CN109385551A - A kind of coated with titanium oxide/graphene oxide enhancing preparation method for material of substrate containing magnalium - Google Patents
A kind of coated with titanium oxide/graphene oxide enhancing preparation method for material of substrate containing magnalium Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
Abstract
A kind of coated with titanium oxide/graphene oxide enhancing preparation method for material of substrate containing magnalium, by adsorbing Ti ion using hydro-thermal high pressure, and in the case where graphene oxide carries functional group's effect, and obtain anatase titanium dioxide GO TiO2 in after baking in water-less environment.Gained powder mixes ultrasound and ball milling with magnesium powder.And mixing cold pressing hot extrusion is obtained into interphase, it is then imported in melt in ultrasound environments, melt temperature control is near liquidus curve and ultrasonic.Gained compounding flux imports in the precoated sand mold after preheating, then carries out ultrasound until solidification.Gained blank variable conduit moulding hot extrusion obtains after rodlike blank to isometrical angle repeatedly squeezes again again, obtains coated with titanium oxide/graphene oxide enhancing based composites containing magnalium.Aluminum matrix composite technology of preparing handled by the present invention has simple, safety, low cost.Gained Mg17Al12 phase and crystal grain are tiny, and graphene oxide in multiple extruding dispersion distribution preferably, simultaneously as coat there are the wetabilitys of GO to be improved so that it is preferable with matrix ining conjunction with.
Description
Technical field
The invention belongs to technical field of material.
Background technique
The two-dimensional material for the monoatomic layer thickness that graphene nanometer sheet is made of sp2 hydbridized carbon atoms, shows one
The unusual physical property of series.Graphene nanometer sheet causes physics, chemistry and materialogy because of its special two-dimensional structure
The great interest of boundary researcher, basic research and engineering Application Research in relation to graphene become research hotspot in recent years.
Since graphene has high intensity, tensile strength up to 130GPa, imply graphene have in material application study it is huge
Big application space.
Mg-based material, especially magnesium alloy have many advantages, such as that density is small, and light weight, intensity are big and damping performance is strong, extensively
It is applied in the traffic transport industries such as aviation and automobile generally.The alloy is a kind of typical eutectic alloy, it has preferable
Casting character, while have both again specific strength height, it is cheap the advantages that.Under normal conditions, the Mg in alloy17Al12Easily present
Chinampa type or coarse bulk out, this is easy to isolate matrix in loading process, seriously affects the mechanical property of matrix, thus right
In one of the research emphasis that the refinement of the phase is magnesium alloy.On the other hand, using carbon material such as carbon nanotube or graphene come
Enhance the research of the intensity and other mechanical properties of metal_based material as current research hot topic, and achieves a degree of
Progress.The applied defect of right graphene oxide (GO) in a metal is also more obvious.Graphene oxide shows very poor wetting
Property, this directly results in not strong with metal interface associativity, is unfavorable for the preparation of composite material.Thus, improve itself and matrix
Wetability simultaneously selects correct process to become the key using graphene enhancing alumina-base material abrasion.
Graphene, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method is mainly by carboxylated
Graphene through sensitization plays, after activation, plating in chemical plating fluid is put into, as the progress of reaction can be in carboxylated graphene surface
Graininess coating is obtained, but expensive, and commonly use toxic reagent, not environmentally and high production cost, is not suitable for extensive raw
It produces.
The control of carbon material dispersibility is usually embodied in made of metal for during.Currently, passing through in-situ synthesis and powder
It is relatively conventional that metallurgy method prepares carbon material aluminum matrix composite.However the defect of these types of method is also it is clear that powder smelting
Gold is popular research direction, but interface cohesion and compactness problem fail effectively to be solved.There are techniques for in-situ synthesis
Excessively complicated and process such as is difficult to control at the short slabs.And the dispersion of paddling process is not solved effectively.
It is 108060321A in publication number, in a kind of entitled preparation method of graphene reinforced aluminum matrix composites,
Promote the dispersion of graphene using semi-solid casting combination extrusion, and is prepared for graphene reinforced aluminum matrix composites.
However the method not can effectively improve the Problem of Wettability of graphene and easily occur graphene in process of setting and reunites again
Problem etc., thus quality is not able to maintain preferable consistency.
It is 107058786A in publication number, in a kind of entitled preparation method of magnesium-based graphene composite material, uses
Interphase briquetting adds the method for ultrasonic founding to prepare graphene mg-based material, however the wetting of this method and unresolved graphene
The agglomeration traits again of property problem and graphene in casting process.It is also not directed to Mg simultaneously17Al12Refinement the problems such as.
In publication 106702193A, entitled " a kind of preparation method of graphene/aluminum composite material ", use
The conventional powder metallurgicals methods such as mixing, drying, ball milling, cold pressing, sintering and extruding are prepared for graphene enhancing aluminum-base composite material
Material, though improving to wetability, the problems such as right material is not directed to melting, the compactness of itself, is still more prominent.
Therefore, in conclusion still lacking a kind of cost-effective graphene enhancing magnesium-aluminium alloy material preparation skill at present
Art.
Summary of the invention
The object of the present invention is to provide a kind of technologies of preparing of new reinforced Si phase magnesium alloy materials.It is in magnesium alloy
Addition coating TiO in material2Graphene oxide, due to there is coat, wetability is changed graphene oxide after processing
It is kind.Continual ultrasonic is in process of setting to solve reuniting in process of setting again.The method of the secondary hot extrusion of later-stage utilization is to oxidation
Graphene disperses again, to reach dispersion reinforced phase and refine Mg simultaneously17Al12The purpose of phase.It is compared to traditional founding or pressure
Power casting, it has many advantages, such as, such as the basis material range of choice being applicable in is wide, customization performance is strong, excellent bonding performance.Separately
Outside, from current experiment result it is found that due to graphene oxide excellent thermal conductivity so that the Mg in process of setting17Al12Mutually heat
Amount can comparatively fast be spread out of, and increase degree of supercooling, thus may make Mg by the graphene that the method is added17Al12It mutually obtains to a certain extent
Refinement, and be crushed in extrusion process, rounding, dispersion.
The present invention is achieved by the following technical solutions.
A kind of method of titanium-oxide-coated graphene oxide enhancing enhancing magnalium based composites of the present invention, including
Following steps.
(1) by graphene oxide in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is anhydrous
Vapour.The proportion of graphene oxide and ethyl alcohol is 0.2 ~ 0.4g: 50ml.
(2) by step (1) pretreated graphene oxide dispersion pour into glycerine and tetraisopropyl titanate composition
It is sealed in precursor liquid, and is ultrasonically treated 1 ~ 1.5h again.Among these, glycerine and tetraisopropyl titanate volume ratio be 10:0.4 ~
1.2。
(3) forerunner's suspension of step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
35%~70%.Reaction kettle is integrally put into reacting furnace again and is heated, is warming up to 70~110 DEG C with 1~5 DEG C/min, heat preservation 1~
2h, then after being warming up to 175 ~ 180 DEG C with 1~3 DEG C/min, take out reaction kettle after keeping the temperature 10~15h；Reaction kettle should be air-cooled to room
Warm rear is openable.
(4) solution obtained by step (3) is taken out, centrifugal treating, and be repeatedly centrifuged by pouring into analysis straight alcohol to solution
Colourless, revolving speed is controlled in 9000 ~ 16000rpm.Whole process sealing guarantees without steam.
(5) the mixed-powder vacuum drying that step (4) is obtained, after will be in the powder under protection of argon gas 450 ~ 500 DEG C
Roasting.Time controls in 1 ~ 3h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
(6) mass fraction is that the graphene oxide of 4% ~ 15% titania coating of magnesium alloy powder is put into low power in methanol
Ultrasonic vibration obtains mixed powder suspension, the time no more than 30min, after be dried in vacuum drying box.
(7) mixing that step (6) obtains is imported ball milling crucible and carries out ball milling, argon gas progress is passed through in the mechanical milling process
Protection, revolving speed control are 300 ~ 350rpm.
(8) by mixing cold pressing treatment obtained by step (7), obtain pole shape embryo material, after by the blank in 100 ~ 150 DEG C of temperature
Hot extrusion in, extrusion ratio control are 32 ~ 45, and chopping is that the graphene oxide that height is 5mm or so is pre- after obtaining rodlike blank
Body processed is spare.
(9) corresponding magnalium sill is melted in muffle furnace, after be transferred to self-control in the crucible of bottom ultrasonic device
Constant temperature processing, temperature are controlled near liquidus curve, and ultrasonic power control is 0.7 ~ 2.1Kw.Temperature is controlled in the liquid of corresponding alloy
Near phase line, and different direction is divided to import in melt precast body obtained by step (8) in 0.7 ~ 1.0g/min speed, whole argon gas
Protection.
(10) melt obtained by step (9) is imported it is cooling in precoated sand mold groove, among these, mold is preheated to 150 ~
250 DEG C, and in melt importing process the processing of mold same continual ultrasonic until melt solidifies, ultrasonic power control 0.7 ~
2.8Kw, the process must be imported with argon gas side to prevent from burning.
(11) moulding mixture obtained by step (10) is carried out the processing of variable conduit plasticity hot extrusion, temperature control is 150 ~ 200 DEG C, pressure head
Control is controlled in 0.4 ~ 1.2mm/s rate, extrusion ratio 11 ~ 32.
(12) bar obtained by step (11) is carried out isometrical angle hot extrusion, number is 2 ~ 8 times, and temperature control is 100 ~ 250
DEG C, pressure head is controlled in 0.2 ~ 1.5mm/s rate, and corner is controllable to 90 ~ 150 °.
Hydrothermal reaction kettle liner described in step (3) of the present invention is polytetrafluoroethylene (PTFE).
The present invention has following technical effect that (1) solution uses ethyl alcohol rather than water, participates in reaction itself and increase to wave
Hair property, pressure is bigger, beneficial to the surface tension for reducing solution.(2) this method is simple and effective is suitable for batch production.(3) should
Method is not required to expensive instrument, and reaction temperature is lower, and danger coefficient is low.(4) graphene oxide is in aluminum alloy materials process of setting
The effect lasts dispersion of ultrasound, has better interface simultaneously, avoids the reunion of graphene oxide under the conditions of founding.(5) oxygen
Particularity of the graphite alkene due to its structure, it is extremely difficult to disperse, during secondary extrusion, fault in material is reduced, graphene oxide
Dispersed again in extrusion process, meanwhile, Mg17Al12It is mutually also preferably refined and rounding, crystal grain itself also obtains
Preferable refinement.(6) graphene oxide carries functional group using surface and adsorbs Ti ion and during the vacuum baking in later period
Form TiO2Coat effectively improves the wetability and associativity of graphene oxide in the base.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
By graphene oxide in the analysis straight alcohol clock pre-dispersed 1h of ultrasound, temperature is room temperature, and whole-process control is without steam.Volume
Than being strict controlled in 0.2:50, after that gained dispersion liquid poured into sealing in the precursor liquid of glycerine and tetraisopropyl titanate composition is super
Sonication 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein suspended
Liquid product accounts for the molten product 50% of reaction kettle.Place into reacting furnace and heat, be warming up to 90 DEG C with 5 DEG C/min, keep the temperature 2h, then with 3 DEG C/
After min is warming up to 180 DEG C, 10h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into point
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It afterwards will be in gained powder under protection of argon gas 450 DEG C
Roasting.Time controls in 2h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
AM60 magnalium material is melted in muffle furnace, after be transferred to self-control in the crucible of bottom ultrasonic device at constant temperature
Reason.Temperature is controlled in 650 DEG C, and the intermediate alloy for being squeezed into gained graphene oxide and magnesium powder in 0.7g/min speed divides not
It is imported in melt with orientation, whole argon gas protection, ultrasound is controlled in 0.7Kw.Resulting materials import corresponding precoated sand mold groove
Middle cooling, among these, mold are preheated to 150 DEG C, and the same continual ultrasonic of mold is handled until melt in melt importing process
Solidification.Gained moulding mixture is subjected to secondary hot extrusion processing afterwards, temperature control is 200 DEG C, and pressure head control is squeezed in 0.4mm/s rate
Than control 45, after carry out 3 Equal Channel Angular Pressings again under the conditions of 100 DEG C, corner control is 130 °.
Embodiment 2.
By graphene oxide in the analysis straight alcohol clock pre-dispersed 3h of ultrasound, temperature is room temperature, and whole-process control is without steam.Volume
Than being strict controlled in 0.2:50, after that gained dispersion liquid poured into sealing in the precursor liquid of glycerine and tetraisopropyl titanate composition is super
Sonication 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.8.Hydro-thermal process is carried out later, wherein suspended
Liquid product accounts for the molten product 50% of reaction kettle.Place into reacting furnace and heat, be warming up to 90 DEG C with 3 DEG C/min, keep the temperature 1h, then with 2 DEG C/
After min is warming up to 180 DEG C, 12h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into point
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It afterwards will be in gained powder under protection of argon gas 450 DEG C
Roasting.Time controls in 1h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
AZ61 magnalium material is melted in muffle furnace, after be transferred to self-control in the crucible of bottom ultrasonic device at constant temperature
Reason.Temperature is controlled in 660 DEG C, and the intermediate alloy being squeezed into gained graphene oxide and magnesium powder in 1g/min speed not Tongfang
Position imports in melt, and whole argon gas protection, ultrasound is controlled in 1.4Kw.Resulting materials import cold in corresponding precoated sand mold groove
But, among these, mold is preheated to 150 DEG C, and the same continual ultrasonic of mold is handled up to melt solidification in melt importing process,
Ultrasound is controlled in 1.4Kw.Gained moulding mixture is subjected to secondary hot extrusion processing afterwards, temperature control is 150 DEG C, and pressure head is controlled in 0.7mm/
S rate, extrusion ratio control 11, after carry out 3 Equal Channel Angular Pressings again under the conditions of 230 DEG C, corner control is 100 °.
Embodiment 3.
By graphene oxide in the analysis straight alcohol clock pre-dispersed 2h of ultrasound, temperature is room temperature, and whole-process control is without steam.Volume
Than being strict controlled in 0.4:50, after that gained dispersion liquid poured into sealing in the precursor liquid of glycerine and tetraisopropyl titanate composition is super
Sonication 1h.Among these, glycerine and tetraisopropyl titanate volume ratio are 10:0.4.Hydro-thermal process is carried out later, wherein suspended
Liquid product accounts for the molten product 60% of reaction kettle.Place into reacting furnace and heat, be warming up to 100 DEG C with 1 DEG C/min, keep the temperature 2h, then with 3 DEG C/
After min is warming up to 180 DEG C, 10h is kept the temperature.It is air-cooled after taking-up reaction kettle.Gained solution takes out, centrifugal treating, and by pouring into point
Analysis straight alcohol is repeatedly centrifuged colourless to solution.Whole process sealing guarantees without steam.It afterwards will be in gained powder under protection of argon gas 500 DEG C
Roasting.Time controls in 1h.The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained.
AZ91D magnalium material is melted in muffle furnace, after be transferred to self-control with bottom ultrasonic device crucible in constant temperature
Processing.Temperature is controlled in 660 DEG C, and leads the intermediate alloy different direction that gained GO is squeezed into magnesium powder in 0.6g/min speed
Enter in molten aluminum, whole argon gas protection, ultrasound is controlled in 2.1Kw.Resulting materials import cooling in corresponding precoated sand mold groove, this
Wherein, mold is preheated to 200 DEG C, and the same continual ultrasonic processing of mold is ultrasonic up to melt solidification in melt importing process
It is controlled in 2.1Kw.Gained moulding mixture is subjected to secondary hot extrusion processing afterwards, temperature control is 150 DEG C, and pressure head is controlled in 1mm/s rate,
Extrusion ratio control 16, after carry out 6 Equal Channel Angular Pressings again under the conditions of 200 DEG C, corner control is 90 °.
Claims (1)
1. a kind of coated with titanium oxide/graphene oxide enhances the preparation method for material of substrate containing magnalium, feature the following steps are included:
(1) by graphene oxide in analysis straight alcohol the pre-dispersed 1 ~ 3h of ultrasound, temperature is room temperature, and whole-process control is without steam, oxygen
The proportion of graphite alkene and ethyl alcohol is 0.2 ~ 0.4g: 50ml；
(2) step (1) pretreated graphene oxide dispersion is poured into the forerunner of glycerine and tetraisopropyl titanate composition
It is sealed in liquid, and is ultrasonically treated 1 ~ 1.5h again, glycerine and tetraisopropyl titanate volume ratio are 10:0.4 ~ 1.2；
(3) forerunner's suspension of step (2) is imported in hydrothermal reaction kettle, wherein suspension volume account for the molten product of reaction kettle 35%~
70%；Reaction kettle is integrally put into reacting furnace again and is heated, is warming up to 70~110 DEG C with 1~5 DEG C/min, keeps the temperature 1~2h, then with
After 1~3 DEG C/min is warming up to 175 ~ 180 DEG C, reaction kettle is taken out after keeping the temperature 10~15h, reaction kettle is air-cooled to room temperature；
(4) solution obtained by step (3) is taken out, centrifugal treating, and by pour into analysis straight alcohol be repeatedly centrifuged it is colourless to solution,
Revolving speed control guarantees in 9000 ~ 16000rpm, whole process sealing without steam；
(5) then the mixed-powder vacuum drying that step (4) is obtained roasts in 450 ~ 500 DEG C under protection of argon gas；Time control
The graphene oxide that surface has needle-shaped anatase type titanium oxide coating can be obtained in 1 ~ 3h in system；
(6) mass fraction is that the graphene oxide of 4% ~ 15% titania coating of magnesium alloy powder is put into methanol, low power ultrasound
Concussion obtains mixed powder suspension, the time≤30min, is then dried in vacuum drying box；
(7) mixing that step (6) obtains is imported ball milling crucible and carries out ball milling, be passed through argon gas in mechanical milling process and protected,
Revolving speed control is 300 ~ 350rpm；
(8) by mixing cold pressing treatment obtained by step (7), pole shape embryo material is obtained, then the hot extrusion in 100 ~ 150 DEG C of temperature fields
Pressure, extrusion ratio control are 32 ~ 45, and chopping is that the graphene oxide precast body that height is 5mm or so is spare after obtaining rodlike blank；
(9) corresponding magnalium sill is melted in muffle furnace, after be transferred to self-control with constant temperature in the crucible of bottom ultrasonic device
Processing, temperature are controlled near liquidus curve, and ultrasonic power control is 0.7 ~ 2.1Kw, and temperature is controlled in the liquidus curve of corresponding alloy
Near, and dividing different direction to import in melt precast body obtained by step (8) in 0.7 ~ 1.0g/min speed, whole argon gas is protected
Shield；
(10) melt obtained by step (9) is imported cooling in precoated sand mold groove, mold is preheated to 150 ~ 250 DEG C, and molten
Until melt solidifies, ultrasonic power is controlled in 0.7 ~ 2.8Kw, with argon gas side the same continual ultrasonic processing of mold in body importing process
Face is imported with anti-burning；
(11) moulding mixture obtained by step (10) is carried out the processing of variable conduit plasticity hot extrusion, temperature control is 150 ~ 200 DEG C, pressure head control
In 0.4 ~ 1.2mm/s rate, extrusion ratio is controlled 11 ~ 32；
(12) bar obtained by step (11) is carried out isometrical angle hot extrusion, number is 2 ~ 8 times, and temperature control is 100 ~ 250 DEG C, pressure
In 0.2 ~ 1.5mm/s rate, corner is controllable to 90 ~ 150 ° for head control；
Hydrothermal reaction kettle liner described in step (3) is polytetrafluoroethylene (PTFE).
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| CN111363942A (en) * | 2020-02-27 | 2020-07-03 | 南昌航空大学 | Preparation method of rare earth oxide @ graphene nanosheet/aluminum-based blank |
| CN115491659A (en) * | 2022-11-01 | 2022-12-20 | 西北工业大学 | Method for improving mechanical property of metal-based composite material by modifying graphene on surface of titanium dioxide |
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| CN111020327A (en) * | 2019-11-25 | 2020-04-17 | 温州广立生物医药科技有限公司 | Tissue-regenerating absorbable magnesium alloy and preparation method thereof |
| CN111363942A (en) * | 2020-02-27 | 2020-07-03 | 南昌航空大学 | Preparation method of rare earth oxide @ graphene nanosheet/aluminum-based blank |
| CN115491659A (en) * | 2022-11-01 | 2022-12-20 | 西北工业大学 | Method for improving mechanical property of metal-based composite material by modifying graphene on surface of titanium dioxide |
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