CN106927705A - A kind of method in copper facing steel fiber surface controllable growth graphene coated film - Google Patents
A kind of method in copper facing steel fiber surface controllable growth graphene coated film Download PDFInfo
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- CN106927705A CN106927705A CN201710075136.2A CN201710075136A CN106927705A CN 106927705 A CN106927705 A CN 106927705A CN 201710075136 A CN201710075136 A CN 201710075136A CN 106927705 A CN106927705 A CN 106927705A
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- copper facing
- facing steel
- cement
- fiber surface
- temperature
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/48—Metal
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Abstract
The present invention provides a kind of method of utilization chemical vapour deposition technique in copper facing steel fiber surface controllable growth graphene coated film.Mainly comprise the following steps that：1) cleanings copper facing steel fibre；2) copper facing steel fibre is carried out the high temperature anneal by；3) regulation and control chemical vapor deposition method parameter and copper plated steel position of fibers；4) carries out graphene growth in copper facing steel fiber surface, is evenly coated, the graphene film that thickness is controllable.The technological process is simple to operation, the Graphene stable chemical nature of copper facing steel fiber surface, intensity and corrosion resistance of the copper facing steel fibre in cement-base composite material can be effectively improved, and can be as the forming core of hydrated reaction of cement point so as to advantageously facilitate hydrated reaction of cement, the structure for making cement form densification finally effectively prevents the generation of crackle from improving the intensity of cement-base composite material.Had broad application prospects in cement-base composite material field.
Description
Technical field
The present invention relates in the method in copper facing steel fiber surface controllable growth graphene coated film, belong to materialized length of schooling
Standby technical field.
Background technology
Graphene be one kind by carbon atom with sp2Hydridization formed with cellular crystal structure two-dimension nano materials, solely
Special lattice structure makes it have excellent mechanics, optically and thermally electricity, performance.Graphene scene effect transistor, high frequency
The aspects such as electronic device, transparent conductive film, composite, energy storage material, electrochemical sensor have broad application prospects.
The method for preparing Graphene at present mainly has micromechanics stripping method, SiC epitaxial growth methods, oxidation-reduction method and change
Learn vapour deposition process.Chemical vapour deposition technique is mainly under the high temperature conditions using Copper Foil catalysis carbon source cracking and in copper foil surface
Reaction generation graphene film.Compared with the Graphene that oxidation-reduction method is prepared, chemical vapour deposition technique Graphene lacks
Fall into less with more perfect lattice structure, so chemical vapour deposition technique Graphene has higher quality and excellent conduction
Property.Due to the extraordinary physics of Graphene and chemical property, it is more and more in the application study of field of compound material, is especially building
Build Material Field and also obtain increasingly wider application.Research shows to change with nano material (CNT, Graphene) combination
The micro-property of cement.Introduced in cement mortar nano material can reduce porosity and hydration rate cause to produce it is stronger and more
Durable product.Specific surface area high allows nano material effectively to control the extension of the micro-crack of cement-base composite material.
General cement-based material belongs to fragile material, and its tension, rupture strength are low, and fragility is big, easy to crack.Therefore, exist
Copper facing steel fibre is mixed in cement-based material can strengthen toughening cement, so as to improve the resistance to crack extension ability of cement-based material
And durability.But Presence of an interface combines the problems such as being easy to corrosion again when copper facing steel fibre is with cement-based material combination simultaneously, so
Using chemical vapour deposition technique these problems can be effectively improved in the graphene coated film that copper facing steel fiber surface grows.
The present invention with copper facing steel fibre as substrate, by chemical vapour deposition technique in its superficial growth graphene coated film,
Intensity and corrosion resistance of the copper facing steel fibre in cement-base composite material can be effectively improved, it is possible to anti-as hydrated cementitious
So as to advantageously facilitate hydrated reaction of cement, the structure for making cement form densification finally effectively prevents the product of crackle to the forming core point answered
The raw intensity for improving cement-base composite material.Had broad application prospects in cement-base composite material field.
The content of the invention
Goal of the invention：Steel fibre and cement-base composite material interface can be effectively solved it is an object of the invention to provide one kind
With reference to problem and the method that improves material fragility and corrosion resistance.The method is using chemical vapour deposition technique in copper facing steel fibre table
Graphene coating film long of looking unfamiliar can improve the extension of the micro-crack of cement-based material so as to improve cement-base composite material
Toughness.
Technical scheme：To realize above-mentioned purpose, one kind of the invention is in copper facing steel fiber surface controllable growth Graphene
The technical scheme that the method for coating film is used for：
The hanging annealing for being put into quartz ampoule and a period of time being carried out in tube furnace after copper facing steel fibre is cleaned with water,
Carrier gas and carbon-source gas are passed through in tube furnace afterwards stone is grown in copper facing steel fiber surface by aumospheric pressure cvd method
Black alkene；
Wherein：
The length of the copper facing steel fibre is 1-13mm, a diameter of 0.1-0.5mm.
Described carrier gas is argon gas and hydrogen, and carbon-source gas are methane.
Described aumospheric pressure cvd method includes following four process：
1) temperature-rise period：The started temperature of temperature rise period is room temperature, and heating rate is 10 DEG C/min, and end temp is 900-
1050 DEG C, the flow of argon gas and hydrogen is respectively 100-200sccm and 20-50sccm；
2) temperature of annealing stage is 900-1050 DEG C, and the time is 20-30min, and the flow of argon gas and hydrogen is respectively
100-200sccm and 20-50sccm.
3) temperature of growth phase is 900-1050 DEG C, and the time is 10-20min, argon gas, hydrogen, the flow difference of methane
It is 200-300sccm, 40-100sccm, 4-10sccm.
4) rate of temperature fall of temperature-fall period is 20 DEG C/min, and the flow of argon gas and hydrogen is respectively 100-200sccm and 20-
50sccm。
Compared with other methods for preparing Graphene, the Graphene good crystallinity of chemical vapour deposition technique preparation, quality are high
With less fault of construction such that it is able to effectively reduce concrete base material to the corrosiveness of copper facing steel fibre, stone is improve
The durability of the copper facing steel fibre of black alkene cladding.Simultaneously as the graphene coated film of chemical vapor deposition and copper facing steel fibre
Adhesion between the Copper Foil on surface is higher, it is possible to prevente effectively from the copper plated steel of cement-based material and non-deposited graphite alkene clad
The weak problem of interface cohesion existed between fiber.
Beneficial effect：Copper facing steel fibre can be effectively improved by the synergy of Graphene and steel fibre multiple in cement base
Intensity and corrosion resistance in condensation material, it is possible to as the forming core point of hydrated reaction of cement so as to advantageously facilitate hydrated cementitious
Reaction, the structure for making cement form densification finally effectively prevents the generation of crackle from improving the intensity of cement-base composite material.In water
Cement-based composite material field has broad application prospects.With traditional copper facing steel fiber reinforced cement base graphite alkene composite
Compare, high-quality graphene clad prepared by the present invention has the physicochemical properties of stabilization such that it is able to further improve plating
Corrosion resistance of the copper steel fiber in cement material, while graphene coated layer is used as reinforcing fiber and the interfaces transition of cement matrix
Material improves interface stability and interface binding power, so as to suppressing the generation of micro-crack in cement material and expanding.Therefore,
The intensity and toughness of cement-based material are obtained for raising.
Specific embodiment
A. the cleaning of copper facing steel fibre：
Copper facing steel fibre is first cleaned by ultrasonic 5-15min with acetone, 5-15min is then cleaned with EtOH Sonicate, then spend
Ionized water is cleaned by ultrasonic 10-20min, the copper facing steel fibre drying for completing will be finally cleaned with nitrogen standby；
B. the preparation of copper facing steel fiber surface Graphene：
Standby copper facing steel fibre will be dried up vacantly to be put into quartz ampoule, vavuum pump is opened and vacuum is down to 5-15Pa and use again
Argon gas is backfilled to normal pressure.Begun to warm up after setting heating schedule.Heating process is divided into following four successive stages:
1) started temperature of temperature rise period is room temperature, and heating rate is 10 DEG C/min, and end temp is 900-1050 DEG C, argon
The flow of gas and hydrogen is respectively 100-200sccm and 20-50sccm.
2) temperature of annealing stage is 900-1050 DEG C, and the time is 20-30min, and the flow of argon gas and hydrogen is respectively
100-200sccm and 20-50sccm.
3) temperature of growth phase is 900-1050 DEG C, and the time is 10-20min, argon gas, hydrogen, the flow difference of methane
It is 200-300sccm, 40-100sccm, 4-10sccm.
4) rate of temperature fall of temperature-fall period is 20 DEG C/min, and the flow of argon gas and hydrogen is respectively 100-200sccm and 20-
50sccm。
Temperature-fall period takes out the copper facing steel fibre for preparing and completing after terminating, and completes whole preparation process.
Embodiment 1：
1) copper facing steel fibre is put into the acetone beaker for fill 5-20ml and is cleaned by ultrasonic 5-15min, afterwards by copper plated steel
Fiber is picked up to be put into ethanol from acetone and is cleaned by ultrasonic 5-15min, copper facing steel fibre is picked up and is put into ultrasound in deionized water
Cleaning 10-20min, is finally dried up standby with nitrogen.
2) the copper facing steel fibre of drying is put into quartz boat, copper facing steel fibre and quartz boat are loaded into gas phase afterwards sinks
In the quartz ampoule of product system, flange sealed silica envelope is used afterwards, vavuum pump is opened afterwards the vacuum in quartz ampoule is extracted into 5-
15Pa, is finally backfilled to normal pressure using argon gas by quartz ampoule.
3) quartz ampoule begins to warm up process after being backfilled to normal pressure.First, quartz ampoule is added with the firing rate of 10 DEG C/min
Heat keeps flow respectively 100sccm, 20sccm. of argon gas and hydrogen during this to 900 DEG C
4) temperature starts annealing process after reaching 900 DEG C, keeps 20min to complete annealing process, to remove copper facing steel fibre
The oxide on surface, the flow of argon gas and hydrogen is respectively 100sccm, 20sccm in annealing process.
5) growth course is started after annealing process terminates, 900 DEG C of temperature holding is constant in growth course, and growth time is
10min, argon gas, hydrogen, the gas flow of methane are respectively 200sccm, 40sccm, 4sccm in growth course.
6) after growth course terminates, quartz ampoule is cooled to room temperature with the speed of 20 DEG C/min, the argon gas in temperature-fall period and
The flow of hydrogen is respectively 100sccm, 20sccm.Cooling is taken out copper facing steel fibre and completes its surface stone after terminating from quartz ampoule
The preparation of black alkene.
Embodiment 2：
1) the step of is same as embodiment 1 1).
2) the step of is same as embodiment 1 2).
3) quartz ampoules begin to warm up process after being backfilled to normal pressure.First, quartz ampoule is added with the firing rate of 10 DEG C/min
Heat keeps flow respectively 150sccm, 30sccm. of argon gas and hydrogen during this to 1000 DEG C
4) temperature starts annealing process after reaching 1000 DEG C, keeps 24min to complete annealing process, fine to remove copper plated steel
The oxide in dimension table face, the flow of argon gas and hydrogen is respectively 150sccm, 30sccm in annealing process.
5) annealing processes start growth course after terminating.1000 DEG C of temperature holding is constant in growth course, and growth time is
14min, argon gas, hydrogen, the gas flow of methane are respectively 240sccm, 50sccm, 5sccm in growth course.
6) after growth courses terminate, heating terminates, and quartz ampoule is cooled to room temperature, temperature-fall period with the speed of 20 DEG C/min
In argon gas and the flow of hydrogen be respectively 150sccm, 30sccm.It is complete that cooling takes out copper facing steel fibre after terminating from quartz ampoule
Into the preparation of its surface Graphene.
Embodiment 3：
1) the step of is same as embodiment 1 1).
2) the step of is same as embodiment 1 2).
3) quartz ampoules begin to warm up process after being backfilled to normal pressure.First, quartz ampoule is added with the firing rate of 10 DEG C/min
Heat keeps flow respectively 180sccm, 40sccm. of argon gas and hydrogen during this to 1020 DEG C
4) temperature starts annealing process after reaching 1020 DEG C, keeps 28min to complete annealing process, fine to remove copper plated steel
The oxide in dimension table face, the flow of argon gas and hydrogen is respectively 180sccm, 40sccm in annealing process.
5) annealing processes start growth course after terminating.1020 DEG C of temperature holding is constant in growth course, and growth time is
18min, argon gas, hydrogen, the gas flow of methane are respectively 280sccm, 80sccm, 8sccm in growth course.
6) after growth courses terminate, heating terminates, and quartz ampoule is cooled to room temperature, temperature-fall period with the speed of 20 DEG C/min
In argon gas and the flow of hydrogen be respectively 180sccm, 40sccm.It is complete that cooling takes out copper facing steel fibre after terminating from quartz ampoule
Into the preparation of its surface Graphene.
Embodiment 4：
1) the step of is same as embodiment 1 1).
2) the step of is same as embodiment 1 2).
3) quartz ampoules begin to warm up process after being backfilled to normal pressure.First, quartz ampoule is added with the firing rate of 10 DEG C/min
Heat keeps flow respectively 200sccm, 50sccm. of argon gas and hydrogen during this to 1050 DEG C
4) temperature starts annealing process after reaching 1050 DEG C, keeps 30min to complete annealing process, fine to remove copper plated steel
The oxide in dimension table face, the flow of argon gas and hydrogen is respectively 200sccm, 50sccm in annealing process.
5) annealing processes start growth course after terminating.1050 DEG C of temperature holding is constant in growth course, and growth time is
20min, argon gas, hydrogen, the gas flow of methane are respectively 300sccm, 100sccm, 10sccm in growth course.
6) after growth courses terminate, heating terminates, and quartz ampoule is cooled to room temperature, temperature-fall period with the speed of 20 DEG C/min
In argon gas and the flow of hydrogen be respectively 200sccm, 50sccm.It is complete that cooling takes out copper facing steel fibre after terminating from quartz ampoule
Into the preparation of its surface Graphene.
Claims (4)
1. a kind of method in copper facing steel fiber surface controllable growth graphene coated film, it is characterised in that：By copper facing steel fibre
With the hanging annealing for being put into quartz ampoule and carrying out in tube furnace a period of time after cleaning, carrier gas is passed through in tube furnace afterwards
Graphene is grown in copper facing steel fiber surface by aumospheric pressure cvd method with carbon-source gas.
2. as claimed in claim 1 in the method for copper facing steel fiber surface controllable growth graphene coated film, it is characterised in that：
The length of the copper facing steel fibre is 1-13mm, a diameter of 0.1-0.5mm.
3. as claimed in claim 1 in the method for copper facing steel fiber surface controllable growth graphene coated film, it is characterised in that：
Described carrier gas is argon gas and hydrogen, and carbon-source gas are methane.
4. as claimed in claim 1 in the method for copper facing steel fiber surface controllable growth graphene coated film, it is characterised in that：
Described aumospheric pressure cvd method includes following four process：
1) temperature-rise period：The started temperature of temperature rise period is room temperature, and heating rate is 10 DEG C/min, and end temp is 900-1050
DEG C, the flow of argon gas and hydrogen is respectively 100-200sccm and 20-50sccm；
2) temperature of annealing stage is 900-1050 DEG C, and the time is 20-30min, and the flow of argon gas and hydrogen is respectively 100-
200sccm and 20-50sccm.
3) temperature of growth phase is 900-1050 DEG C, and the time is 10-20min, and argon gas, hydrogen, the flow of methane are respectively
200-300sccm、40-100sccm、4-10sccm。
4) rate of temperature fall of temperature-fall period is 20 DEG C/min, and the flow of argon gas and hydrogen is respectively 100-200sccm and 20-
50sccm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381556A (en) * | 2017-08-08 | 2017-11-24 | 东南大学 | A kind of no metal catalytic is quickly in the method for glass surface deposited graphite alkene |
| CN108128792A (en) * | 2017-11-29 | 2018-06-08 | 温州医科大学 | A kind of preparation method of the electrically conductive rare-earth oxide sulfate micron tube of cerium dopping and application |
| CN109763320A (en) * | 2018-12-24 | 2019-05-17 | 西安交通大学 | A kind of technique that graphene film repairs carbon fiber surface hole and crackle |
| CN112960927A (en) * | 2021-01-25 | 2021-06-15 | 哈尔滨工业大学（深圳） | Nano material adsorption steel fiber and preparation method and application thereof |
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