CN104561847A - Silicon particle and carbon nanotube mixing enhanced aluminum-based composite material and preparation method thereof - Google Patents
Silicon particle and carbon nanotube mixing enhanced aluminum-based composite material and preparation method thereof Download PDFInfo
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- CN104561847A CN104561847A CN201310522531.2A CN201310522531A CN104561847A CN 104561847 A CN104561847 A CN 104561847A CN 201310522531 A CN201310522531 A CN 201310522531A CN 104561847 A CN104561847 A CN 104561847A
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Abstract
The invention relates to a silicon particle and carbon nanotube mixing enhanced aluminum-based composite material and a preparation method thereof. The composite material is prepared from an aluminum alloy matrix and an enhancing bulk phase, wherein the enhancing bulk phase is prepared from a carbon nanotube and silicon; the percent by volume of the aluminum alloy matrix is 30-50vol.%, the percent by volume of the carbon nanotube is 0.5-2vol.% and the percent by volume of silicon is 49-68vol.%. By adopting a powder metallurgic process, the aluminum-based composite material with comprehensive performances such as low density, high bending strength, high elasticity modulus and low coefficient of thermal expansion is prepared. The density of the novel aluminum-based composite material is 2.43-2.52g/cm<3>, the bending strength is 400-500MPa, the elasticity modulus is 115-125GPa and the coefficient of thermal expansion is 8.5-10.9*10<-6>/K. As a result of excellent performances of the material, the using requirement of a spacecraft supporting structural member can be satisfied well.
Description
Technical field
The present invention relates to aluminum matrix composite of a kind of silicon grain and carbon nanotube mixing enhancing and preparation method thereof; in particular, provide the powder metallurgy preparation technique of a kind of multi-walled carbon nano-tubes (CNTs) and silicon grain hybrid composite; enable prepared material be applied to space precision device support structural part, belong to advanced material research and development field.
Technical background
With aerospace science technology development, the novel Spacecraft guidance and control being applied to every field presents the features such as precise structure, thin-walled property, maximization, its precision parts and structural part are to lightweight, low cost, high-performance, high reliability future development, thus reduce the own wt of aerospacecraft, improve payload capability and the operation stability of spacecraft, this proposes higher over-all properties requirement to material.For space precision device support structural part, available type material must have the characteristics such as low density, low-expansion coefficient and good processing forming, also to have high strength, suitable rigidity to realize the secure support effect to accurate functional component simultaneously, but traditional metal alloy, pottery and polymer materials, all cannot meet the performance requirements such as novel spacecraft loss of weight, environmental stability, safe reliability as aluminium, titanium alloy, Invar alloy, Kovar alloy etc., these all impel people develop and design type material.
High-performance aluminum-base composite material has played vital role in the application of the high-tech sectors such as space technology, aerospace, high-speed transit, electronic devices and components, is typical hi tech and new material.The SiCp/Al matrix material of current aerospace field widespread use has high intensity and Young's modulus, can meet the requirement of Spacecraft Material, but its density is comparatively large, and is difficult to when grain volume fraction is higher carry out mechanical workout, limits the application of this material.
Silicon has higher Young's modulus (130-190GPa), lower hardness (processibility is good), low density (2.3g/cm
3), thermal conductivity and thermal expansivity are respectively 156W/mK and 4.1 × 10
-6k
-1.Some documents and patent report cross the Si particle-reinforced aluminum and reasonable offer matrix material thereof that adopt high-volume fractional, but the material that obtains is applied in the field such as heat management, piston of automobile mostly, be applied to little report of space flight supporting structure aspect, this cause that mainly the high silica-alumina material intensity prepared of traditional technology and method is lower.
Summary of the invention
Main purpose of the present invention is to provide the aluminum matrix composite of a kind of silicon grain and carbon nanotube mixing enhancing.
The novel crystal carbon with hollow structure that CNTs is made up of graphite synusia, all known the most solid, one of material that rigidity is the highest, its axial modulus of elasticity at present from theory estimate and test determination up to more than 1TPa, tensile strength is 100GPa, the tensile strain being greater than 40% can be born, and brittle behaviour, viscous deformation or bond rupture can not be presented.In addition, CNTs thermal conductivity is 3000 ~ 6000W/mK, is the material that in known materials, thermal conductivity is the highest, simultaneously its thermal expansivity extremely low (well below Silicified breccias).And when adopting CNTs Matrix Composites Reinforced by Stirring, the CNTs volume fraction added general lower (high body divides CNTs to be not easily uniformly dispersed), this causes the CNTs of low volume fraction to reduce degree less (often can not meet low density and low-expansion coefficient requirement) to aluminum substrate density and thermal expansivity, but greatly can improve Young's modulus and the intensity of matrix.
Therefore, the present invention adopts the Si particle reinforced aluminum alloy matrix of Gao Tifen, density and the thermal expansivity of alloy matrix aluminum is greatly reduced with this, simultaneously by adding appropriate CNTs(≤2.0vol.%) improve intensity and the Young's modulus of matrix, be intended to by Si and CNTs two kinds of mixed intensified alloy matrix aluminums of material, prepare the material with low thermal coefficient of expansion, low density, high-flexural strength, high elastic coefficient, make target material meet the performance requirement of empty sky structure devices.
The aluminum matrix composite that a kind of silicon grain and carbon nanotube mixing strengthen, by alloy matrix aluminum and reinforcement phase composite, reinforcement is made up of carbon nanotube (CNTs) and silicon (Si), the volume percent of alloy matrix aluminum is 30 ~ 50vol.%, the volume fraction of carbon nanotube (CNTs) is 0.5 ~ 2vol.%, and the volume fraction of silicon is 49 ~ 68vol.%.
Described alloy matrix aluminum is 2009Al etc.; The carbon nanotube (CNTs) that described carbon nanotube (CNTs) is plated surface tungsten.Described reinforcement is multi-walled carbon nano-tubes (CNTs) and silicon Si particle mixing reinforcement mutually,
The volume fraction of carbon nanotube (CNTs) can be preferably 1 ~ 2vol.%, and the volume fraction of silicon (Si) particle is 49.5 ~ 68vol.%.
Another object of the present invention is to provide a kind of method preparing novel aluminium based matrix material, mainly comprise the surface preparation of CNTs, the ball milling of powder mix powder, powder isostatic cool pressing, the vacuum outgas of isostatic cool pressing billet, isostatic cool pressing billet HIP sintering, the step such as hot isostatic pressing billet thermal treatment, thus obtain the aluminum matrix composite with low density, high-flexural strength, high elastic coefficient and low thermal coefficient of expansion over-all properties.
A preparation method for silicon grain and carbon nanotube hybrid composite, comprises the steps:
(1) surface pre-treating process of CNTs: first CNTs is carried out surface acid-washing process, rinse post-drying with water; Then Metalorganic Chemical Vapor Deposition is adopted to carry out plating W process;
(2) ball milling blending processes of powders: CNTs, Si powder after plating W process and alloy matrix aluminum powder are put into the mixing of ball mill ball milling, the volume percent of alloy matrix aluminum is 30 ~ 50vol.%, carbon nanotube (CNTs) is 0.5 ~ 2vol.%, and silicon Si particle is 49 ~ 68vol.%;
(3) powder isostatic sintering technique: the powder mix after ball milling is carried out isostatic cool pressing, then carries out Fruit storage by isostatic cool pressing billet, then carries out hot isostatic pressing;
(4) thermal treatment process: hot isostatic pressing material is carried out fixation rates, at 510 DEG C of insulation 2h, water-cooled natural aging 100h.
In step (1), described CNTs is nominal diameter is 20 ~ 30nm, and length is 20 ~ 30 μm, and density is 1.7g/cm
3, purity is many walls CNTs of 95%; Carry out surface acid-washing process, to remove the catalyst impurities on CNTs surface, acid solution used is the vitriol oil and concentrated nitric acid mixed solution (H
2sO
4and HNO
3volume ratio is 3:1), the time that CNTs soaks in nitration mixture is 30min, adopts deionized water rinse several times to CNTs and dry after filtering acid solution.
Plated surface W process is carried out to CNTs, to improve the wettability of CNTs and made of Al-Cu alloy matrix.Plating W adopts mocvd method, tungsten hexacarbonyl (W (CO)
6) be presoma, high-purity H
2for carrier band gas (flow 200ml/min), plating temperature 400 ~ 500 DEG C, time 60min.
In step (2), described alloy matrix aluminum is 2009Al, by nitration mixture and plating W pretreated after CNTs, nominal diameter to be the Si powder of 5 μm and nominal diameter be that the 2009Al powder of 25 μm mixes in rotary type ball mill, rotating speed is 100 revs/min, Ball-milling Time is 30h, bearing steel ball is ball milling ball, and ratio of grinding media to material is 2:1, and mixed powder process is for being dry mixed.
In step (3), the powder after ball milling is loaded rubber package set and carries out isostatic cool pressing, isostatic cool pressing pressure is 150MPa, and the dwell time is 0.5h; Isostatic cool pressing billet is carried out vacuum outgas, and vacuum outgas temperature top temperature is 560 DEG C, and devolatilization vacuum degree is less than 10
-3pa; Carry out hot isostatic pressing after the soldering and sealing of vacuum stripping billet, hip temperature is 560 ~ 590 DEG C, and pressure is 100MPa, heat-insulation pressure keeping time 3h.
In step (4), fixation rates is carried out to hot isostatic pressing material, with the speed of 5 ~ 8 DEG C/min chamber type electric resistance furnace be warming up to 510 DEG C and be incubated 30min, subsequently hot isostatic pressing material being put into stove inside holding 2h, water-cooled, natural aging 100h.
The invention has the advantages that CNTs has carried out plating W process before mixing powder, improve the interface wet ability of CNTs and metal aluminum alloy matrix; By adding CNTs and Si particle mixing REINFORCED Al alloy substrate, Young's modulus and intensity, reduction density and the thermal expansivity of matrix significantly can be strengthened.Divide Si particle reinforce Al alloy phase ratio with simple high body, CNTs and Si particle mixing strengthen composite density lower, thermal expansivity is less, Young's modulus and bending strength higher.The matrix material prepared has low density, high-flexural strength, high elastic coefficient and low thermal coefficient of expansion over-all properties, can be applied to space precision device structured material.
The present invention adopts powder metallurgical technique, divide CNTs(≤2vol.% mainly through low body) and high body divide Si particle (>=49vol.%) mix strengthen alloy matrix aluminum, reduce density and the thermal expansivity of matrix, improve Young's modulus and the bending strength of matrix simultaneously, obtain the material of a kind of aerospace low density, low thermal coefficient of expansion, high-flexural strength and high elastic coefficient.The density of the novel aluminium based matrix material of the present invention is 2.43 ~ 2.52g/cm
3, bending strength is 400 ~ 500MPa, and Young's modulus is 115 ~ 125GPa, and thermal expansivity is 8.5 ~ 10.9 × 10
-6k
-1.The excellent properties of this material better can meet the service requirements of spacecraft supporting structure.
Accompanying drawing explanation
Fig. 1 is preparation were established figure.
Fig. 2 is carbon nanotube plating tungsten schematic diagram.
Main Reference Numerals:
1 carrier band gas transmission pipeline 2 vapor deposition chamber
3 deposition chamber heat device 4 gas pipeline valves
5 spring 6 shaking devices
7 oil bath pan heating unit 8 tungsten hexacarbonyl charging bottles
The mixed gas of A solid-state tungsten hexacarbonyl B gaseous state tungsten hexacarbonyl and carrier band hydrogen
C carbon nanotube D nitrogen
E hydrogen F oil bath pan oil
Embodiment
By following embodiment, the present invention is described in further detail, but working of an invention mode is not limited thereto.
As shown in Figure 1, for preparation were established figure of the present invention, first by CNTs plated surface W, then carry out ball milling with Si powder and mix powder-isostatic cool pressing-vacuum outgas-hot isostatic pressing-fixation rates together with 2009Al powder, finally obtain the aluminum matrix composite of silicon grain and carbon nanotube mixing enhancing.
As shown in Figure 2, be carbon nanotube plating tungsten schematic diagram, carbon nanotube plating tungsten step is: carbon nanotube C is put into vapor deposition chamber 2 by (1), and solid-state tungsten hexacarbonyl A crystal puts into tungsten hexacarbonyl charging bottle 8.Open gas pipeline valve 4, hydrogen E(or nitrogen D) air in carrier band gas transmission pipeline 1, tungsten hexacarbonyl charging bottle 8 and vapor deposition chamber 2 is driven out of; (2) start deposition chamber heat device 3 and carbon nanotube C is heated to tungsten plating temperature, starting shock device 6 makes carbon nanotube C be in vibrating state (ensureing that following tungsten evenly can be plated on carbon nanotube C surface); (3) place the oily F of oil bath pan in oil bath pan, start oil bath pan heating unit 7 and solid-state tungsten hexacarbonyl A heating sublimation is transformed into gaseous state tungsten hexacarbonyl, gaseous state tungsten hexacarbonyl and the carrier band hydrogen E flowed through are mixed to form mixed gas B and flow into vapor deposition chamber 2; (4) the mixed gas B of gaseous state tungsten hexacarbonyl and carrier band hydrogen touches carbon nanotube C surface, tungsten hexacarbonyl now in gas B absorbs the concurrent biochemical decomposition (equation is as follows) of heat on carbon nanotube C surface, decompose the tungsten generated and be plated on carbon nanotube C surface formation plating tungsten carbon nanotube (W-CNTs), the CO produced then discharges sediment chamber with hydrogen, completes carbon nanotube C surface tungsten metal plating process.
Embodiment 1
The composition of matrix material by volume mark is: many walls CNTs(diameter 20 ~ 30nm, length is 20 ~ 30 μm, and density is 1.7g/cm
3, purity is 95%) and content be 1vol.%, Si powder (diameter 5 μm) content be 49vol.%, 2009Al powder (mean diameter 25 μm) is 50vol.%.The composition of 2009Al alloy by the component of mass percentage is: copper 3.2 ~ 4.4, magnesium 1.0 ~ 1.6, silicon 0.25, iron 0.2, zinc 0.1, oxygen 0.6, and surplus is aluminium.
First, CNTs is put into ethanol solution and carries out ultrasonic wave dispersion treatment 30min, then pull out, put into the vitriol oil and concentrated nitric acid mix acid liquor (H
2sO
4and HNO
3volume ratio is 3:1) stir 30min, elimination acid solution also with deionized water rinsing CNTs number time, dries CNTs.CNTs is put into metal organic chemical vapor deposition stove and carry out plating W process.With tungsten hexacarbonyl (W (CO) during plating W
6) be presoma, high-purity H
2for carrier band gas (flow 200ml/min), plating temperature 450 DEG C, time 60min.Then, CNTs and the Si powder, the 2009Al powder that have plated W are put into ball mill, and adding bearing steel ball ratio of grinding media to material is 2:1, continuous ball milling 30h, and rotating speed is 100 revs/min, and mixed powder process is for being dry mixed.
Taken out by powder and load isostatic cool pressing rubber bag, good seal jacket carries out isostatic cool pressing.Isostatic cool pressing pressure and dwell time are respectively 150MPa and 0.5h.Material after isostatic cool pressing is loaded in metal capsule after resting and reorganizing in suitable surface and carries out Fruit storage.Degassing temperature top temperature is 560 DEG C, treats that low vacuum is in 10
-3pa terminates degassed.Carry out hot isostatic pressing to the material after degassed, hip temperature and pressure are respectively 560 DEG C and 100MPa, and the heat-insulation pressure keeping time is 3h.Finally, hot isostatic pressing material is carried out fixation rates, with the speed of 5 ~ 8 DEG C/min chamber type electric resistance furnace is warming up to 510 DEG C and is incubated 30min and treat that furnace temperature is stablized, put into hot isostatic pressing material insulation 2h, water-cooled natural aging 100h subsequently.
Resulting materials carries out the performance test results: density 2.52g/cm
3, bending strength 500MPa, Young's modulus 115GPa, linear expansivity 10.9 × 10
-6k
-1.
1vol.% in said process is plated tungsten carbon nanotube to change 1vol.% into and do not plate tungsten carbon nanotube (all the other composite material compositions proportionings and matrix material preparation process all identical), the composite property test result prepared is: bending strength is 468MPa, Young's modulus 109GPa, linear expansivity 11.4 × 10
-6k
-1.When performance comparison result shows same volume mark, plating tungsten carbon nanotube is more obvious than not plating tungsten carbon nanotube to the strengthening effect of matrix, namely plates the strengthening of tungsten carbon nano tube surface and has larger strengthening effect to substrate performance.
Embodiment 2
The composition of matrix material by volume mark is: many walls CNTs(diameter 20 ~ 30nm, length is 20 ~ 30 μm, and density is 1.7g/cm
3, purity is 95%) and content be 2vol.%, Si powder (diameter 5 μm) content be 68vol.%, 2009Al powder (mean diameter 25 μm) is 30vol.%.The composition of 2009Al alloy by the component of mass percentage is: copper 3.2 ~ 4.4, magnesium 1.0 ~ 1.6, silicon 0.25, iron 0.2, zinc 0.1, oxygen 0.6, and surplus is aluminium.
First, CNTs is put into ethanol solution and carries out ultrasonic wave dispersion treatment 30min, then pull out, put into the vitriol oil and concentrated nitric acid mix acid liquor (H
2sO
4and HNO
3volume ratio is 3:1) stir 30min, elimination acid solution also with deionized water rinsing CNTs number time, dries CNTs.CNTs is put into metal organic chemical vapor deposition stove and carry out plating W process.With tungsten hexacarbonyl (W (CO) during plating W
6) be presoma, high-purity H
2for carrier band gas (flow 200ml/min), plating temperature 500 DEG C, time 60min.Then, CNTs and the Si powder, the 2009Al powder that have plated W are put into ball mill, and adding bearing steel ball ratio of grinding media to material is 2:1, continuous ball milling 30h, and rotating speed is 100 revs/min, and mixed powder process is for being dry mixed.
Taken out by powder and load isostatic cool pressing rubber bag, good seal jacket carries out isostatic cool pressing.Isostatic cool pressing pressure and dwell time are respectively 150MPa and 0.5h.Material after isostatic cool pressing is loaded in metal capsule after resting and reorganizing in suitable surface, after soldering and sealing, carries out Fruit storage.Degassing temperature top temperature is 560 DEG C, treats that low vacuum is in 10
-3pa terminates degassed.Carry out hot isostatic pressing to the material after degassed, hip temperature and pressure are respectively 590 DEG C and 100MPa, and the heat-insulation pressure keeping time is 3h.Finally, hot isostatic pressing material is carried out fixation rates, with the speed of 5 ~ 8 DEG C/min box resistivity is warming up to 510 DEG C and is incubated 30min and treat that furnace temperature is stablized, put into hot isostatic pressing material insulation 2h, water-cooled natural aging 100h subsequently.
Resulting materials carries out the performance test results: density 2.43g/cm
3, bending strength 400MPa, Young's modulus 125GPa, linear expansivity 8.5 × 10
-6k
-1.
For embodying the strengthening effect of plating tungsten carbon nano tube surface strengthening to substrate performance, only the 2vol.% in said process is plated tungsten carbon nanotube to change 2vol.% into and do not plate tungsten carbon nanotube (all the other composite material compositions proportionings and matrix material preparation process all identical), the composite property test result prepared is: bending strength is 369MPa, Young's modulus 119GPa, linear expansivity 9.0 × 10
-6k
-1.When performance comparison result shows same volume mark, plating tungsten carbon nanotube is more obvious than not plating tungsten carbon nanotube to the strengthening effect of matrix.
The density of the novel aluminium based matrix material obtained by the inventive method is 2.43 ~ 2.52g/cm
3, bending strength is 400 ~ 500MPa, and Young's modulus is 115 ~ 125GPa, and thermal expansivity is 8.5 ~ 10.9 × 10
-6k
-1.The excellent properties of this material better can meet the service requirements of spacecraft supporting structure.
Claims (10)
1. the aluminum matrix composite of a silicon grain and carbon nanotube mixing enhancing, it is characterized in that: by alloy matrix aluminum and reinforcement phase composite, described reinforcement is made up of carbon nanotube and silicon, the volume percent of alloy matrix aluminum is 30 ~ 50vol.%, carbon nanotube is 0.5 ~ 2vol.%, and silicon is 49 ~ 68vol.%.
2. the aluminum matrix composite of silicon grain according to claim 1 and carbon nanotube mixing enhancing, is characterized in that: described alloy matrix aluminum is 2009Al.
3. the aluminum matrix composite of silicon grain according to claim 1 and carbon nanotube mixing enhancing, is characterized in that: described carbon nanotube is the carbon nanotube of plated surface tungsten.
4. a preparation method for silicon grain and carbon nanotube hybrid composite, comprises the steps:
(1) first carbon nanotube is carried out surface acid-washing process, rinse post-drying with water; Then Metalorganic Chemical Vapor Deposition is adopted to carry out the process of plating tungsten;
(2) carbon nanotube, silica flour and alloy matrix aluminum powder after the process of plating tungsten are put into the mixing of ball mill ball milling, the volume percent of alloy matrix aluminum is 30 ~ 50vol.%, and carbon nanotube is 0.5 ~ 2vol.%, and silicon is 49 ~ 68vol.%;
(3) powder mix after ball milling is carried out isostatic cool pressing, then isostatic cool pressing billet is carried out Fruit storage, then carry out hot isostatic pressing;
(4) hot isostatic pressing material is carried out fixation rates, at 510 DEG C of insulation 2h, water-cooled natural aging 100h.
5. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, is characterized in that: described carbon nanotube is nominal diameter is 20 ~ 30nm, and length is 20 ~ 30 μm, and density is 1.7g/cm
3, purity is the multi-walled carbon nano-tubes of 95%.
6. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, is characterized in that: during surface acid-washing process, the vitriol oil and the concentrated nitric acid mixed solution of acid solution used to be volume ratio be 3:1.
7. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, it is characterized in that: during plating tungsten process, take tungsten hexacarbonyl as presoma, high-purity hydrogen is carrier band gas, plating temperature is 400 ~ 500 DEG C, and the time is 60min.
8. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, is characterized in that: described alloy matrix aluminum is the nominal diameter of 2009Al, 2009Al powder is 25 μm, and the nominal diameter of Si powder is 5 μm.
9. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, is characterized in that: during ball milling mixing, rotating speed is 100 revs/min, and Ball-milling Time is 30h, and ratio of grinding media to material is 2:1.
10. the preparation method of silicon grain according to claim 4 and carbon nanotube hybrid composite, is characterized in that: described isostatic cool pressing pressure is 150MPa, and the dwell time is 0.5h; Described vacuum outgas temperature is up to 560 DEG C, and devolatilization vacuum degree is less than 10
-3pa; Described hip temperature is 560 ~ 590 DEG C, and pressure is 100MPa, heat-insulation pressure keeping time 3h.
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| CN114134373A (en) * | 2021-11-16 | 2022-03-04 | 哈尔滨铸鼎工大新材料科技有限公司 | Silicon-aluminum alloy packaging material with high tensile strength and preparation method thereof |
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Cited By (2)
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