CN105063404A - Preparation method of titanium matrix graphene alloy - Google Patents
Preparation method of titanium matrix graphene alloy Download PDFInfo
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- CN105063404A CN105063404A CN201510382475.6A CN201510382475A CN105063404A CN 105063404 A CN105063404 A CN 105063404A CN 201510382475 A CN201510382475 A CN 201510382475A CN 105063404 A CN105063404 A CN 105063404A
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Abstract
The invention provides a preparation method of titanium matrix graphene alloy. The method comprises the following steps: preparing graphene and titanium and/or titanium alloy mixed powder, filling a jacket with the mixed powder, carrying out vacuum degassing, carrying out hot isostatic pressing, re-melting, and homogenizing. A certain amount of the titanium matrix graphene alloy precast ingots are re-melted in titanium alloy melt, the content of graphene in a composite material can be well controlled through calculating, and graphene cannot float, so the content of graphene in the titanium matrix graphene alloy can be accurately controlled; and the preparation method is provided on the basis of semi-continuous melting casting, and has the advantages of simple operation, high production efficiency, low preparation cost, and easy realization of large scale industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of alkene alloy, be specifically related to a kind of preparation method of titanium base alkene alloy.
Background technology
Graphene is a kind of New Two Dimensional nano material, the two-dimensional material of the monoatomic layer thickness that its nanometer sheet is made up of sp2 hydbridized carbon atoms, be thin, the hardest nano material in known world, intensity is up to 1.01Tpa, be 100 times of structure iron, density is but 1/5 of structure iron.Thermal conductivity is up to 5300W/mK, and higher than carbon nanotube and diamond, under normal temperature, electronic mobility is more than 200000cm2/VS, higher than CNT (carbon nano-tube) or silicon crystal, resistivity only about 1 Ω m, than titanium or silver lower, be the material that world resistivity is minimum.
Graphene belongs to nanometer materials, has surfactivity, is easily combined with other materials particle.The topmost application of nanoparticle is as packing material during other non-nano material modifications, but all relative difficulty are produced and preserved to a lot of nanoparticles, Graphene compares to be convenient to produce on a large scale and preserve, and therefore can be used as packing material during other materials modification.Due to the toughness of Graphene and intensity and surfactivity, when as packing material, Graphene can be made to become recessive welding material between other base mateiral crystal grain, form chain bridge effect at crystal grain boundary.Base mateiral intercrystalline, by graphenic surface active function, forms the form that crystal grain boundary presents seamless connection.After crystal grain boundary in base mateiral forms seamless connection, the masterpiece used time outside, its Grain Boundary Sliding phenomenon reduces, and resistance to stress ability increases, thus the intensity of the base mateiral be filled is strengthened along with the raising of resistance to stress ability.
Conventional processing methods has been difficult to improve the intensity of metallic substance, uses Graphene that density small intensity is large as strongthener, can also reduce the density of material while improving Strength of Metallic Materials.Be compound to Graphene in the metallic substance such as aluminium, titanium, magnesium, can obtain high-strength light, have both the matrix material of the structure-function integration of the functional performances such as conduction, heat conduction.
On 05 08th, 2014, the scientific research personnel of industry Hang Cai institute of Air China initiated in international Graphene research field novel alloy material " alkene alloy " material that a class has excellent properties.
But it is less that Graphene exists size, specific surface area is large, is difficult to dispersion, is easy to the problem of reuniting, has a strong impact on the performance of alkene alloy.All there is the problem yielded poorly in the technique of current graphene reinforced metal-matrix composite, is difficult to form scale operation.
Summary of the invention
For overcoming the above-mentioned defect that existing alkene alloy exists, the invention provides a kind of method preparing Graphene and metal mixed powder, the method improve the blending processes of powders of Graphene and titanium and/or titanium alloy powder, being distributed in titanium and/or titanium alloy substrate of graphene nanometer sheet even dispersion.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of preparation method of titanium base alkene alloy comprises the steps:
A) prepare Graphene and titanium and/or titanium alloy mixed powder, described powder comprises following parts by weight component: Graphene 3% ~ 10%, and titanium and/or titanium alloy powder are surplus;
A-1) Graphene monodisperse liquor is prepared;
A-1-1) solution is configured;
A-1-2) by Graphene pass into solution;
A-1-3) by step a-1-2) the Graphene organic solution prepared puts into ultrasonic oscillation device and stirs;
A-2) titanium and/or titanium alloy powder are joined step a-1) gained Graphene monodisperse liquor;
A-3) by step a-2) gained Graphene and titanium and/or titanium alloy mixing solutions put into ball grinder ball milling 20 ~ 40h;
A-4) by step a-3) obtained mixing solutions is in 50 ~ 60 DEG C and stir lower oven dry;
B) Graphene step a) obtained and titanium and/or titanium alloy mixed powder load in the stainless steel jacket for preparing (jacket internal diameter is 80 ~ 120mm, and jacket cavity heights is 85 ~ 300mm);
C) carrying out vacuum stripping 2 ~ 4h after jacket being heated to 700 ~ 900 DEG C to vacuum tightness is 1.0 × 10
-3pa, pounds flat, welded seal by jacket;
D) by step c) jacket of sealing that obtains carries out hot isostatic pressing, temperature 700 DEG C ~ 900 DEG C, pressure 100 ~ 200MPa, and the heat-insulation pressure keeping time is 2 ~ 4h;
E) jacket after hot isostatic pressing is carried out mechanical workout, jacket skin is removed in turning, and obtaining diameter is 55 ~ 85mm, is highly the cylindrical prefabricated ingot of 55 ~ 200mm;
F) in the protection atmosphere of rare gas element by a) titanium and/or the identical titanium of titanium alloy powder and/or titanium alloy to add on crucible post-heating crucible to this titanium and/or titanium alloy fusing point 30 DEG C ~ 80 DEG C and obtain titanium and/or melts of titanium alloy with step;
G) in the protection atmosphere of rare gas element, keeping crucible temperature constant by step e) the cylindrical prefabricated ingot that obtains adds crucible and obtains titanium and/or the melts of titanium alloy that melting has cylindrical prefabricated ingot, after stirring, titanium base alkene alloy melt is cast to rapidly in graphite jig, obtains titanium base alkene alloy cast ingot in protection atmosphere hollow cold to the room temperature of rare gas element;
H) by step g) the titanium base alkene alloy cast ingot that obtains carries out Homogenization Treatments, temperature is be incubated 24 ~ 48h at 750 DEG C ~ 950 DEG C, be carry out hot extrusion at 15: 1 ~ 20: 1 with the extrusion machine of tonnage 200 ~ 500t with extrusion ratio, obtain titanium base alkene alloy bar material.
Further, step a-2) in the particle diameter of titanium and/or titanium alloy powder be 5 ~ 100 μm.
Further, step a-1-1) in the weight of organic solvent of configuration be 19 ~ 191 times of Graphene; Described organic solvent is one or more that select from ethanol, NMP, polyoxyethylene glycol or PVP, and in described aqueous solutions of organic solvent, the mass percent of organic solvent is 20% ~ 100%.
Further, step a-1-3) by step a-1-2) the Graphene organic solution prepared put into ultrasonic oscillation device carry out solution stirring time >=2h.
Further, step a-3) in ball material 10: 1 ~ 15: 1 in ball grinder, the rotating speed >=300r/min of described ball mill, the abrading-ball of described ball mill is high-carbon-chromium bearing steel material abrading-ball.
Further, step a-4) in drying course bake out temperature be 50 ~ 60 DEG C, carry out mechanical stirring while oven dry.
Further, step f) and g) in rare gas element be SF
6+ N
2, two kinds of gas volume ratios are 1: 3.
Further, by step g) the titanium base alkene alloy cast ingot that obtains carries out Homogenization Treatments, and temperature is be incubated 24 ~ 48h at 700 DEG C ~ 900 DEG C, uses rolling mill roll forming, obtains titanium base alkene sheet alloy.
Further, titanium base alkene alloy comprises the component of following weight percent: Graphene 0.1% ~ 5%, and titanium and/or titanium alloy are surplus.
Owing to have employed technique scheme, compared with prior art, beneficial effect of the present invention comprises:
1. the preparation method of a kind of titanium base alkene alloy of the present invention, by the prefabricated ingot remelting of a certain amount of titanium base alkene alloy in titanium alloy melting liquid, by calculating the content controlling Graphene in matrix material very well, due to Graphene, emersion is not next, in titanium base alkene alloy, content can accurately control, be the preparation method proposed based on semicontinuous founding, technological operation be simple, production efficiency is high, cheap for manufacturing cost, be easy to realize extensive industrialization.
2. the preparation method of a kind of titanium base alkene alloy of the present invention, after remelting and diluting, Graphene is still dispersed in titanium liquation, when solidifying, the dispersivity of Graphene is very strong, secondary agglomeration can not occur, strand is functional, can be squeezed into bar and be rolled into sheet material after carrying out Homogenization Treatments.
3. the preparation method of a kind of titanium base alkene alloy of the present invention, has atmosphere protection in the remelting of prefabricated ingot and castingprocesses, avoids oxidation and the sex change of titanium and/or titanium alloy and Graphene.
4. the preparation method of a kind of titanium base alkene alloy of the present invention, realizes being separated of prefabricated ingot and casting technique, is easy to the preparation realizing large-sized titanium base alkene alloy in enormous quantities, reduces production cost, has excellent future in engineering applications.
5. the preparation method of a kind of titanium base alkene alloy of the present invention, by the mode of high-energy ball milling, by the collision of ball milling pearl, graphene uniform is disperseed, solve Graphene easily to reunite the problem of not easily disperseing, together with being mounted to titanium and/or titanium alloy powder by Graphene, Graphene is mixed uniformly with titanium and/or titanium alloy powder powder.
6. the preparation method of a kind of titanium base alkene alloy of the present invention, by high-energy ball milling Graphene is mounted to titanium and/or titanium alloy powder surface, graphene uniform is scattered in titanium and/or titanium alloy substrate, achieve the mortise at Graphene and titanium and/or titanium alloy interface, Graphene and titanium and/or titanium alloy powder powder have good bonding interface, for the performance of Graphene and titanium and/or titanium alloy composite material is given security.
7. the preparation method of a kind of titanium base alkene alloy of the present invention, improves the blending processes of powders of Graphene and titanium and/or titanium alloy powder, graphene nanometer sheet even dispersion be distributed in titanium and/or titanium alloy substrate; The method of the prefabricated ingot of remelting and diluting is adopted to improve the wettability of Graphene and melts of titanium alloy, it is dispersed in melts of titanium alloy, matrix material after dilution to be become the dispersivity of Graphene after molten metal excellent by solid remelting, without secondary agglomeration phenomenon, when again solidifying, the dispersivity of Graphene is very strong, and casting and forgeability are greatly improved.
Embodiment
Below in conjunction with example, the present invention will be described in detail.
Embodiment 1:
Prepare titanium base Graphene, concrete steps are as follows:
A) prepare Graphene and titanium mixed powder, powder comprises: Graphene 10g (Hummer ' s legal system standby), titanium alloy powder 1kg; Titanium alloy comprises the component of following weight percent:
Al4.0 ~ 6.0%; Sn2.0 ~ 3.0%; Fe≤0.50%; C≤0.08%; N≤0.05%; H≤0.015%; O≤0.20%; Other elements (single)≤0.10%; Other elements (total amount)≤0.40%; Ti is surplus.
A-1) Graphene monodisperse liquor is prepared;
A-1-1) configure aqueous solutions of organic solvent, the weight of organic solvent is 19 times of Graphene, and organic solvent is from ethanolic soln, and in aqueous solutions of organic solvent, the mass percent of organic solvent is 80%;
A-1-2) Graphene is dissolved in aqueous solutions of organic solvent;
A-1-3) by step a-1-2) the Graphene organic solution prepared puts into ultrasonic oscillation device and carries out solution stirring, the time 2h of stirring;
A-2) QZr0.2 titanium alloy powder is joined step a-1) gained Graphene monodisperse liquor, the particle diameter of titanium alloy powder is 5 ~ 100 μm;
A-3) by step a-2) gained Graphene and metal mixed solution puts into ball grinder mechanical ball milling 20 ~ 40h, ball material 10: 1 in ball grinder, the rotating speed 300r/min of ball mill;
A-4) being equipped with through step a-3) baking oven put into by the beaker of Graphene that ball milling obtains and metal mixed solution dries, and in drying course, bake out temperature is 50 DEG C, carries out mechanical stirring while oven dry;
B) Graphene step a) obtained and titanium alloy mixed powder load the stainless steel jacket interior (jacket internal diameter is 80mm, and jacket cavity heights is 85mm) prepared;
C) carrying out vacuum stripping 2 to vacuum tightness after jacket being heated to 700 DEG C is 1.0 × 10
-3pa, pounds flat, welded seal by jacket;
D) by step c) jacket of sealing that obtains carries out hot isostatic pressing, temperature 900 DEG C, pressure 110MPa, and the heat-insulation pressure keeping time is 2h;
E) jacket after hot isostatic pressing is carried out mechanical workout, jacket skin is removed in turning, and obtaining diameter is 55mm, is highly the cylindrical prefabricated ingot of 55mm;
F) in the protection atmosphere of rare gas element by with step a) 9kg titanium alloy that titanium alloy powder is identical to add on crucible post-heating crucible to this titanium and/or titanium alloy fusing point 80 DEG C and obtain melts of titanium alloy;
G) in the protection atmosphere of rare gas element, keeping crucible temperature constant by step e) the cylindrical prefabricated ingot that obtains adds crucible and obtains the melts of titanium alloy that melting has cylindrical prefabricated ingot, after stirring, titanium base alkene alloy melt is cast to rapidly in graphite jig, obtains titanium base alkene alloy cast ingot in protection atmosphere hollow cold to the room temperature of rare gas element; Rare gas element is SF
6+ N
2, two kinds of gas volume ratios are 1: 3;
H) by step g) the titanium base alkene alloy cast ingot that obtains carries out Homogenization Treatments, temperature is be incubated 24h at 750 DEG C, be 730 DEG C with the extrusion machine of tonnage 200 ~ 500t at extrusion temperature, be carry out hot extrusion at 20: 1 with extrusion ratio, obtain the titanium base alkene alloy bar material of Φ 12mm.
The room temperature tensile intensity of the titanium base alkene alloy bar material taking above technique to prepare is 1110MPa, and elongation is 9%.With titanium alloy (the tensile strength 1030MPa not adding Graphene, elongation is 10%) compare, the intensity detail of titanium base alkene alloy bar material improves, and while gaining in strength, unit elongation and specific conductivity do not decline, and highlight Graphene and have obvious advantage compared with other wild phases.
Embodiment 2 ~ 5 is listed in the table below, and sequence of process steps wherein and term implication and embodiment 1 are with, the different numerical value of the parameter corresponding from embodiment 1 that listed is:
Table 1 titanium base alkene alloy and corresponding titanium/titanium alloy substrate performance comparison
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit, although with reference to above-described embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or equivalent replacement, and not departing from any amendment of spirit and scope of the invention or equivalent replacement, it all should be encompassed in the middle of right of the present invention.
Claims (9)
1. a preparation method for titanium base alkene alloy, is characterized in that: described method comprises the steps:
A) prepare Graphene and titanium and/or titanium alloy mixed powder, described powder comprises following parts by weight component: Graphene 3% ~ 10%, and titanium and/or titanium alloy powder are surplus;
A-1) Graphene monodisperse liquor is prepared;
A-1-1) solution is configured;
A-1-2) by Graphene pass into solution;
A-1-3) by step a-1-2) the Graphene organic solution prepared puts into ultrasonic oscillation device and stirs;
A-2) titanium and/or titanium alloy powder are joined step a-1) gained Graphene monodisperse liquor;
A-3) by step a-2) gained Graphene and titanium and/or titanium alloy mixing solutions put into ball grinder ball milling 20 ~ 40h;
A-4) by step a-3) obtained mixing solutions is in 50 ~ 60 DEG C and stir lower oven dry;
B) it is 80 ~ 120mm that Graphene step a) obtained and titanium and/or titanium alloy mixed powder load internal diameter, and cavity heights is the stainless steel jacket of 85 ~ 300mm;
C) jacket being heated to 700 ~ 900 DEG C, to carry out vacuum stripping 2 ~ 4h to vacuum tightness be 1.0 × 10
-3pa, pounds flat, welded seal by jacket;
D) in 700 DEG C ~ 900 DEG C, by step c under 100 ~ 200MPa pressure) the jacket hot isostatic pressing 2 ~ 4h of sealing that obtains;
E) jacket after hot isostatic pressing is carried out mechanical workout, jacket skin is removed in turning, and obtaining diameter is 55 ~ 85mm, is highly the cylindrical prefabricated ingot of 55 ~ 200mm;
F) in the protection atmosphere of rare gas element, crucible heating 30 DEG C ~ 80 DEG C obtained copper and/or copper alloy melt to fusing point of titanium a) identical with step and/or titanium alloy powder will be housed;
G) in the protection atmosphere of rare gas element, keeping crucible temperature constant by step e) the cylindrical prefabricated ingot that obtains adds crucible and obtains titanium and/or the melts of titanium alloy that melting has cylindrical prefabricated ingot, after stirring, titanium base alkene alloy melt is cast to rapidly in graphite jig, obtains titanium base alkene alloy cast ingot in protection atmosphere hollow cold to the room temperature of rare gas element;
H) by step g) the titanium base alkene alloy cast ingot that obtains carries out Homogenization Treatments, temperature is be incubated 24 ~ 48h at 750 DEG C ~ 950 DEG C, be carry out hot extrusion at 15: 1 ~ 20: 1 with the extrusion machine of tonnage 200 ~ 500t with extrusion ratio, obtain titanium base alkene alloy bar material.
2. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described step a-2) in the particle diameter of titanium and/or titanium alloy powder be 5 ~ 100 μm.
3. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described step a-1-1) in the weight of organic solvent of configuration be 19 ~ 191 times of Graphene; Described solvent by mass percent 20% ~ 100% ethanol, NMP, polyoxyethylene glycol or PVP and water form.
4. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described step a-1-3) by step a-1-2) graphene solution prepared puts into ultrasonic oscillation device and at least stirs 2h.
5. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, it is characterized in that: described step a-3) in ball grinder ratio of grinding media to material be 10: 1 ~ 15: 1, ball milling under rotating speed at least 300r/min, the abrading-ball of described ball mill is high-carbon-chromium bearing steel material abrading-ball.
6. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described step a-4) in drying course bake out temperature be 50 ~ 60 DEG C, carry out mechanical stirring while oven dry.
7. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described step f) and g) in rare gas element be SF
6+ N
2, two kinds of gas volume ratios are 1: 3.
8. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, it is characterized in that: described by step g) the titanium base alkene alloy cast ingot that obtains carries out Homogenization Treatments, temperature is be incubated 24 ~ 48h at 750 DEG C ~ 950 DEG C, uses rolling mill roll forming, obtains titanium base alkene sheet alloy.
9. the preparation method of a kind of titanium base alkene alloy as claimed in claim 1, is characterized in that: described titanium base alkene alloy comprises the component of following weight percent: Graphene 0.1% ~ 5%, and titanium and/or titanium alloy are surplus.
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| CN107502772B (en) * | 2017-07-17 | 2019-06-07 | 无锡吉仓纳米材料科技有限公司 | A kind of preparation method and casting graphene/aluminum alloy composite materials of casting graphene/aluminum alloy composite materials |
| CN108531769A (en) * | 2018-04-16 | 2018-09-14 | 厦门奈福电子有限公司 | A kind of graphene-metallic composite and its prepare raw material, method and application |
| CN109609806A (en) * | 2018-07-05 | 2019-04-12 | 重庆大学 | A kind of graphene oxide enhancing titanium composite material and preparation method thereof |
| CN109022907A (en) * | 2018-07-20 | 2018-12-18 | 东南大学 | A kind of graphene enhancing titanium composite material and its preparation method and application that three-dimensional network shape is distributed |
| CN109554577A (en) * | 2018-12-28 | 2019-04-02 | 北京理工大学 | A kind of preparation method of the graphene enhancing titanium composite material of lamellar structure |
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Address after: 100095 Haidian District hot springs town, Beijing Village Applicant after: China Hangfa Beijing Institute of Aerial Materials Address before: 100095 Haidian District hot springs town, Beijing Village Applicant before: Beijing Institute of Aeronautical Materials, China Aviation Industry Group Corporation |
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Application publication date: 20151118 |