CN103773980A - Preparation method of high-performance graphene nanosheet reinforced magnesium matrix composite - Google Patents
Preparation method of high-performance graphene nanosheet reinforced magnesium matrix composite Download PDFInfo
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- CN103773980A CN103773980A CN201410076577.0A CN201410076577A CN103773980A CN 103773980 A CN103773980 A CN 103773980A CN 201410076577 A CN201410076577 A CN 201410076577A CN 103773980 A CN103773980 A CN 103773980A
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Abstract
The invention discloses a preparation method of a high-performance graphene nanosheet reinforced magnesium matrix composite, relates to a preparation method of a graphene nanosheet reinforced magnesium matrix composite, and aims at solving the problems that a graphene nanosheet has relatively low wettability and is not uniformly dispersed in a matrix metal. The method comprises the following steps: (I) mixing and ball-milling the graphene nanosheet and Zn powder; (II) adding the composite powder into an Mg-Zn alloy melt; (III) performing ultrasonic treatment; (IV) pouring and solidifying. According to the method disclosed by the invention, the preparation process of the composite is simple and feasible, the mechanical properties of the prepared composite are remarkably improved, and the graphene nanosheet has good wettability and is uniformly dispersed in the matrix metal. The method disclosed by the invention is applied to preparation of a high-performance graphene nanosheet reinforced magnesium matrix composite.
Description
Technical field
The present invention relates to the preparation method that a kind of graphene nanometer sheet strengthens magnesium base composite material, belong to Nano-composite materials technical field.
Background technology
Graphene (Graphene) be a kind of by carbon atom with sp
2hybridized orbital composition hexangle type is the flat film of honeycomb lattice, is the two-dimensional material of only having a carbon atom thickness.Graphene is considered to hypothetical structure always, stable existence separately, until 2004, the physicist A.K.Geim of Univ Manchester UK and K.S.Novoselov successfully isolate Graphene by experiment from graphite, and confirm that it can Individual existence, two people also serve as reasons because of " in the initiative experiment of two-dimentional grapheme material ", jointly obtain Nobel Prize in physics in 2010.
Graphene be at present the thinnest be in the world the hardest nano material also, higher than carbon nanotube and diamond, taller 200 times of its strength ratio iron and steel, has the tensile modulus (rigidity) of 1TPa.Under normal temperature, its electronic mobility exceedes 15000cm
2/ Vs, and resistivity only approximately 10
-6Ω cm is the material of current known resistivity minimum.Another characteristic of Graphene is to observe at normal temperatures quantum hall effect.Graphene nanometer sheet (Graphene nanoplates, Gnp) refers to that carbon-coating number is more than 10 layers, the ultra-thin Graphene stratiform accumulation body of thickness within the scope of 5-100nm.Graphene nanometer sheet has kept the original planar carbon six-ring of graphite conjugation crystalline structure, has excellent physical strength, conduction, heat conductivility, and good lubricated, high temperature resistant and anticorrosion properties.With respect to common graphite, the thickness of graphene nanometer sheet is within the scope of nanoscale, can be used as the reinforcement of nano metal based composites.
But, because the wettability of graphene nanometer sheet and magnesium alloy is bad, and its nano level size also makes to produce powerful Van der Waals force and very easily reunion between graphene nanometer sheet, this all makes the reinforced effects of graphene nanometer sheet in matrix material not bring into play completely, so how to make graphene nanometer sheet soak the good and dispersed key that success is prepared nano Mg base composite material that becomes in matrix metal.
Summary of the invention
The object of the invention is in order to solve graphene nanometer sheet wettability in matrix metal poorly and disperse inhomogeneous problem, provide high-performance graphene nanometer sheet to strengthen the preparation method of magnesium base composite material.
The preparation method that high-performance graphene nanometer sheet of the present invention strengthens magnesium base composite material, realizes by following steps:
One, graphene nanometer sheet and Zn powder are mixed, ball milling 6h～12h under the rotating speed of 250r/min～450r/min, obtains Gnp@Zn composite powder, and wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 10～15: 1;
Two, composite powder step 1 being obtained joins in Mg-Zn alloy melt, at 530 ℃～630 ℃, stir 10min～20min, wherein in Mg-Zn alloy melt, the massfraction of Zn is that the massfraction of 2%～6%, Gnp in mixed alloy melt is 0.3%～3%;
Three, step 2 is obtained to mixed alloy melt and be warmed up to 650 ℃～750 ℃, then carry out supersound process, ultrasonic power is 500w～800w, and ultrasonic time is 5min～10min;
Four, the blend melt after step 3 supersound process being poured into temperature is in the mould of 300 ℃～500 ℃, and at the Under Pressure Solidification of 100MPa～150MPa, obtains high-performance graphene nanometer sheet and strengthen magnesium base composite material.
Beneficial effect of the present invention:
The present invention compared with prior art, its advantage is to pass through Zn powder and graphene nanometer sheet sheet mixing and ball milling in advance, can effectively disperse the graphene nanometer sheet of reuniting and make Gnp be dispersed in uniformly the surface of Zn powder, finally stir composite ultraphonic ripple legal system for matrix material, by the effect of high-energy ultrasound, can effectively solve the poor and Gnp of magnesium alloy fused mass and Gnp wettability and be difficult for the difficulty of disperseing, fully play the reinforced effects of Gnp, make the nano Mg base composite material of good mechanical properties.
The technique that the present invention prepares matrix material is simple, feasible, and the composite materials property of preparation has significantly and to improve, and graphene nanometer sheet wettability in matrix metal is good and be uniformly dispersed, and can be used for structured material.
Accompanying drawing explanation
Fig. 1 is the SEM figure that the high-performance graphene nanometer sheet prepared of embodiment mono-strengthens magnesium base composite material;
Fig. 2 is the SEM figure that the high-performance graphene nanometer sheet prepared of embodiment bis-strengthens magnesium base composite material;
Fig. 3 is the SEM figure that the high-performance graphene nanometer sheet prepared of embodiment tri-strengthens magnesium base composite material.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment high-performance graphene nanometer sheet strengthens the preparation method of magnesium base composite material, carries out according to the following steps:
One, graphene nanometer sheet and Zn powder are mixed, ball milling 6h～12h under the rotating speed of 250r/min～450r/min, obtains Gnp@Zn composite powder, and wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 10～15: 1;
Two, composite powder step 1 being obtained joins in Mg-Zn alloy melt, at 530 ℃～630 ℃, stir 10min～20min, wherein in Mg-Zn alloy melt, the massfraction of Zn is that the massfraction of 2%～6%, Gnp in mixed alloy melt is 0.3%～3%;
Three, step 2 is obtained to mixed alloy melt and be warmed up to 650 ℃～750 ℃, then carry out supersound process, ultrasonic power is 500w～800w, and ultrasonic time is 5min～10min;
Four, the blend melt after step 3 supersound process being poured into temperature is in the mould of 300 ℃～500 ℃, and at the Under Pressure Solidification of 100MPa～150MPa, obtains high-performance graphene nanometer sheet and strengthen magnesium base composite material.
The beneficial effect of present embodiment:
Present embodiment compared with prior art, its advantage is to pass through Zn powder and graphene nanometer sheet sheet mixing and ball milling in advance, can effectively disperse the graphene nanometer sheet of reuniting and make Gnp be dispersed in uniformly the surface of Zn powder, finally stir composite ultraphonic ripple legal system for matrix material, by the effect of high-energy ultrasound, can effectively solve the poor and Gnp of magnesium alloy fused mass and Gnp wettability and be difficult for the difficulty of disperseing, fully play the reinforced effects of Gnp, make the nano Mg base composite material of good mechanical properties.
The technique that present embodiment is prepared matrix material is simple, feasible, and the composite materials property of preparation has significantly and to improve, and graphene nanometer sheet wettability in matrix metal is good and be uniformly dispersed, and can be used for structured material.
Embodiment two: present embodiment is different from embodiment one: in the Gnp@Zn composite powder described in step 1, the mass ratio of Zn powder and Gnp is 10～13.5: 1.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: the ball milling described in step 1 adopts steel ball and steel ball tank, and ball material mass ratio is 8～15: 1.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: the ball milling 8h～10h under the rotating speed of 300r/min～400r/min described in step 1.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: in the Mg-Zn alloy melt described in step 2, the massfraction of Zn is 3%～5%.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: stir 10min～20min described in step 2 at 580 ℃～600 ℃.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: the alloy melt that step 2 is obtained described in step 3 is warmed up to 650 ℃～700 ℃, then carries out supersound process.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: the supersound process described in step 3 is carried out supersound process for ultrasonic bar is stretched into 10mm～40mm under alloy melt liquid level.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight: it is in the mould of 350 ℃～450 ℃ that the blend melt by after step 3 supersound process described in step 4 is poured into temperature, and at the Under Pressure Solidification of 100MPa～120MPa.Other is identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: it is in the mould of 400 ℃ that the blend melt by after step 3 supersound process described in step 4 is poured into temperature, and at the Under Pressure Solidification of 100MPa.Other is identical with one of embodiment one to nine.
Verify beneficial effect of the present invention by following examples:
Embodiment mono-:
The present embodiment high-performance graphene nanometer sheet strengthens the preparation method of magnesium base composite material, carries out according to the following steps:
One, graphene nanometer sheet and Zn powder are mixed, mixed powder (is disperseed at Zn powder surface uniform to graphene nanometer sheet) under the speed of 300r/min after ball milling 8h with steel ball and steel ball tank, take out for subsequent usely, wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 15: 1;
Two, composite powder step 1 being obtained joins in semi-solid magnesium-zinc alloy, at 600 ℃, mechanical stirring 10min(to Gnp is tentatively uniformly dispersed in alloy melt), obtain semi-solid alloy melt, wherein in magnesium-zinc alloy zinc massfraction be that the massfraction of 3%, Gnp in semi-solid alloy melt is 0.3%;
Three, after stirring, the semi-solid alloy melt that step 2 is obtained is warmed up to 700 ℃ to liquid, then carries out supersound process, and ultrasonic power is 500w, and ultrasonic time is 5min, promotes the dispersion of Gnp and improves Gnp and the wettability of magnesium alloy;
Four, by the liquid alloy melt cast after step 3 supersound process in being preheating to the mould of 450 ℃, and at the Under Pressure Solidification of 100MPa, obtain high-performance graphene nanometer sheet and strengthen magnesium base composite material.
The SEM that high-performance graphene nanometer sheet prepared by the present embodiment strengthens magnesium base composite material schemes as shown in Figure 1, and the larger flap that is positioned at substrate in figure is Zn powder, and being distributed on substrate Zn powder is Gnp compared with flakes.As seen from Figure 1, Gnp presents and is uniformly distributed on substrate Zn powder, has realized adding with dispersed of Gnp.
Embodiment bis-:
The present embodiment high-performance graphene nanometer sheet strengthens the preparation method of magnesium base composite material, carries out according to the following steps:
One, graphene nanometer sheet and Zn powder are mixed, mixed powder (is disperseed at Zn powder surface uniform to graphene nanometer sheet) under the speed of 350r/min after ball milling 10h with steel ball and steel ball tank, take out for subsequent usely, wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 13.5: 1;
Two, composite powder step 1 being obtained joins in semi-solid magnesium-zinc alloy, at 590 ℃, mechanical stirring 15min(to Gnp is tentatively uniformly dispersed in alloy melt), obtain semi-solid alloy melt, wherein in magnesium-zinc alloy zinc massfraction be that the massfraction of 4%, Gnp in semi-solid alloy melt is 1.2%;
Three, after stirring, the semi-solid alloy melt that step 2 is obtained is warmed up to 670 ℃ to liquid, then carries out supersound process, and ultrasonic power is 600w, and ultrasonic time is 7.5min, promotes the dispersion of Gnp and improves Gnp and the wettability of magnesium alloy;
Four, by the liquid alloy melt cast after step 3 supersound process in being preheating to the mould of 400 ℃, and at the Under Pressure Solidification of 120MPa, obtain high-performance graphene nanometer sheet and strengthen magnesium base composite material.
The SEM that high-performance graphene nanometer sheet prepared by the present embodiment strengthens magnesium base composite material schemes as shown in Figure 2, and the larger flap that is positioned at substrate in figure is Zn powder, and being distributed on substrate Zn powder is Gnp compared with flakes.As seen from Figure 2, Gnp presents and is uniformly distributed on substrate Zn powder, has realized adding with dispersed of Gnp.
Embodiment tri-:
The present embodiment high-performance graphene nanometer sheet strengthens the preparation method of magnesium base composite material, carries out according to the following steps:
One, graphene nanometer sheet and Zn powder are mixed, mixed powder (is disperseed at Zn powder surface uniform to graphene nanometer sheet) under the speed of 400r/min after ball milling 12h with steel ball and steel ball tank, take out for subsequent usely, wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 10: 1;
Two, composite powder step 1 being obtained joins in semi-solid magnesium-zinc alloy, at 580 ℃, mechanical stirring 20min(to Gnp is tentatively uniformly dispersed in alloy melt), obtain semi-solid alloy melt, wherein in magnesium-zinc alloy zinc massfraction be that the massfraction of 5%, Gnp in semi-solid alloy melt is 3.0%;
Three, after stirring, the semi-solid alloy melt that step 2 is obtained is warmed up to 650 ℃ to liquid, then carries out supersound process, and ultrasonic power is 800w, and ultrasonic time is 10min, promotes the dispersion of Gnp and improves Gnp and the wettability of magnesium alloy;
Four, by the liquid alloy melt cast after step 3 supersound process in being preheating to the mould of 350 ℃, and at the Under Pressure Solidification of 150MPa, obtain high-performance graphene nanometer sheet and strengthen magnesium base composite material.
The SEM that high-performance graphene nanometer sheet prepared by the present embodiment strengthens magnesium base composite material schemes as shown in Figure 3, and the larger flap that is positioned at substrate in figure is Zn powder, and being distributed on substrate Zn powder is Gnp compared with flakes.As seen from Figure 3, Gnp presents and is uniformly distributed on substrate Zn powder, has realized adding with dispersed of Gnp.
Above embodiment shows, the Gnp of different volumes mark presents and is uniformly distributed on substrate Zn powder, has realized adding with dispersed of Gnp.
Above embodiment proves, the present invention makes Gnp distribute at Zn powder surface uniform by Zn powder and Gnp mixing and ball milling, processes and effectively solved Gnp and in matrix material, disperse difficulty inhomogeneous and that wettability is poor through stirring composite ultraphonic ripple method.
Claims (10)
1. high-performance graphene nanometer sheet strengthens the preparation method of magnesium base composite material, it is characterized in that it comprises the following steps:
One, graphene nanometer sheet and Zn powder are mixed, ball milling 6h～12h under the rotating speed of 250r/min～450r/min, obtains Gnp@Zn composite powder, and wherein in Gnp@Zn composite powder, the mass ratio of Zn powder and Gnp is 10～15: 1;
Two, composite powder step 1 being obtained joins in Mg-Zn alloy melt, at 530 ℃～630 ℃, stir 10min～20min, wherein in Mg-Zn alloy melt, the massfraction of Zn is that the massfraction of 2%～6%, Gnp in mixed alloy melt is 0.3%～3%;
Three, step 2 is obtained to mixed alloy melt and be warmed up to 650 ℃～750 ℃, then carry out supersound process, ultrasonic power is 500w～800w, and ultrasonic time is 5min～10min;
Four, the blend melt after step 3 supersound process being poured into temperature is in the mould of 300 ℃～500 ℃, and at the Under Pressure Solidification of 100MPa～150MPa, obtains high-performance graphene nanometer sheet and strengthen magnesium base composite material.
2. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that in the Gnp@Zn composite powder described in step 1, the mass ratio of Zn powder and Gnp is 10～13.5: 1.
3. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the ball milling described in step 1 adopts steel ball and steel ball tank, and ball material mass ratio is 8～15: 1.
4. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the ball milling 8h～10h under the rotating speed of 300r/min～400r/min described in step 1.
5. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, and the massfraction that it is characterized in that Zn in the Mg-Zn alloy melt described in step 2 is 3%～5%.
6. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that at 580 ℃～600 ℃, stirring 10min～20min described in step 2.
7. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the alloy melt that step 2 is obtained described in step 3 is warmed up to 650 ℃～700 ℃, then carries out supersound process.
8. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the supersound process described in step 3 carries out supersound process for ultrasonic bar is stretched into 10mm～40mm under alloy melt liquid level.
9. high-performance graphene nanometer sheet according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that it is in the mould of 350 ℃～450 ℃ that the blend melt by after step 3 supersound process described in step 4 is poured into temperature, and at the Under Pressure Solidification of 100MPa～120MPa.
10. high-performance graphene nanometer sheet according to claim 9 strengthens the preparation method of magnesium base composite material, it is characterized in that it is in the mould of 400 ℃ that the blend melt by after step 3 supersound process described in step 4 is poured into temperature, and at the Under Pressure Solidification of 100MPa.
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| CN105256211A (en) * | 2015-10-09 | 2016-01-20 | 天长市兴宇铸造有限公司 | Graphene modifying Mg-Al-Mn magnesium alloy material for casting automobile parts and preparation method thereof |
| CN105624457A (en) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | Graphene enhanced magnesium-based composite and preparing method thereof |
| CN106148748A (en) * | 2015-04-01 | 2016-11-23 | 贵州顶效经济开发区沈兴实业有限责任公司 | A kind of Graphene titanium alloy smelting method |
| CN106337180A (en) * | 2015-07-13 | 2017-01-18 | 中南大学 | Anti-oxidation method used for preparing magnesium alloy artificial bone by laser |
| CN107858571A (en) * | 2017-11-01 | 2018-03-30 | 内蒙古汇豪镁业有限公司 | A kind of magnesium alkene alloy preparation method |
| CN109207787A (en) * | 2018-11-22 | 2019-01-15 | 哈尔滨工业大学 | A kind of preparation method of in-situ authigenic graphene enhancing magnesium-based composite material |
| CN109385551A (en) * | 2018-09-17 | 2019-02-26 | 南昌大学 | A kind of coated with titanium oxide/graphene oxide enhancing preparation method for material of substrate containing magnalium |
| JP2019506358A (en) * | 2016-02-09 | 2019-03-07 | ナノテク インストゥルメンツ, インコーポレイテッドNanotek Instruments, Inc. | Chemical-free production of graphene reinforced inorganic matrix composites |
| CN109554573A (en) * | 2019-01-18 | 2019-04-02 | 哈尔滨工业大学 | A kind of magnesium alloy preparation method of containing graphene fining agent and application |
| CN109576513A (en) * | 2018-11-02 | 2019-04-05 | 天津大学 | A kind of preparation method of high-strength and high ductility Mg-Al-Zn system magnesium alloy |
| CN111363945A (en) * | 2020-02-27 | 2020-07-03 | 南昌航空大学 | Preparation and interface optimization method of modified graphene nanosheet magnesium-aluminum material |
| CN113005313A (en) * | 2021-02-23 | 2021-06-22 | 太原理工大学 | Preparation method of configuration design pre-dispersed graphene nanosheet reinforced magnesium-based composite material |
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| CN106337180A (en) * | 2015-07-13 | 2017-01-18 | 中南大学 | Anti-oxidation method used for preparing magnesium alloy artificial bone by laser |
| CN106337180B (en) * | 2015-07-13 | 2019-01-01 | 中南大学 | A kind of anti-oxidation method preparing magnesium alloy artificial bone for laser |
| CN105256211A (en) * | 2015-10-09 | 2016-01-20 | 天长市兴宇铸造有限公司 | Graphene modifying Mg-Al-Mn magnesium alloy material for casting automobile parts and preparation method thereof |
| JP2019506358A (en) * | 2016-02-09 | 2019-03-07 | ナノテク インストゥルメンツ, インコーポレイテッドNanotek Instruments, Inc. | Chemical-free production of graphene reinforced inorganic matrix composites |
| JP6998879B2 (en) | 2016-02-09 | 2022-02-10 | ナノテク インストゥルメンツ，インコーポレイテッド | Chemical-free production of graphene-reinforced inorganic matrix composites |
| CN105624457A (en) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | Graphene enhanced magnesium-based composite and preparing method thereof |
| CN105624457B (en) * | 2016-03-22 | 2017-08-04 | 北京工业大学 | Graphene enhancing magnesium-based composite material and preparation method thereof |
| CN107858571A (en) * | 2017-11-01 | 2018-03-30 | 内蒙古汇豪镁业有限公司 | A kind of magnesium alkene alloy preparation method |
| CN109385551A (en) * | 2018-09-17 | 2019-02-26 | 南昌大学 | A kind of coated with titanium oxide/graphene oxide enhancing preparation method for material of substrate containing magnalium |
| CN109576513A (en) * | 2018-11-02 | 2019-04-05 | 天津大学 | A kind of preparation method of high-strength and high ductility Mg-Al-Zn system magnesium alloy |
| CN109207787B (en) * | 2018-11-22 | 2020-08-11 | 哈尔滨工业大学 | Preparation method of in-situ synthesized graphene reinforced magnesium-based composite material |
| CN109207787A (en) * | 2018-11-22 | 2019-01-15 | 哈尔滨工业大学 | A kind of preparation method of in-situ authigenic graphene enhancing magnesium-based composite material |
| CN109554573A (en) * | 2019-01-18 | 2019-04-02 | 哈尔滨工业大学 | A kind of magnesium alloy preparation method of containing graphene fining agent and application |
| CN109554573B (en) * | 2019-01-18 | 2021-05-04 | 哈尔滨工业大学 | Preparation method and application of magnesium alloy containing graphene refiner |
| CN111363945A (en) * | 2020-02-27 | 2020-07-03 | 南昌航空大学 | Preparation and interface optimization method of modified graphene nanosheet magnesium-aluminum material |
| CN111363945B (en) * | 2020-02-27 | 2021-06-04 | 南昌航空大学 | Preparation and interface optimization method of modified graphene nanosheet magnesium-aluminum material |
| CN113005313A (en) * | 2021-02-23 | 2021-06-22 | 太原理工大学 | Preparation method of configuration design pre-dispersed graphene nanosheet reinforced magnesium-based composite material |
| CN113005313B (en) * | 2021-02-23 | 2021-10-22 | 太原理工大学 | Preparation method of configuration design pre-dispersed graphene nanosheet reinforced magnesium-based composite material |
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Application publication date: 20140507 |