CN104401968A - Method for preparing stereo graphene based on 3D printing of foam metal - Google Patents
Method for preparing stereo graphene based on 3D printing of foam metal Download PDFInfo
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- CN104401968A CN104401968A CN201410237601.4A CN201410237601A CN104401968A CN 104401968 A CN104401968 A CN 104401968A CN 201410237601 A CN201410237601 A CN 201410237601A CN 104401968 A CN104401968 A CN 104401968A
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Abstract
The invention aims to provide a method for preparing stereo graphene based on 3D printing of foam metal. The method comprises the following steps: S1, a three-dimensional digital model of foam metal is designed by a computer; S2, in a vacuum or argon environment, a layer of metal powder is uniformly laid on a stainless steel substrate by a powder laying mechanism; S3, the powder layer is preheated to reach the sintering degree; S4, an electron beam scans the powder layer to fuse loosely-connected particles so as to generate a layered cross-section of a forming part; S5, a workbench descends the height of a layer, and a new layer of powder is laid; S6, the steps (2), (3), (4) and (5) are repeated successively so as to form lumpy foam metal; S7, the same kind of metal particles are used for shot blasting so as to remove residual powder adhered to the forming part; S8, graphene grows on the prepared foam metal; and S9, a corrosive liquid is used to corrode the foam metal base so as to obtain the three-dimensional structured graphene. According to the invention, the problems of material waste, complex process and low precision are solved.
Description
Technical field
The present invention relates to a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal, belong to the preparation field of three-dimensional Graphene.
Background technology
Foamed metal refers to that porosity reaches more than 90%, has the porous metal of some strength and rigidity.Porous foam metal material is actually the matrix material of metal and gas, has that proportion is little, specific surface is large, energy absorption is good, resistance flame, heat and flame, anti-thermal shock, air-sensitive, can regenerate, the advantage such as processibility is good.Porous foam metal material can be divided into through hole body foamed metal and closed pore body foamed metal.Through hole body foamed metal has high, sound absorption properties good, perviousness is excellent, electromagnetic wave absorbability the is good advantage of heat exchange heat-sinking capability; And closed pore body foamed metal has the advantages such as thermal conductivity is low.Therefore, as a kind of new function material, porous foam metal, in electronics, communication, chemical industry, metallurgy, machinery, building, transportation, even has purposes widely in aeronautical and space technology.
At present, the foamed metal of merchandized handling has foamed aluminium, foam copper, nickel foam, foam iron-nickel etc.And the preparation method of foamed metal mainly contains following six kinds: casting, powder metallurgic method, metal deposition, sintering process, molten metal foaming, eutectic directional solidification method.Wherein the technological process of molten metal foaming is by after metal melting, adds whipping agent wherein, and the gas utilizing whipping agent to separate out produces bubble, after the cooling period, can obtain foamed metal.Molten metal foaming is mainly used in the preparation of the foamed metals such as Al, Sn of low melting point.Metal deposition adopts the method for chemistry or physics that metal is deposited on labile organism, and the method for recycling sintering is by organic matter removal.Metal deposition mainly comprises galvanic deposit and vapour deposition two kinds of methods.The technological process of sintering process is first sponge is cut into required shape, makes it fully absorb slurries containing metal-powder, through oversintering thermal treatment, sponge is decomposed after drying.Continuing heating makes organometallic compound decompose and material is sintered, and just can obtain the higher foamed metal of voidage after cooling.The production method technical process of existing foamed metal is complicated, and production process has waste gas waste sludge discharge, there is environmental pollution and the problem to operator's physical effects.Meanwhile, be sacrifice its mechanical property to exchange porous, high-ratio surface sum high pass porosity for, the problem of ubiquity intensity and poor impact resistance with aforementioned production method porous foam metal out; Foamed metal is aluminium due to what adopt, the elemental metals of copper and mickel, and its surface abrasion resistance corrosion resisting property need to improve.
Although the Chinese patent patent No. be 200680018697.9 propose a kind of metal is applied molten metal drop by thermospray or be atomized by molten metal be deposited at least part of described hole surface on to obtain metallized hole surface, but also must by from open-cell foam materials, waste material, tolerance range is low, and step is comparatively complicated.
Graphene (graphene) is a kind of novel charcoal material, and it has by the tightly packed bi-dimensional cellular shape crystalline structure of monolayer carbon atom.Graphene is unique and perfect structure makes it have the characteristics such as excellent electricity, mechanics, calorifics and optics, such as Graphene have 100 times of superhigh current carrying transport factors to silicon, the intensity up to 130GPa, well snappiness and nearly 20% percentage of elongation, excessive heat conductance, specific surface area up to 2600m2/g, and a few near-transparent, in very wide wave band, photoabsorption only has 2.3%.The physical properties of these excellences makes Graphene lead in matrix material, high performance lithium ion battery and ultracapacitor etc. show huge application potential at RF transistors, hypersensor, flexible transparent conductive film, superpower and height.
Current CVD method mainly with planar metal such as Copper Foil, nickel films as growing substrate, the graphene film of two dimensional surface can only be obtained, although be suitable for the application of nanometer electronic device and transparent conductive film, be difficult to the requirement meeting the application of the magnanimity such as matrix material, energy storage material.Although the Chinese patent patent No. is the making method that CN 201210176658.9 proposes a kind of Graphene, its Graphene prepared is two-dimensional graphene, can not prepare three-dimensional grapheme.Paper " Three-dimensional graphene architectures " reports the method for growing three-dimensional Graphene on Ni foam materials, but it can not the shape of accurate control Ni foam materials, and the preparation of Ni foam materials can not disposal molding, these are all unfavorable for that the industrialization of Graphene is produced.
Summary of the invention
For the problems referred to above, the invention provides a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal, described foamed metal can melt fast forming machine by electron beam and realize the direct printing-forming of hardware, combine the advantage that 3D prints, solve waste of material, complex procedures, the problem that tolerance range is low.And prepare three-dimensional Graphene further on this basis, open up the Application Areas that Graphene is new.
Technical program of the present invention lies in:
Prepare a method for three-dimensional Graphene based on 3D printing foamed metal, it is characterized in that, comprise following step:
S1: the three-dimensional digital model utilizing Computer Design foamed metal;
S2: in vacuum or ar gas environment, Pu Fen mechanism lays layer of metal powder equably on stainless steel substrate;
S3: in vacuum or ar gas environment, preheating bisque, makes it reach sintering degree;
S4: in vacuum or ar gas environment, the loose powder connected of electron beam scanning bisque fusing produces the layer cross section of drip molding;
S5: in vacuum or ar gas environment, worktable declines a layer height, lays new one deck powder;
S6: repeating step (2), (3), (4), (5) successively, forms block foam metal;
S7: carry out shot peening with same metal powder, so that the residual powder on drip molding is cohered in removing;
S8: adopt chemical Vapor deposition process growing graphene on obtained foamed metal;
S9: use corrosive fluid foamed metal substrate to be eroded the Graphene that can obtain three-dimensional structure.
Wherein, described foamed metal is made up of metallic nickel or metallic copper.
Described foamed metal structures is stereo grid shaped.
Described foamed metal layer cross section is made up of well-regulated polygonal mesh.
The mean length of described grid is 0-10cm, and width average is 0-10cm, and mean thickness is 0-10cm.
The mean length of described grid is 0-5mm, and width average is 0-5mm.
Metal grill wire diameter is 0-50um.
Described Pu Fen mechanism is paving powder cake or powder-laying roller.
Described corrosive fluid is corrodible foamed metal substrate and does not destroy the one of graphene-structured.
Described corrosive fluid is the iron trichloride corrosive fluid of corroding metal copper, or the salpeter solution of corroding metal nickel.
The invention has the advantages that:
The present invention adopts electron-beam melting technique, the three-dimensional model of foamed metal is designed in advance by computer, and the two-dimensional silhouette scanning pattern of grid is set, and then print formation foamed metal, foamed metal can be designed and manufactured into different structure formation, simultaneously technique comparatively traditional method greatly simplify, the foamed metal obtained is meticulousr, material use efficiency is higher, the typical case of CAD/CAM integrated digital manufacturing technology, on this basis, the Graphene of stereo structure can be grown, be conducive to qualitative orientation batch production Graphene.
Accompanying drawing explanation
Fig. 1 a, Fig. 1 b, Fig. 1 c, Fig. 1 d are the making processes schematic diagram of the embodiment of the present invention.
Fig. 2 is the single cell structure schematic diagram of foamed metal that the embodiment of the present invention makes.
Fig. 3 is the three-dimensional block diagram of Graphene be prepared into.
Embodiment
For above-mentioned feature and advantage of the present invention can be become apparent, special embodiment below, is described in detail below by reference to the accompanying drawings.
Below will be described in further detail the present invention by specific embodiment.
With reference to Fig. 1, a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal, comprises following step:
S1: the three-dimensional digital model utilizing Computer Design foamed metal;
S2: in vacuum or ar gas environment, Pu Fen mechanism lays layer of metal powder equably on stainless steel substrate;
S3: in vacuum or ar gas environment, preheating bisque, makes it reach sintering degree;
S4: in vacuum or ar gas environment, the loose powder connected of electron beam scanning bisque fusing produces the layer cross section of drip molding;
S5: in vacuum or ar gas environment, worktable declines a layer height, lays new one deck powder;
S6: repeating step (2), (3), (4), (5) successively, forms block foam metal;
S7: carry out shot peening with same metal powder, so that the residual powder on drip molding is cohered in removing;
S8: adopt chemical Vapor deposition process growing graphene on obtained foamed metal;
S9: use corrosive fluid foamed metal substrate to be eroded the Graphene that can obtain three-dimensional structure.
Above-mentioned foamed metal is made up of metallic nickel or metallic copper.
Above-mentioned foamed metal structures is stereo grid shaped.
Above-mentioned foamed metal layer cross section is made up of well-regulated polygonal mesh.
The mean length of above-mentioned grid is 0-10cm, and width average is 0-10cm, and mean thickness is 0-10cm.
The mean length of above-mentioned grid is 0-5mm, and width average is 0-5mm.
Metal grill wire diameter is 0-50um.
Above-mentioned Pu Fen mechanism is paving powder cake or powder-laying roller.
Above-mentioned corrosive fluid is corrodible foamed metal substrate and does not destroy the one of graphene-structured.
Above-mentioned corrosive fluid is the iron trichloride corrosive fluid of corroding metal copper, or the salpeter solution of corroding metal nickel.
Specific embodiment:
Undertaken by following several step:
(S11) utilize the three-dimensional digital model of Computer Design foamed metal, adoptable three-dimensional picture software package draws together Pro/E, SolidWorks, CATIA, UG, Solidege, AUTO CAD;
(S12) adopt RP-Tools software to carry out two-dimensional digital process to the three-dimensional digital model of foamed metal, the short transverse namely along model carries out segmentation section to model, obtains the two-dimensional silhouette figure of each layer cross section;
(S13) data model of foamed metal is input in 3D printer program, material on every layer of two dimensional surface and shape is drawn according to built data model, design superlaser printing path and melting, sintering time, below realization be about to perform step under the control of the computer, foamed metal without mould free forming;
(S14) stainless steel substrate being positioned over 3D is printed as in die cavity, vacuumizes and passes into rare gas element, as argon gas, forms protective atmosphere;
(S15) printing curve foamed metal.
The formed material of above-mentioned graphical foamed metal comprises metal nanoparticle, and metal species comprises copper, nickel etc.;
Above-mentioned graphical foamed metal is the metal frame-shaped structure of ordered grid structure;
Above-mentioned graphical foamed metal can adopt laser sintered or melt extrude forming technique to prepare;
The preferred laser sintered metal copper nano granules of the present embodiment is made into orderly stereo grid shaped metal array, and concrete steps are as follows:
(S151) metal grill print parameters is determined.According to the 2D sublayer pattern of 3D modeling, determine the parameter of orderly latticed foamed metal, comprise the size of grid, the wire diameter of shape and grid; This length of side implementing preferred square foamed metal screen frame is 10cm; The length of side of each born of the same parents' shape little square metal screen frame is 5mm; Metal grill wire diameter is that the concrete data of 50um(are to be determined)
(S152) metal copper nano granules transfer.Utilize powder-laying roller equipment in the horizontal direction copper nano particles to be evenly transferred to substrate surface, or utilize the shower nozzle increased in material equipment (3D printing), along its scanning pattern (metal grill wire diameter direction) is mobile, copper nano particles is uniformly coated on substrate surface; The present embodiment shower nozzle preferably increased in material equipment (3D printing) moves along its scanning pattern and copper nano particles is uniformly coated on substrate surface.
(S153) metal copper nano granules melting.Controlling laser beam makes its sintering temperature be 1085 DEG C, and laser head moves along spraying travel direction, and the superlaser that laser sends leads to and irradiates the metal copper nano granules powder of substrate surface, and dissolves the copper nano particles on its scanning pattern.
(S154) graphical foamed metal preparation.After fusing, copper and stainless steel substrate are sintered together, and form orderly stereo grid shaped metal array;
(S155) substrate surface treatment.The substrate manufactured is shifted out 3D printing device, and cleaning array surface, with inner, comprise spraying and prints and remain in the unnecessary metal copper nano granules of substrate surface in laser sintered process.
(S16): adopt chemical Vapor deposition process, chemical oxidization method, the growing graphene on obtained foamed metal of the either method in organic synthesis method.
(S161) the excellent chemical Vapor deposition process of the present embodiment growing graphene on foamed metal.
(S162) use the foamed metal copper billet of acetone and process, be placed in the silica tube of tube furnace;
(S163) normal pressure is warmed up to 800 DEG C-1000 DEG C under an argon atmosphere, and argon flow amount keeps 600sccm(1sccm=1mL/min), temperature rise rate is 8 DEG C/min;
(S164) after metal block reaches target temperature, pass into hydrogen reducing annealing, flow is 60sccm, and argon flow amount and temperature remain unchanged;
(S165), after 20min, 10-50sccm methane, 100sccm hydrogen and 1000sccm argon gas is passed into;
(S166), after growing 5-15min, close methane and hydrogen, lower the temperature with stove under an argon atmosphere;
(S167), after cooling terminates, foamed metal copper billet is taken out.
(S17) use liquor ferri trichloridi that foamed metal copper substrate corrosion is fallen the Graphene that can obtain three-dimensional structure, as shown in Figure 3.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (10)
1. prepare a method for three-dimensional Graphene based on 3D printing foamed metal, it is characterized in that, comprise following step:
S1: the three-dimensional digital model utilizing Computer Design foamed metal;
S2: in vacuum or ar gas environment, Pu Fen mechanism lays layer of metal powder equably on stainless steel substrate;
S3: in vacuum or ar gas environment, preheating bisque, makes it reach sintering degree;
S4: in vacuum or ar gas environment, the loose powder connected of electron beam scanning bisque fusing produces the layer cross section of drip molding;
S5: in vacuum or ar gas environment, worktable declines a layer height, lays new one deck powder;
S6: repeating step (2), (3), (4), (5) successively, forms block foam metal;
S7: carry out shot peening with same metal powder, so that the residual powder on drip molding is cohered in removing;
S8: adopt chemical Vapor deposition process growing graphene on obtained foamed metal;
S9: use corrosive fluid foamed metal substrate to be eroded the Graphene that can obtain three-dimensional structure.
2. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 1, is characterized in that: described foamed metal is made up of metallic nickel or metallic copper.
3. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 1, is characterized in that: described foamed metal structures is stereo grid shaped.
4. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 1, is characterized in that: described foamed metal layer cross section is made up of well-regulated polygonal mesh.
5. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 3, is characterized in that: the mean length of described grid is 0-10cm, and width average is 0-10cm, and mean thickness is 0-10cm.
6. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 4, is characterized in that: the mean length of described grid is 0-5mm, and width average is 0-5mm.
7. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 4, is characterized in that: metal grill wire diameter is 0-50um.
8. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 1, is characterized in that: described Pu Fen mechanism is paving powder cake or powder-laying roller.
9. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 1, is characterized in that: described corrosive fluid is corrodible foamed metal substrate and does not destroy the one of graphene-structured.
10. a kind of method preparing three-dimensional Graphene based on 3D printing foamed metal according to claim 9, is characterized in that: described corrosive fluid is the iron trichloride corrosive fluid of corroding metal copper, or the salpeter solution of corroding metal nickel.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104801704A (en) * | 2015-03-26 | 2015-07-29 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN105695786A (en) * | 2016-03-01 | 2016-06-22 | 中国兵器科学研究院宁波分院 | Method for preparing titanium-based graphene composite material through 3D printing technology |
| WO2018017369A3 (en) * | 2016-07-12 | 2018-04-05 | William Marsh Rice University | Three-dimensional (3d) printing of graphene materials |
| CN108687345A (en) * | 2018-06-13 | 2018-10-23 | 东莞宜安科技股份有限公司 | A kind of 3D printing method |
| CN108691570A (en) * | 2017-04-05 | 2018-10-23 | 通用电气公司 | In conjunction with the component of 3D cognizance codes |
| CN110449590A (en) * | 2018-05-08 | 2019-11-15 | 长飞光纤光缆股份有限公司 | A kind of preparation method and product of graphene-Cu-base composites |
| CN113753880A (en) * | 2021-08-27 | 2021-12-07 | 北京航空航天大学 | Method for preparing three-dimensional graphene structure through 3D printing |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104801704A (en) * | 2015-03-26 | 2015-07-29 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN104801704B (en) * | 2015-03-26 | 2017-01-25 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN105695786A (en) * | 2016-03-01 | 2016-06-22 | 中国兵器科学研究院宁波分院 | Method for preparing titanium-based graphene composite material through 3D printing technology |
| WO2018017369A3 (en) * | 2016-07-12 | 2018-04-05 | William Marsh Rice University | Three-dimensional (3d) printing of graphene materials |
| US11970399B2 (en) | 2016-07-12 | 2024-04-30 | William Marsh Rice University | Three-dimensional (3D) printing of graphene materials |
| CN108691570A (en) * | 2017-04-05 | 2018-10-23 | 通用电气公司 | In conjunction with the component of 3D cognizance codes |
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| CN110449590A (en) * | 2018-05-08 | 2019-11-15 | 长飞光纤光缆股份有限公司 | A kind of preparation method and product of graphene-Cu-base composites |
| CN110449590B (en) * | 2018-05-08 | 2021-03-09 | 长飞光纤光缆股份有限公司 | Preparation method and product of graphene-copper-based composite material |
| CN108687345A (en) * | 2018-06-13 | 2018-10-23 | 东莞宜安科技股份有限公司 | A kind of 3D printing method |
| CN108687345B (en) * | 2018-06-13 | 2019-12-24 | 东莞宜安科技股份有限公司 | 3D printing method |
| CN113753880A (en) * | 2021-08-27 | 2021-12-07 | 北京航空航天大学 | Method for preparing three-dimensional graphene structure through 3D printing |
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