite fibre can be with essence by whole heating using microwave area with setting speed
Its cooling opportunity is really controlled, so as to contribute to optimize technique.And the composite fibre of the present invention passes through whole microwave with setting speed
The method of the thermal treatment zone also with the process compatible of fiber process, hence help to the batch production of ferrous alloy composite fibre.And it is micro-
Wave heating (the usual time is in seconds), due to selectively heating Graphene derivative layer and ferrous alloy fiber surface, not only may be used
With the high energy consumption for avoiding other heating (the usual time is in hours) that heat up from causing due to needing Heat transmission etc., and leave micro-
Wave heating area can quickly cool down, therefore greatly shorten process time, so the application prepares Graphene using heating using microwave
The method of layer cladding ferrous alloy composite fibre can not only obtain the graphite that surface has good conductive ability and antiseptic power
Alkene layer, and due to using open heat and heat selective microwave heating technique and can effectively reducing energy consumption be simultaneously
Shortening process time hence helps to the further research and development and popularization and application of ferrous alloy and grapheme material.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of ferrous alloy composite fibre and preparation method thereof, will graphite
Alkene layer is coated on ferrous alloy fiber surface and obtains the New-type composite fibre with good conductive ability and antiseptic power.This
It is bright to also proposed the preparation method that graphene layer coats ferrous alloy fiber, can quickly and easily prepare graphene layer cladding
Ferrous alloy composite fibre, hence help to the further development of ferrous alloy composite fibre with application.
Technical scheme：A kind of ferrous alloy composite fibre of the present invention, ferrous alloy fiber surface coated graphite alkene layer.Institute
The carbon content for stating graphene layer is more than 90%.The ferrous alloy is included by iron, steel and stainless steel.
A kind of preparation method of ferrous alloy composite fibre of the present invention, the ferrous alloy Surface coating graphene layer leads to
Cross following method to realize：Graphene derivative solution is prepared first, then by Graphene derivative solution coating in selected iron
Based alloy fiber surface forms the ferrous alloy composite fibre of Graphene derivative layer cladding, is subsequently combined fibre under setting atmosphere
Dimension causes ferrous alloy composite fibre to be processed and by its table by microwave heating high-temperature with setting speed motion by heating using microwave area
The Graphene derivative layer in face is converted into graphene layer, and subsequent ferrous alloy composite fibre leaves heating using microwave area and is cooled,
Then extrusion process can obtain the ferrous alloy composite fibre of graphene layer cladding.
The Graphene derivative refers to the oxide i.e. graphene oxide of Graphene and the graphene oxide and stone of reduction
Black alkene edge derivative.
The setting atmosphere refers to inert atmosphere, reducing atmosphere or vacuum state；The inert atmosphere refers to gas
Not with the gas of Graphene derivative reaction, such as nitrogen, helium, argon gas；The reducing atmosphere is referred in gas containing can
The gas of reduced graphene derivative, such as hydrogen, alcohols, alkanes gas；The vacuum state refers to that air pressure is less than 4KPa (phases
- 20KPa is less than to relative degree of vacuum)；
The ferrous alloy composite fibre leaves heating using microwave area and cooled applies by cold atmosphere or additionally cold
Air-flow body and cool down.
The Graphene derivative layer is converted into graphene layer and refers to that the Graphene of oxidation is reduced in high temperature and is converted into
Graphene, and then there is high temperature off-clip edge functional group and be converted into Graphene in graphene edge derivative.
When the composite fibre is heated by heating using microwave area with setting speed motion according to heating using microwave area size Control
Between.
The ferrous alloy composite fibre can be repeated to spread out with multiple high temp process Graphene by microwave heating high-temperature process
Biosphere.
It is described that Graphene derivative solution coating is formed into Graphene derivative layer in selected ferrous alloy fiber surface
The ferrous alloy composite fibre of cladding, subsequently composite fibre is made with setting speed motion by heating using microwave area under setting atmosphere
Obtain ferrous alloy composite fibre and be converted into graphene layer by microwave heating high-temperature process and by the Graphene derivative layer on its surface,
Subsequently ferrous alloy composite fibre leaves heating using microwave area and is cooled, and then the serial procedures of extrusion process can repeat, i.e.,
Graphene derivative can be repeatedly coated with and microwave high-temperature is carried out and processed to obtain the graphene layer for thickening.
The coating includes dip-coating, spraying, brushing, foam coating, layer assembly coating, contact coating.
Beneficial effect：The present invention compared with prior art, with advantages below：
The application is used for the two-dimensional graphene material with good conductive ability and sealing ability to coat iron-based conjunction first
Golden fiber forms the composite iron-base alloy fiber with good conductive ability and antiseptic power.Give nationality simultaneously to be spread out by Graphene
Biological solution coating, composite fibre with setting speed by heating using microwave area and microwave selective heat Graphene derivative floor and
Ferrous alloy fiber surface and high-temperature process Graphene derivative layer are simultaneously translated into graphene layer, such that it is able to convenient, fast
Speed, low energy consumption ground obtain the new iron-based alloy composite fibre with good conductive ability and antiseptic power.The present invention can be
Ferrous alloy fiber, the further development of grapheme material and application are made contributions.
Description of the drawings
Fig. 1 is ferrous alloy composite fibre preparation flow schematic diagram.
Fig. 2 is that fiber bypasses metal baffle schematic diagram by guide wheel.
Have in figure：1st, ferrous alloy fiber；2nd, immersion liquid pond, 2a, solution；3rd, liquid squeezing roll；4th, drying room；5th, metal baffle, 5a,
Aperture；6th, microwave oven, 6a, microwave input, 6b, heating cavity；7th, atmosphere chamber, 7a, gas population, 7b, gas vent；8、
Temperature control afterwards, 8a, temperature controlled fluid entrance, 8b, temperature controlled fluid outlet；9th, guide wheel；10th, compression roller.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further illustrated.
First the nationality of ferrous alloy fiber 1 is coated with Graphene derivative solution by guide wheel 9 by solution 2a in immersion liquid pond 2,
Then the ferrous alloy composite fibre for being coated with Graphene derivative layer goes redundant solution by the way that liquid squeezing roll 3 is crowded, subsequently compound fibre
Dimension is dried by drying room 4, and subsequent composite fibre is entered in the micro-wave oven 6 protected by the metal baffle 5 for being provided with aperture 5a.
Microwave-oven-heating region is arranged atmosphere chamber 7 and is controlled in heating using microwave region iron-based using gas access 7a and gas vent 7b
Atmosphere around alloy composite fibre.Then nationality is closed under setting atmosphere by microwave input 6a input microwaves to iron-based
Graphene derivative layer on golden composite fibre then passes through out foraminate metal baffle and leaves micro-wave oven by heating using microwave
6 and enter the area of rear temperature control 8 and export 8b design temperatures circulation of fluid using temperature controlled fluid entrance 8a and temperature controlled fluid and control micro-
The temperature of the ferrous alloy composite fibre after Wave heating process, then passes through the ferrous alloy composite fibre that microwave heating treatment is crossed
The ferrous alloy composite fibre coated by graphene layer is obtained by the extruding of compression roller 10.
Wherein ferrous alloy baffle plate 5 can be beneficial to fiber by aperture 5a is opened continuously operation is changed to guide fiber by guide wheel 9
Bypass ferrous alloy baffle plate and continuously run so as to be conducive to stop microwave and strengthen the protection to human body.As shown in Figure 2.
It is that people need the one of solution that graphene layer is converted into after ferrous alloy fiber surface coated graphite ene derivative layer
Individual challenge.Except extra high temperature long time treatment, general chemistry reduction and high temperature reduction method process Graphene derivative
Afterwards the content of wherein carbon is difficult more than 90%, and extra high temperature long time treatment not only energy consumption is big, but also can be to graphite
The laminate structure of ene derivative causes to damage.Therefore in the urgent need to developing new technology Graphene derivative layer is converted into into stone
Black alkene layer.Have Microwave Absorption Properties and microwave using Graphene derivative first in the world for this present invention quick with heating up
The characteristics of, by the way that Graphene derivative floor is passed through into heating using microwave area with setting speed under setting atmosphere, so as to accurately control
Heat time processed and avoid heating inequality in the case of heat Graphene derivative layer and by Graphene derivative layer conversion
For graphene layer.In fact, microwave treatment is applied in Graphene associated materials some correlative studys.Such as people's system
A kind of method of standby graphene oxide is exactly microwave treatment graphite oxide, and high temperature of the nationality by heating using microwave up to more than 2,000 degrees Celsius is led
Graphite oxide inside is caused to produce a large amount of gases and be separated from each other few layer even single-layer graphene oxide in graphite and come.And 2,000
Degree Celsius high temperature above almost can thoroughly redox graphene and be translated into Graphene.Our experiences show that
Microwave heating treatment is including including graphene oxide, redox graphene, graphene edge derivative under nonoxidizing atmosphere
Graphene derivative can efficiently be converted into Graphene.Problem is that conventional microwave heats due to concentrating heating, therefore
Local temperature is high, causes vigorous reaction to produce gas and so that the structure of Graphene derivative material is destroyed, and Graphene spreads out
Biosphere becomes chip, it is therefore necessary to which effective control microwave heating process causes effectively high-temperature process Graphene to derive
Thing, can avoid destruction of the vigorous reaction to Graphene derivative material structure again.Our experiences show that under setting atmosphere
Graphene derivative can be efficiently converted into Graphene by of short duration heating using microwave of the time less than 3 seconds, but due to reduction
The drastically expansion including the gas including aqueous vapor for producing is that cause Graphene derivative material structure to destroy one is important to be pushed away
Hand, therefore we just generate rapid microwave heating, subsequently quick cooling causes to reduce steam for producing etc. and avoids drastically expanding
Thinking.Experiment show by being passed through cold nitrogen in the case of, Graphene derivative material after by microwave fast heating by
In quick cooling the gas for producing is reduced therefore, it is possible to preferably keeping the structure of Graphene derivative material and being eventually converted into
Grapheme material.Certainly the nitrogen for being passed through cooling is cooled down while heating material, need to be changed from from the point of view of energy ezpenditure
Enter.The another question that Graphene derivative material microwave heats is that uneven problem is heated in heating using microwave area, this
It is relevant with the uniformity of thermoelectric field is added in micro-wave oven, although micro-wave oven can be improved by designing such as curve antenna structure mode
Heating uniformity, but electric field is uneven is difficult to avoid that, and the effect of non-uniform heat flux then causes Graphene derivative material to convert
Effect for Graphene has differences and affects overall performance in zones of different, and may occur if the heat time is improved
A part of Graphene derivative material is destroyed because of over-heating, and another part then may also without well also
It is former.So in order to reduce one side heating using microwave, one side cooling fluid cooling zone carrys out the increase of energy consumption and improves microwave heating treatment
Uniformity, we consider Graphene derivative material under setting atmosphere so that setting speed is heated by heating using microwave area
Precise control heat time, the method for then quickly cooling down so that the Graphene derivative in all regions passes through whole microwave
The thermal treatment zone and obtain relatively uniform heating, and unless special requirement cooling just first room temperature cooling after the completion of heating using microwave, so
Leave micro-wave oven afterwards to be cooled down so as to reduce the energy consumption of cooling by cooling device again.Experiment shows that our method effect is good
It is good, for Graphene derivative layer is converted into graphene layer, the content of the carbon of graphene layer more than 90%, due to common graphite
3% oxygen is adsorbed with, therefore close to reducing completely, and good electrical property is presented.
With reference to embodiment, the present invention is further illustrated.
Embodiment one：
Graphene oxide powder and redox graphene powder are prepared first.30 grams of graphite mixing 15g sodium nitrate and 750
The milliliter concentrated sulfuric acid.Mixture is cooled in ice bath 0 degree Celsius, and is stirred after 2h, be slowly added to 90 grams of potassium permanganate, kept
Mixture temperature is less than 5 degrees Celsius in mixed process.The mixture is stirred for a hour, and is heated to by removing ice bath
Room temperature.Add 1 liter of distilled water in mixture and the temperature in oil bath increases to 90 degrees Celsius.Add 300 milliliters of water in addition, and
It is stirred for one and a half hours.The color of mixture becomes brown.Mixture and then 300 milliliters of hydrogen peroxide with 30% and 30 liters
Hot water treatment and dilution.The mixture further with excessive water washing, until the pH value of filtrate is almost neutral so as to obtain
Obtain graphene oxide.Subsequently graphene oxide freeze-drying can be obtained into graphene oxide powder.Then by graphene oxide
Powder disperses in water and is reduced 12 hours at 80 degrees Celsius with hydrazine hydrate.Redox graphene is formed with black precipitate, is used
0.45 μm of PTFE film is collected by filtration, and is rinsed with substantial amounts of water.Product is carried by methyl alcohol, tetrahydrofuran (THF) and water with Soxhlet
Follow the example of and be further purified.Finally, the redox graphene for being obtained is subzero 120 Celsius under 0.05 millimetres of mercury vacuum environment
Degree is lyophilized.Subsequently deionized water prepares the redox graphene aqueous solution of 0.5 mg/ml.
Secondly a diameter of 0.5 millimeter of SWH82B steel wires are obtained.Then above-mentioned steel wire is passed through with 60 ms/min of speed
The redox graphene aqueous solution immersion liquid pond of 0.5 mg/ml is coated and to form surface and be coated with redox graphene
The composite steel wire of layer, it is unnecessary molten that subsequent composite steel wire is that liquid squeezing roll that 200 N/centimetre hardness are 90 degree is removed by line pressure
Liquid, then composite steel wire enter 150 degrees Celsius of drying rooms and be dried, obtain to surface and be coated with the clad steel of redox graphene layer
Silk.Then composite steel wire is by opening foraminate stainless steel shoe into the heating using microwave area of argon gas protection.Heating using microwave area by
10 power are 1000W micro-wave ovens connection composition, and heating zone length reaches 1 meter, and then composite steel wire nationality is by microwave-oven-heating about 1
Second, subsequently cooled down using the cold air of recirculated cooling water temperature control into rear temperature control area by aperture on steel shoe, it is multiple thereafter
Close steel wire carries out extrusion process by the compression roller that line pressure is 1200 Ns/centimetre.Above-mentioned coating-heating using microwave-the cooling of repetition-
Extrusion process obtains graphene layer carbon content for three times and is more than 5000Sm more than 90% electrical conductivity-1Graphene layer cladding clad steel
Silk.It is existing to there is no significantly corrosion for one week in the sulfuric acid solution of 1M in the composite steel wire in the case of not exposing exposed head end yet
As showing excellent corrosion resistance features.
Embodiment two：
A diameter of 3 millimeters of SWRM10 steel wires are obtained first, subsequently steel wire are passed through into 30 centimetres with the speed of 0.1 meter per second
The graphene oxide water solution of 10 long mg/mls, obtains the composite steel wire that surface is coated with graphene oxide layer after being dried.
In nitrogen and hydrogen ratio it is 55 by the composite steel wire:With the speed of 0.1 meter per second in room temperature shape under protecting under 1 reducing atmosphere
10 centimetres of thermals treatment zone of micro-wave oven diameter under state by power for 1000W are heated about 1 second, are subsequently again introduced into room temperature region
Cooled down, then composite steel wire carries out extrusion process, the above-mentioned microwave of repetition by the compression roller that line pressure is 1000 Ns/centimetre
Heating-cooling-extrusion process 20 times,.Obtain graphene layer carbon content and be more than 5000Sm more than 90% electrical conductivity-1Graphene layer
The composite steel wire of cladding.The composite steel wire does not also occur for one week in the salpeter solution of 1M in the case of not exposing exposed head end
Significantly corrosion phenomenon, shows excellent corrosion resistance features.
Embodiment three：
The graphene platelet of edge carboxylated is prepared first.5 grams of graphite and 100 grams of dry ice are added containing 1000 grams of diameter
In the ferrous alloy capsule of 5 millimeters of ferrous alloy balls.Container is sealed and is fixed on planetary ball mill (F-P4000), and with
500rpm (rev/min) speed is stirred 48 hours.Subsequently, internal pressure is slowly discharged by a gas vent.Terminate in ball milling
When by opening container cover in atmosphere, by the wet steam in air cause carboxylate occur violent hydration reaction generate carboxylic acid and
Send out flash of light.Products obtained therefrom 1M hydrochloric acid solutions carry out soxhlet type to be thoroughly acidified carboxylate and remove presumable ferrous alloy
Impurity.Final subzero under 0.05 millimetres of mercury vacuum environment 120 degrees Celsius obtain edge carboxylated Graphene in lyophilized 48 hours
The furvous powder of nanometer sheet.Edge carboxylated graphene nanometer sheet is obtained for 30 minutes by the ultrasound in isopropanol
The homodisperse solution of 0.1wt%.
Then the 6*29Fi+FC steel wire ropes of 2 centimetres of diameter are obtained.Subsequently steel wire rope is passed through into 50 with the speed of 0.1 meter per second
The edge carboxylated Graphene aqueous isopropanol of the 0.1wt% of centimeter length, obtains surface and is coated with edge carboxyl fossil after being dried
The composite steel wire rope of black alkene layer.The composite steel wire rope is led to the speed of 0.05 meter per second under helium protection under room temperature state
Overpower is heated about 2 seconds for 10 centimetres of thermals treatment zone of micro-wave oven diameter of 1000W, be subsequently again introduced into room temperature region carry out it is cold
But, then composite steel wire rope carries out extrusion process by the compression roller that line pressure is 1300 Ns/centimetre, and the above-mentioned solution of repetition is applied
Cloth-heating using microwave-cooling-extrusion process 3 times,.Obtain graphene layer carbon content and be more than 5000Sm more than 90% electrical conductivity-1Stone
The composite steel wire rope of black alkene layer cladding.The composite steel wire rope is not exposed in the case of exposed head end one week in the sulfuric acid solution of 1M
There is no obvious corrosion phenomenon, show excellent corrosion resistance features yet.
Example IV：
Edge halo graphene nanometer sheet is prepared first.5 grams of graphite are added containing 1000 grams 5 millimeters of ferrous alloys of diameter
In the ferrous alloy capsule of ball.Then capsule is sealed and five circulations charge and discharge argon under 0.05 millimetres of mercury vacuum pressure condition
Gas.Hereafter, it is that 8.75atm adds chlorine from gas access by cylinder pressure.Container is sealed and is fixed on planetary ball mill
(F-P4000), and with 500rpm (rev/min) speed stir 48 hours.Products obtained therefrom is successively carried out with methyl alcohol and 1M hydrochloric acid solutions
Soxhlet type is thoroughly removing small molecule organic impurities and presumable ferrous alloy impurity.Finally in 0.05 millimetres of mercury vacuum
The subzero 120 degrees Celsius furvous powder for obtaining edge chlorination graphene nanometer sheet for lyophilized 48 hours under environment.Then 0.1 is prepared
The edge chloro Graphene N of mg/ml, N '-dimethyl formamide DMF solution.
Secondly a diameter of 100 microns of 301 type stainless steel wires are obtained.Then stainless steel wire is led to the speed of 0.5 meter per second
The edge chloro Graphene N of 0.1 mg/ml of 40 centimeter lengths is crossed, N '-dimethyl formamide DMF solution obtains table after being dried
Face is coated with the composite stainless steel silk of edge chlorination graphene layer.The composite stainless steel silk is protected in the nitrogen containing 5% hydrogen
Under 10 centimetres of thermals treatment zone of micro-wave oven diameter with the speed of 0.02 meter per second under room temperature state by power as 1000W carry out plus
Heat about 5 seconds, is subsequently cooled down by recirculated cooling water, and then composite stainless steel silk is by extruding that line pressure is 500 Ns/centimetre
Roller carries out extrusion process, repeats above-mentioned solution coating-heating using microwave-cooling-extrusion process process 8 times,.Obtain graphene layer carbon
Content is more than 5000Sm more than 90% electrical conductivity-1Graphene layer cladding composite stainless steel silk.The composite stainless steel silk is not sudden and violent
There is no obvious corrosion phenomenon within one week in the salpeter solution of 1M in the case of revealing exposed head end yet, show excellent resistance to
Corrosion characteristics.
Embodiment five
The 6*19+FC steel wire ropes of 2 millimeters of diameter are obtained first.Then by steel wire rope with the speed operation of 1 point of meter per second, and
Allow steel wire rope apart from 6 centimetres of electrostatic atomiser nozzle, the voltage of 8KV is applied on electrostatic spray nozzles, and with 200 mul/min
Speed the redox graphene aqueous solution of 0.5 mg/ml is sprayed on steel wire rope by nozzle, subsequent room temperature do
It is dry, and repeat electrostatic spraying and drying at room temperature 10 times, obtain the steel wire composite rope of redox graphene layer cladding.This is combined
Rope is vacuum dried 10 hours at 50 degrees Celsius.Then composite fibre led to the speed room temperature of 0.05 meter per second under nitrogen protection
Overpower is heated about 2 seconds for 10 centimetres of thermals treatment zone of micro-wave oven diameter of 1000W, be subsequently again introduced into room temperature region carry out it is cold
But, subsequent composite steel wire rope is extruded by the compression roller that line pressure is 500 Ns/centimetre, the above-mentioned heating using microwave of repetition-cold
But-extrusion process 5 times, subsequent composite steel wire rope carries out extrusion process acquisition by the compression roller that line pressure is 1300 Ns/centimetre
The steel wire composite rope that graphene layer of electrical conductivity of the graphene layer carbon content more than 90% more than 5000S/M is coated.The clad steel
There is no obvious corrosion phenomenon in one week in the salpeter solution of 1M in cord, show in the case of not exposing exposed head end yet
Excellent corrosion resistance features.
Embodiment six
A diameter of 0.914 millimeter of iron wire is obtained first, subsequently iron wire is passed through into 40 centimeter lengths with the speed of 0.1 meter per second
1 mg/ml the redox graphene aqueous solution, surface is obtained after being dried and is coated with the compound of redox graphene layer
Iron wire.The compound iron wire is passed through into power as 800W with the speed of 0.02 meter per second under the vacuum environment of 2KPa in room temperature condition
10 centimetres of thermals treatment zone of micro-wave oven diameter heated about 5 seconds, be subsequently again introduced into room temperature region and cooled down, repetition it is above-mentioned micro-
Wave heating-cooling procedure 5 times, be then combined iron wire carries out extrusion process by the compression roller that line pressure is 800 Ns/centimetre.Obtain
Obtain graphene layer carbon content and be more than 5000Sm more than 90% electrical conductivity-1Graphene layer cladding compound iron wire.The compound iron wire
There is no obvious corrosion phenomenon within one week in the hydrochloric acid solution of 1M in the case of not exposing exposed head end yet, show excellent
Corrosion resistance features.
Embodiment seven
3 millimeters of 7*7 steel wire ropes of diameter are obtained first.Subsequently steel wire rope is passed through into 30 centimeter lengths with the speed of 0.1 meter per second
The graphene oxide water solution of 10 mg/mls, obtains the compound steel wire rope that surface is coated with graphene oxide layer after being dried.Will
The graphene oxide water solution of the compound mg/ml of steel wire rope cycling coating 10 and dry run 2 times, then steam in hydrazine hydrate
95 degrees Celsius of process obtain Surface coating for 24 hours with redox graphene layer in vapour the compound of redox graphene
Steel wire rope.Subsequently 10 centimetres of micro-wave oven diameter of the power as 1000W is passed through with the speed of 0.05 meter per second under room temperature under nitrogen protection
The thermal treatment zone is heated about 2 seconds, is subsequently again introduced into room temperature region and is cooled down, the above-mentioned cooling-heating using microwave of repetition-cooled
Journey 10 times, subsequently carries out three acquisition Graphenes of extruding to compound steel wire rope under the line pressure of 800 Ns/centimetre by compression roller
Derivative layer carbon content is more than 90%, the compound steel wire rope that graphene layer of the electrical conductivity more than 5000S/M is coated.The compound iron wire
There is no obvious corrosion phenomenon in one week in the hydrochloric acid solution of 1M in the case where exposed head end is not exposed in rope, show yet
Excellent corrosion resistance features.
Claims (10)
1. a kind of ferrous alloy composite fibre, it is characterised in that ferrous alloy fiber surface coated graphite alkene layer.
2. a kind of ferrous alloy composite fibre according to claim 1, it is characterised in that the carbon content of the graphene layer
More than 90%.
3. a kind of ferrous alloy composite fibre according to claim 1, it is characterised in that the ferrous alloy include by iron,
Steel or stainless steel.
4. a kind of a kind of preparation method of ferrous alloy composite fibre as claimed in claim 1, it is characterised in that the preparation side
Method is：Graphene derivative solution is prepared first, then by Graphene derivative solution coating in selected ferrous alloy fiber
Surface forms the ferrous alloy composite fibre of Graphene derivative layer cladding, subsequently under setting atmosphere composite fibre setting speed
Degree motion causes ferrous alloy composite fibre to be processed and by the Graphene on its surface by microwave heating high-temperature by heating using microwave area
Derivative layer is converted into graphene layer, and subsequent ferrous alloy composite fibre leaves heating using microwave area and is cooled, then at extruding
Reason can obtain the ferrous alloy composite fibre of graphene layer cladding.
5. a kind of preparation method of ferrous alloy composite fibre according to claim 4, it is characterised in that the Graphene
Derivative refers to the oxide i.e. graphene oxide of Graphene and the graphene oxide of reduction and graphene edge derivative.
6. a kind of preparation method of ferrous alloy composite fibre according to claim 4, it is characterised in that the setting gas
Atmosphere refers to inert atmosphere, reducing atmosphere or vacuum state.The inert atmosphere refers to that gas is not anti-with Graphene derivative
The gas answered；The reducing atmosphere is referred in gas containing the gas for being capable of reduced graphene derivative；The vacuum state
Refer to that air pressure, less than 4KPa, with respect to relative degree of vacuum -20KPa is less than.
7. the preparation method of a kind of ferrous alloy composite fibre according to claim 4, it is characterised in that the iron-based is closed
Golden composite fibre leaves heating using microwave area and cooled apply by cold atmosphere or additionally cold air-flow body and cool down.
8. a kind of preparation method of ferrous alloy composite fibre according to claim 4, it is characterised in that the Graphene
Derivative layer is converted into graphene layer and refers to that the Graphene of oxidation is reduced in high temperature and is converted into Graphene, and graphene edge
Then there is high temperature off-clip edge functional group and be converted into Graphene in derivative.
9. the preparation method of a kind of ferrous alloy composite fibre according to claim 4, it is characterised in that the iron-based is closed
Golden composite fibre can be repeated to process Graphene derivative layer with multiple high temp by microwave heating high-temperature process.
10. the preparation method of a kind of ferrous alloy composite fibre according to claim 4, it is characterised in that described by graphite
Ene derivative solution coating is combined in the ferrous alloy that selected ferrous alloy fiber surface forms Graphene derivative layer cladding
Fiber, subsequently composite fibre causes ferrous alloy composite fibre with setting speed motion by heating using microwave area under setting atmosphere
Graphene layer, the compound fibre of subsequent ferrous alloy are converted into by microwave heating high-temperature process and by the Graphene derivative layer on its surface
Dimension is left heating using microwave area and is cooled, and then the serial procedures of extrusion process can repeat, you can be repeatedly coated with Graphene
Derivative simultaneously carries out microwave high-temperature process to obtain the graphene layer for thickening.
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| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
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