CN105127197B - Preparation method for multi-layer metal/graphene composite electrode thin strip - Google Patents
Preparation method for multi-layer metal/graphene composite electrode thin strip Download PDFInfo
- Publication number
- CN105127197B CN105127197B CN201510541161.6A CN201510541161A CN105127197B CN 105127197 B CN105127197 B CN 105127197B CN 201510541161 A CN201510541161 A CN 201510541161A CN 105127197 B CN105127197 B CN 105127197B
- Authority
- CN
- China
- Prior art keywords
- graphene
- metal
- strip
- rolling
- thickness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention provides a preparation method for a multi-layer metal/graphene composite electrode thin strip. The preparation method comprises the following process steps: (1) carrying out primary thinning on a metal material by adopting a synchronous cold rolling process; (2) grinding and cleaning metal thin strips; (2) coating the surfaces of the metal thin strips with graphene paint; (4) tightly laminating upper and lower surfaces of 2-20 metal/graphene thin strips; (5) carrying out synchronous cold rolling on multiple metal/graphene thin strips; (6) carrying out synchronous cold rolling or asynchronous cold rolling on a multi-layer metal/graphene composite thin plate; (7) carrying out asynchronous cold rolling on the multi-layer metal/graphene composite thin plate; and (8) carrying out negative roll-gap asynchronous cold rolling on the multi-layer metal/graphene composite thin plate, thereby obtaining an extremely thin strip. According to the method disclosed by the invention, atomic-scale combination of graphene and metal is achieved; the preparation process is low in requirements on production equipment; the production energy sources are saved; emission of carbon dioxide is reduced; and mass production for the multi-layer metal/graphene composite thin plate with a thickness of 1-4 [mu]m is easy to realize.
Description
Technical field
The invention belongs to technical field of metal is and in particular to a kind of multiple layer metal/Graphene is combined the system of strip in razor-thin
Preparation Method.
Background technology
Graphene is a kind of two-dimension single layer carbon atom new material, by sp2Hydbridized carbon atoms Mi Dui constitute, surface area up to
2630mm2/g.Graphene has the performances such as excellent mechanics, thermal conductance, charge-transporting, optics and gas permeability, such as Young mould
Measure as 1100gpa, fracture strength is 125gpa, thermal conductivity factor is up to 5300w/m k, and under normal temperature, electron mobility exceedes
15000cm2/ v s, and resistivity is only about 1 ω m, only absorbs 2.3% light, almost fully transparent.Using above-mentioned graphite
The excellent characteristic of alkene, by, the such as metal such as copper, aluminium, molybdenum, nickel, titanium, steel compound with other metal materials, can give green wood
Expect more excellent performance.At present, metal material and the compound of Graphene mainly have electrochemical deposition method, ball milling and sinter bonded
Etc. method, but due to complicated process of preparation, and the probability that Graphene is reunited is larger, leads to Graphene dispersion in the base not
Uniformly, have a strong impact on the performance after metal material is combined.Additionally, there is no using cold rolling mode composition metal and Graphene at present,
Prepare the report that multiple layer metal/Graphene is combined strip in razor-thin, compared with method hot rolling, cold rolling combined temp is relatively low, can effectively keep away
Exempt from the formation of phase transformation, microstructure change and fragility intermediate compound that metallic matrix occurs being unfavorable for combining.Cold rolling compound
Uniformly, surface smoothness is high, the defect such as non-oxidation layer for the thickness of composite material of technique preparation.Metal and the bond strength of Graphene
Height, Graphene non-oxidation phenomenon, properties of product are stable.Technique flexibly, both can spiral-plate be combined, and also can be easy to automation
Coil rolling, beneficial to stable, high-yielding.
Content of the invention
The problem existing for prior art, and combine the advantage of cold-rolling process, the present invention provides a kind of multiple layer metal/stone
Black alkene is combined the preparation method of strip in razor-thin.Graphene uniform is coated in metal by roller brush or cvd technique by described preparation method
Thin sheet surface, is prepared multiple layer metal Graphene composite strip by the cold-rolling process of symmetric rolling afterwards, is finally rolled using asynchronous
The cold-rolling process of system is prepared multiple layer metal/Graphene and is combined strip in razor-thin, and this multiple layer metal/Graphene is combined strip in razor-thin logical
The fields such as news, electronics, micro manufacturing, micro-system and medical treatment are respectively provided with good future in engineering applications.The technical scheme is that
A kind of multiple layer metal/Graphene is combined the preparation method of strip in razor-thin, carries out according to following processing step:
(1) preparing thickness is 1～20mm, and width is the metal material of 50～500mm, using synchronous cold-rolling process, through 4～
Metal material is thinned to 0.3～0.9mm by 10 passages, and synchronous cold-rolling process parameter is: roller diameter is 100-180mm, rolling
Speed is 0.5～3m/min, and percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness
The 1/5～1/3 of metal material tensile strength；
(2) by the upper and lower surface polishing of metal sheet band, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature
30～50 DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) Graphene coating being coated uniformly on the metal sheet band surface of step (2), the coating thickness of Graphene is 5～
50 μm, it is placed in the air afterwards and air-dries 10～30min, obtain Metal/grapheme strip blank；
(4) 2～20 Metal/grapheme strip blank upper and lower surfaces are fitted tightly together；
(5) using synchronous cold-rolling process, the multi-disc Metal/grapheme strip blank of step (4) is rolled, technique is joined
Number is: roller diameter is 100-180mm, and mill speed is 0.5～3m/min, first rolling pass reduction 30～70%, second
20～50%, the operation of rolling adopts micro tension milling to secondary reduction ratio, and tension value is the 1/5 of equal thickness metal material tensile strength
～1/3, obtain multiple layer metal/Graphene composite sheet, thickness is 0.5～1mm；
(6) using synchronous cold rolling or cross-shear rolling technique, multiple layer metal/Graphene composite sheet is thinned to 80～200
μm, when using symmetric rolling, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, and tension value is etc.
The 1/5～1/3 of thick metal material tensile strength, percentage pass reduction is 10～15%, is thinned to target through 10～15 passages thick
Degree；
When using asymmetrical rolling, technological parameter is: roller diameter 30～50mm, mill speed 10～60mm/s, friction speed
For 1.05～1.2, tension value is the 1/5～1/3 of equal thickness metal material tensile strength to ratio, and percentage pass reduction is 8～15%, warp
2～4 passages are thinned to target thickness；
(7) adopt cross-shear rolling technique, will be thinning for the multiple layer metal of step (6)/Graphene composite strip through 3～7 passages
To 15～25 μm, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, friction speed ratio 1.1～1.4, tension force
Less than the 1/2 of equal thickness metal material tensile strength, percentage pass reduction is 10～40% to value, and total deformation rate is more than 80%；
(8) using negative roll gap cross-shear rolling technique, the multiple layer metal in step (7)/Graphene composite strip is thinned to 1
～4 μm, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, tension value is little
In the 1/2 of equal thickness metal material tensile strength, percentage pass reduction is 10～40%, rolls 6～10 passages, and total deformation rate is more than
80%, prepare multiple layer metal/Graphene that thickness is 1～4 μm and be combined strip in razor-thin.
The metal material of described step (1) is copper, aluminium, molybdenum, nickel, titanium, steel.
The Graphene coating of described step (3) is the watersoluble plumbago alkene solution of mass concentration 4%, the oil of mass concentration 4%
Property graphene solution, graphene powder.
The mode that Graphene coating is coated uniformly on metal sheet band surface of described step (3) has two kinds: mode one is
By mass concentration be 4% graphene solution or graphene powder even roller brush on metal sheet band surface；Mode two is to adopt cvd
Method, that is, utilize methane as carbon source, grows Graphene by it in metal base surface pyrolytic, thus on strip surface
Uniform deposited graphite alkene.
The laminating type of described step (4) has seam, strong metallic glue or rivet.
The negative roll gap cross-shear rolling technique of described step (8) is that under room temperature condition, double-working is fully pressed against, and occurs larger
Elastic flattening, carry out the asymmetrical rolling process of metal composite strip in this condition.
The present invention has the advantage that with beneficial effect is:
(1) the inventive method using roller brush Graphene coating or cvd method by the way of the deposited graphite alkene layer of strip surface,
Graphene uniform can be made to be dispersed in metal surface, control the content of Graphene in Graphene metal composite strip.
(2) using negative roll gap cold-rolling process, compared with traditional handicraft, rolled piece is connect the inventive method final step with roll
Tactile region significantly increases, and in conjunction with asymmetrical rolling, increases considerably Cuo Zha area ratio, the more conducively plastic deformation of rolled piece, thus
Improve rolling efficiency, that breaks through traditional identical roll neck milling train rolls the thin limit, effectively increases subtracting of Metal/grapheme composite
Thin efficiency, meanwhile, also can improve the performances such as the conductive and heat-conductive of Graphene metal composite strip in razor-thin.
(3) the inventive method can make Graphene and metal reach the combination of atom level, and whole preparation process is to production equipment
Require relatively low, save and produce the energy and reduce CO2 emission, it is easy to accomplish thickness is 1～4 μm of multiple layer metal/Graphene
The batch production of compound strip in razor-thin, being respectively provided with good engineering in fields such as communication, electronics, micro manufacturing, micro-system and medical treatment should
Use prospect.
Brief description
The assembling schematic diagram of the Metal/grapheme that Fig. 1 is prepared for the inventive method.
Fig. 2 is the microstructure picture of the compound strip in razor-thin of 1 μm of multiple layer of copper/Graphene of the embodiment of the present invention 1 preparation.
Fig. 3 is the microstructure picture of the compound strip in razor-thin of 4 μm of multilayer aluminum/Graphenes of the embodiment of the present invention 2 preparation, wherein
Go represents Graphene.
Specific embodiment
The ultrasonic activation instrument model adopting in the embodiment of the present invention: clean alliance jp-010t；
The synchronous cold-rolling mill adopting in the embodiment of the present invention is made products；
The cross-shear rolling machine adopting in the embodiment of the present invention is made products, referring to patent cn 102989765；
The tension motor model adopting in the embodiment of the present invention: three-phase The gear deceleration torque motor ajc 6334；
The negative roll gap asymmetrical rolling cold-rolling mill adopting in the embodiment of the present invention is made products, referring to patent cn
102989765.
Embodiment 1
Prepare multiple layer of copper/Graphene that thickness is 1 μm and be combined strip in razor-thin, processing step is:
(1) preparing industrial pure copper t2 is raw metal, a size of: thickness 2mm, width is 50mm, using synchronous Cold-roller
Copper material is thinned to 0.5mm through 4 passages by skill, and synchronous cold-rolling process parameter is: roller diameter is 180mm, and mill speed is
0.5m/min, percentage pass reduction is 5～20%, and the operation of rolling adopts mild tension condition, and tension value is that equal thickness copper material tension is strong
The 1/5 of degree；
(2) by the upper and lower surface polishing of copper strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 30
DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) by 4% watersoluble plumbago alkene solution even roller brush in the copper strip surface of step (2), the coating of Graphene is thick
Spend for 5～50 μm, be placed in the air afterwards and air-dry 15min, obtain copper/Graphene strip blank；
(4) 6 copper/Graphene strip blank upper and lower surface is fitted tightly together by seam；
(5) using synchronous cold-rolling process, the plurality of copper/Graphene strip blank of step (4) is rolled, technological parameter
For: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is 70%, and the second percentage pass reduction is
50%, the operation of rolling adopts micro tension milling, and tension value is the 1/5 of equal thickness copper material tensile strength, obtains multiple layer of copper/Graphene
Composite sheet, thickness is 0.5mm；
(6) using synchronous cold-rolling process, multiple layer of copper/Graphene composite sheet is thinned to 80 μm, technological parameter is: roll
Diameter 30mm, mill speed 10～50mm/s, tension value be equal thickness copper material tensile strength 1/5, percentage pass reduction be 10～
15%, it is thinned to target thickness through 10 passages；
(7) adopt cross-shear rolling technique, through 3 passages, the multiple layer of copper of step (6)/Graphene composite strip is thinned to 15 μ
M, technological parameter is: roller diameter 30mm, mill speed 50mm/s, friction speed ratio 1.1～1.4, and tension value resists for equal thickness copper material
The 1/3 of tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99%；
(8) using negative roll gap cross-shear rolling technique, the multiple layer of copper in step (7)/Graphene composite strip is thinned to 1 μm,
Technological parameter is: roller diameter 30mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness copper material
The 1/3 of tensile strength, percentage pass reduction is 20～40%, rolls 6 passages, and total deformation rate is 99.9%, and preparing thickness is 1
μm multiple layer of copper/Graphene be combined strip in razor-thin.
Multiple layer of copper/Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is uniform,
The defect such as non-oxidation layer and crackle.Good dispersion degree in Copper substrate for the Graphene, lamella area is big, and soilless sticking phenomenon, with matrix
Conjugation is high, as shown in Figure 2.
Embodiment 2
Prepare multilayer aluminum/Graphene that thickness is 4 μm and be combined strip in razor-thin, processing step is:
(1) preparing commercial-purity aluminium a1060 is raw metal, a size of: thickness 20mm, width is 500mm, using synchronous cold
Aluminium is thinned to 0.9mm through 10 passages by roll process, and synchronous cold-rolling process parameter is: roller diameter is 100mm, mill speed
For 0.5～3m/min, percentage pass reduction is 20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness aluminium tension
The 1/3 of intensity；
(2) by the upper and lower surface polishing of aluminium strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 50
DEG C, scavenging period is 6～10min, is placed in the air and air-dries；
(3) by graphene powder even roller brush in the aluminium strip surface of step (2), the coating thickness of Graphene is 5～50 μ
M, obtains aluminium/Graphene strip blank；
(4) 2 aluminium/Graphene strip blank upper and lower surface is fitted tightly together by seam；
(5) using synchronous cold-rolling process, the multi-disc aluminium/Graphene strip blank of step (4) is rolled, technological parameter
For: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction exists in 30%, second percentage pass reduction
20%, the operation of rolling adopts micro tension milling, and tension value is the 1/3 of equal thickness aluminium tensile strength, obtains multilayer aluminum/Graphene
Composite sheet, thickness is 0.5mm；
(6) using cross-shear rolling technique, multilayer aluminum/Graphene composite sheet is thinned to 200 μm, technological parameter is: roll
Diameter 50mm, mill speed 10～60mm/s, for 1.05～1.2, tension value is the 1/ of equal thickness aluminium tensile strength to friction speed ratio
3, percentage pass reduction is 8～15%, is thinned to target thickness through 4 passages；
(7) adopt cross-shear rolling technique, through 7 passages, the multilayer aluminum of step (6)/Graphene composite strip is thinned to 25 μ
M, technological parameter is: roller diameter 50mm, mill speed 10～50mm/s, friction speed ratio 1.1～1.4, and tension value is equal thickness aluminium
The 1/3 of material tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99.75%；
(8) using negative roll gap cross-shear rolling technique, the multilayer aluminum in step (7)/Graphene composite strip is thinned to 4 μm,
Technological parameter is: roller diameter 50mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness aluminium
The 1/3 of tensile strength, percentage pass reduction is 10～40%, rolls 6 passages, and total deformation rate is 99.96%, and preparing thickness is
4 μm of multilayer aluminum/Graphene is combined strip in razor-thin.
Multilayer aluminum/Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is uniform,
The defect such as non-oxidation layer and crackle.Good dispersion degree in aluminum substrate for the Graphene, lamella area is big, and soilless sticking phenomenon, with matrix
Conjugation is high, as shown in Figure 3.
Embodiment 3
Prepare MULTI-LAYER NICKEL/Graphene that thickness is 4 μm and be combined strip in razor-thin, processing step is:
(1) preparing industrial pure ni is raw metal, a size of: thickness 2mm, width is 50mm, using synchronous cold-rolling process,
Through 4 passages, nickel material is thinned to 0.3mm, synchronous cold-rolling process parameter is: roller diameter is 180mm, mill speed is 0.5m/
Min, percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness nickel material tensile strength
1/5；
(2) by the upper and lower surface polishing of nickel strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 30
DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) utilize cvd method deposited graphite alkene on nickel strip, parameter is as follows: carbon source: methane；Temperature: 700 DEG C；Cooling
Mode: air cooling, obtain nickel/Graphene strip blank.
(4) 20 nickel/Graphene strip blank upper and lower surface is fitted tightly together by strong metallic glue；
(5) using synchronous cold-rolling process, the multi-disc nickel/Graphene strip blank of step (4) is rolled, technological parameter
For: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is 70%, and the second percentage pass reduction is
40%, the operation of rolling adopts micro tension milling, and tension value is the 1/5 of equal thickness copper material tensile strength, obtains multiple layer of copper/Graphene
Composite sheet, thickness is 0.9mm；
(6) using synchronous cold-rolling process, MULTI-LAYER NICKEL/Graphene composite sheet is thinned to 80 μm, technological parameter is: roll
Diameter 30mm, mill speed 10～50mm/s, tension value be equal thickness nickel material tensile strength 1/4, percentage pass reduction be 10～
15%, it is thinned to target thickness through 15 passages；
(7) adopt cross-shear rolling technique, through 3 passages, the MULTI-LAYER NICKEL of step (6)/Graphene composite strip is thinned to 15 μ
M, technological parameter is: roller diameter 30mm, mill speed 50mm/s, friction speed ratio 1.1～1.4, and tension value is that equal thickness nickel material resists
The 1/3 of tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99%；
(8) using negative roll gap cross-shear rolling technique, the MULTI-LAYER NICKEL in step (7)/Graphene composite strip is thinned to 4 μm,
Technological parameter is: roller diameter 30mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness copper material
The 1/3 of tensile strength, percentage pass reduction is 20～40%, rolls 6 passages, and total deformation rate is 99.9%, and preparing thickness is 4
μm MULTI-LAYER NICKEL/Graphene be combined strip in razor-thin.
MULTI-LAYER NICKEL/Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is uniform,
The defect such as non-oxidation layer and crackle.Good dispersion degree in Ni substrate for the Graphene, lamella area is big, and soilless sticking phenomenon, with matrix
Conjugation is high.
Embodiment 4
Prepare multilayer molybdenum/Graphene that thickness is 3 μm and be combined strip in razor-thin, processing step is:
(1) preparing technical pure molybdenum is raw metal, a size of: thickness 2mm, width is 50mm, using synchronous cold-rolling process,
Through 4 passages, copper material is thinned to 0.5mm, synchronous cold-rolling process parameter is: roller diameter is 180mm, mill speed is 3m/min,
Percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is the 1/5 of equal thickness copper material tensile strength；
(2) by the upper and lower surface polishing of molybdenum strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 30
DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) by 4% oiliness graphene solution even roller brush in the molybdenum strip surface of step (2), the coating of Graphene is thick
Spend for 5～50 μm, be placed in the air afterwards and air-dry 15min, obtain molybdenum/Graphene strip blank；
(4) 6 molybdenums/Graphene strip blank upper and lower surface is fitted tightly together by seam；
(5) using synchronous cold-rolling process, the multi-disc molybdenum/Graphene strip blank of step (4) is rolled, technological parameter
For: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is 70%, and the second percentage pass reduction is
40%, the operation of rolling adopts micro tension milling, and tension value is the 1/5 of equal thickness molybdenum materials tensile strength, obtains multilayer molybdenum/Graphene
Composite sheet, thickness is 0.5mm；
(6) using synchronous cold-rolling process, multilayer molybdenum/Graphene composite sheet is thinned to 80 μm, technological parameter is: roll
Diameter 30mm, mill speed 10～50mm/s, tension value be equal thickness molybdenum materials tensile strength 1/4, percentage pass reduction be 10～
15%, it is thinned to target thickness through 10 passages；
(7) adopt cross-shear rolling technique, through 3 passages, the multilayer molybdenum/Graphene composite strip of step (6) is thinned to 15 μ
M, technological parameter is: roller diameter 30mm, mill speed 50mm/s, friction speed ratio 1.1～1.4, and tension value resists for equal thickness molybdenum materials
The 1/3 of tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99%；
(8) using negative roll gap cross-shear rolling technique, the multilayer molybdenum/Graphene composite strip in step (7) is thinned to 3 μm,
Technological parameter is: roller diameter 30mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness molybdenum materials
The 1/3 of tensile strength, percentage pass reduction is 20～40%, rolls 6 passages, and total deformation rate is 99.9%, and preparing thickness is 3
μm multilayer molybdenum/Graphene be combined strip in razor-thin.
Multilayer molybdenum/Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is uniform,
The defect such as non-oxidation layer and crackle.Good dispersion degree in Mo substrate for the Graphene, lamella area is big, and soilless sticking phenomenon, with matrix
Conjugation is high.
Embodiment 5
Prepare multilayer titanium/Graphene that thickness is 3 μm and be combined strip in razor-thin, processing step is:
(1) preparing industrially pure titanium is raw metal, a size of: thickness 2mm, width is 50mm, using synchronous cold-rolling process,
Through 4 passages, copper material is thinned to 0.5mm, synchronous cold-rolling process parameter is: roller diameter is 180mm, mill speed is 0.5m/
Min, percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness copper material tensile strength
1/5；
(2) by the upper and lower surface polishing of titanium strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 30
DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) by 4% watersoluble plumbago alkene solution even roller brush in the titanium strip surface of step (2), the coating of Graphene is thick
Spend for 5～50 μm, be placed in the air afterwards and air-dry 15min, obtain titanium/Graphene strip blank；
(4) 6 titaniums/Graphene strip blank upper and lower surface is fitted tightly together by rivet；
(5) using synchronous cold-rolling process, the multi-disc titanium/Graphene strip blank of step (4) is rolled, technological parameter
For: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is 70%, and the second percentage pass reduction is
40%, the operation of rolling adopts micro tension milling, and tension value is the 1/5 of equal thickness titanium tensile strength, obtains multilayer titanium/Graphene
Composite sheet, thickness is 0.5mm；
(6) using synchronous cold-rolling process, multilayer titanium/Graphene composite sheet is thinned to 80 μm, technological parameter is: roll
Diameter 30mm, mill speed 10～50mm/s, tension value be equal thickness titanium tensile strength 1/4, percentage pass reduction be 10～
15%, it is thinned to target thickness through 10 passages；
(7) adopt cross-shear rolling technique, through 3 passages, the multilayer titanium/Graphene composite strip of step (6) is thinned to 15 μ
M, technological parameter is: roller diameter 30mm, mill speed 50mm/s, friction speed ratio 1.1～1.4, and tension value resists for equal thickness titanium
The 1/3 of tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99%；
(8) using negative roll gap cross-shear rolling technique, the multilayer titanium/Graphene composite strip in step (7) is thinned to 3 μm,
Technological parameter is: roller diameter 30mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness titanium
The 1/3 of tensile strength, percentage pass reduction is 20～40%, rolls 6 passages, and total deformation rate is 99.9%, and preparing thickness is 3
μm multilayer titanium/Graphene be combined strip in razor-thin.
Multilayer titanium/Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is uniform,
The defect such as non-oxidation layer and crackle.Good dispersion degree in Titanium base for the Graphene, lamella area is big, and soilless sticking phenomenon, with matrix
Conjugation is high.
Embodiment 6
Prepare the multilayer q195/ Graphene that thickness is 3 μm and be combined strip in razor-thin, processing step is:
(1) preparing technical pure q195 is raw metal, a size of: thickness 2mm, width is 50mm, using synchronous Cold-roller
Copper material is thinned to 0.5mm through 10 passages by skill, and synchronous cold-rolling process parameter is: roller diameter is 180mm, and mill speed is 2m/
Min, percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness copper material tensile strength
1/5；
(2) by the upper and lower surface polishing of copper strip, recycle ultrasonic activation cleaning, parameter is set to ultrasonic water temperature 30
DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) by 4% watersoluble plumbago alkene solution even roller brush in the q195 strip surface of step (2), the coating of Graphene
Thickness is 5～50 μm, is placed in the air afterwards and air-dries 15min, obtains q195/ Graphene strip blank；
(4) 6 q195/ Graphene strip blank upper and lower surfaces are fitted tightly together by seam；
(5) using synchronous cold-rolling process, the multi-disc q195/ Graphene strip blank of step (4) is rolled, technique is joined
Number is: roller diameter is 180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is 70%, the second percentage pass reduction
For 40%, the operation of rolling adopts micro tension milling, and tension value is the 1/5 of equal thickness q195 material tensile strength, obtains multilayer q195/
Graphene composite sheet, thickness is 0.5mm；
(6) using synchronous cold-rolling process, multilayer q195/ Graphene composite sheet is thinned to 80 μm, technological parameter is: rolls
Roller diameter 30mm, mill speed 10～50mm/s, tension value is the 1/4 of equal thickness q195 material tensile strength, and percentage pass reduction is
10～15%, it is thinned to target thickness through 10 passages；
(7) adopt cross-shear rolling technique, through 3 passages, the multilayer q195/ Graphene composite strip of step (6) is thinned to 15
μm, technological parameter is: roller diameter 30mm, mill speed 50mm/s, friction speed ratio 1.1～1.4, and tension value is equal thickness q195 material
The 1/3 of tensile strength, percentage pass reduction is 10～40%, and total deformation rate is 99%；
(8) the multilayer q195/ Graphene composite strip in step (7) is thinned to by 3 μ using negative roll gap cross-shear rolling technique
M, technological parameter is: roller diameter 30mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is equal thickness
The 1/3 of q195 material tensile strength, percentage pass reduction is 20～40%, rolls 6 passages, and total deformation rate is 99.9%, prepares
Thickness is that 3 μm of multilayer q195/ Graphene is combined strip in razor-thin.
Multilayer q195/ Graphene manufactured in the present embodiment is combined strip in razor-thin surface smoothness height, and flatness is good, and thickness is equal
Even, the defect such as non-oxidation layer and crackle.Good dispersion degree in q195 matrix for the Graphene, lamella area is big, soilless sticking phenomenon, with
Matrix conjugation is high.
Claims (5)
1. a kind of multiple layer metal/Graphene is combined the preparation method of strip in razor-thin it is characterised in that carrying out according to following processing step:
(1) preparing thickness is 1～20mm, and width is the metal material of 50～500mm, using synchronous cold-rolling process, through 4～10 roads
Secondary metal material is thinned to 0.3～0.9mm, synchronous cold-rolling process parameter is: roller diameter be 100-180mm, mill speed
For 0.5～3m/min, percentage pass reduction is 10～20%, and the operation of rolling adopts mild tension condition, and tension value is equal thickness metal
The 1/5～1/3 of Tensile strength；
(2) by the upper and lower surface polishing of metal sheet band, recycle ultrasonic activation cleaning, parameter be set to ultrasonic water temperature 30～
50 DEG C, scavenging period is 5～10min, is placed in the air and air-dries；
(3) Graphene coating is coated uniformly on the metal sheet band surface of step (2), the coating thickness of Graphene is 5～50 μm,
It is placed in the air afterwards and air-dries 10～30min, obtain Metal/grapheme strip blank；
(4) 2～20 Metal/grapheme strip blank upper and lower surfaces are fitted tightly together；
(5) using synchronous cold-rolling process, the multi-disc Metal/grapheme strip blank of step (4) is rolled, technological parameter is:
Roller diameter is 100-180mm, and mill speed is 0.5～3m/min, and first rolling pass reduction is depressed in 30～70%, second passages
20～50%, the operation of rolling adopts micro tension milling to rate, and tension value is the 1/5～1/3 of equal thickness metal material tensile strength,
Obtain multiple layer metal/Graphene composite sheet, thickness is 0.5～1mm；
(6) using synchronous cold rolling or cross-shear rolling technique, multiple layer metal/Graphene composite sheet is thinned to 80～200 μm,
When using symmetric rolling, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, and tension value is uniform thickness
The 1/5～1/3 of degree metal material tensile strength, percentage pass reduction is 10～15%, is thinned to target thickness through 10～15 passages；
When using asymmetrical rolling, technological parameter is: roller diameter 30～50mm, mill speed 10～60mm/s, and friction speed ratio is
1.05～1.2, tension value is the 1/5～1/3 of equal thickness metal material tensile strength, and percentage pass reduction is 8～15%, through 2～4
Passage is thinned to target thickness；
(7) adopt cross-shear rolling technique, through 3～7 passages, the multiple layer metal of step (6)/Graphene composite strip is thinned to 15
～25 μm, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, friction speed ratio 1.1～1.4, tension value is little
In the 1/2 of equal thickness metal material tensile strength, percentage pass reduction is 10～40%, and total deformation rate is more than 80%；
(8) multiple layer metal in step (7)/Graphene composite strip is thinned to by 1～4 μ using negative roll gap cross-shear rolling technique
M, technological parameter is: roller diameter 30～50mm, mill speed 10～50mm/s, friction speed ratio 1.3～1.6, and tension value is less than etc.
The 1/2 of thick metal material tensile strength, percentage pass reduction is 10～40%, rolls 6～10 passages, and total deformation rate is more than
80%, prepare multiple layer metal/Graphene that thickness is 1～4 μm and be combined strip in razor-thin.
2. a kind of multiple layer metal/Graphene according to claim 1 is combined the preparation method of strip in razor-thin it is characterised in that institute
The metal material stating step (1) is copper, aluminium, molybdenum, nickel, titanium, steel.
3. a kind of multiple layer metal/Graphene according to claim 1 is combined the preparation method of strip in razor-thin it is characterised in that institute
The Graphene coating stating step (3) is the watersoluble plumbago alkene solution of mass concentration 4%, the oiliness Graphene of mass concentration 4% is molten
Liquid, graphene powder.
4. a kind of multiple layer metal/Graphene according to claim 1 is combined the preparation method of strip in razor-thin it is characterised in that institute
The mode that Graphene coating is coated uniformly on metal sheet band surface stating step (3) has two kinds: mode one is by mass concentration
Graphene solution for 4% or graphene powder even roller brush are on metal sheet band surface；Mode two is using cvd method, i.e. profit
With methane as carbon source, Graphene is grown in metal base surface pyrolytic by it, thus uniformly sinking on strip surface
Long-pending Graphene.
5. a kind of multiple layer metal/Graphene according to claim 1 is combined the preparation method of strip in razor-thin it is characterised in that institute
The laminating type stating step (4) has seam, strong metallic glue or rivet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510541161.6A CN105127197B (en) | 2015-08-31 | 2015-08-31 | Preparation method for multi-layer metal/graphene composite electrode thin strip |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510541161.6A CN105127197B (en) | 2015-08-31 | 2015-08-31 | Preparation method for multi-layer metal/graphene composite electrode thin strip |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105127197A CN105127197A (en) | 2015-12-09 |
| CN105127197B true CN105127197B (en) | 2017-01-25 |
Family
ID=54712957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510541161.6A Active CN105127197B (en) | 2015-08-31 | 2015-08-31 | Preparation method for multi-layer metal/graphene composite electrode thin strip |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105127197B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105880284B (en) * | 2016-04-11 | 2018-02-09 | 武汉大学 | A kind of high rigidity high-conductivity copper carbon composite and its preparation method and application |
| CN105845942A (en) * | 2016-06-20 | 2016-08-10 | 山东建筑大学 | Preparation method of nano graphene copper foil |
| WO2018032055A1 (en) * | 2016-08-17 | 2018-02-22 | Newsouth Innovations Pty Limited | Graphene based electrical conductors |
| WO2019000055A1 (en) * | 2017-06-30 | 2019-01-03 | Newsouth Innovations Pty Limited | Fabrication of graphene and graphene composite conductors using graphite |
| CN110125179B (en) * | 2018-02-09 | 2021-03-23 | 常州第六元素材料科技股份有限公司 | Graphene composite metal and preparation method thereof |
| CN110126378B (en) * | 2019-03-26 | 2020-09-15 | 北京石墨烯技术研究院有限公司 | Graphene steel composite material and preparation method and application thereof |
| CN111451514B (en) * | 2020-04-07 | 2022-11-11 | 上海交通大学 | Preparation method of nano-phase reinforced aluminum-based composite board |
| CN114309119B (en) * | 2021-12-29 | 2023-10-20 | 常州大学 | Graphene/copper composite deformed copper-chromium-zirconium alloy layered strip and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6046801A (en) * | 1983-08-23 | 1985-03-13 | Toyo Alum Kk | Manufacture of aluminum foil having metallic layer on its surface |
| CN101797584A (en) * | 2010-02-11 | 2010-08-11 | 山东南山铝业股份有限公司 | Four-pass aluminum foil rolling process |
| US20130248229A1 (en) * | 2012-03-21 | 2013-09-26 | Tyco Electronics Corporation | Electrical conductors and methods of manufacturing electrical conductors |
| CN102688885B (en) * | 2012-06-13 | 2014-07-30 | 中南大学 | Preparation method for synchronously cold-rolling iron foil by using laminated method |
-
2015
- 2015-08-31 CN CN201510541161.6A patent/CN105127197B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105127197A (en) | 2015-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105127197B (en) | Preparation method for multi-layer metal/graphene composite electrode thin strip | |
| US9878528B2 (en) | Preparation method of graphene/metal composite board | |
| US9970101B2 (en) | Metal-free CVD coating of graphene on glass and other dielectric substrates | |
| CN105170652B (en) | A kind of preparation method of multi-layer heterogeneous metal composite strip in razor-thin | |
| CN110665969B (en) | Preparation method of high-performance titanium/steel bimetal composite board | |
| CN108193065B (en) | A kind of preparation method of graphene enhancing Cu-base composites | |
| CN106756195B (en) | A kind of graphene enhancing Cu-base composites and its preparation method and application | |
| CN104477892B (en) | Flaky graphite alkene device prepared by the preparation method of a kind of flaky graphite alkene and use the method | |
| CN113664063B (en) | Preparation method of copper-molybdenum-copper layered composite material | |
| CN107053814A (en) | A kind of preparation method of titanium aluminium/intermetallic Ni-Al compound laminar composite | |
| CN102941702A (en) | Infiltration preparation method of Cu-MoCu-Cu three-layer composite plate | |
| CN112718861B (en) | Light alloy rolling composite forming process method capable of controlling edge crack | |
| CN105648249A (en) | Preparation method for carbon nano tube strengthened aluminum-based multilayer composite material | |
| CN105883779B (en) | A kind of scalable process of CVD growth large-area graphene | |
| CN106830965B (en) | Preparation method and application of nano-carbon material reinforced superhard material matrix composite material | |
| CN105499270A (en) | Preparation method by employing double-face coated jacketing plates to roll foil | |
| CN112222188A (en) | Preparation method of high-purity indium foil | |
| JP2011042828A (en) | Method for producing titanium thin sheet | |
| CN105080998B (en) | The method for preparing unrepeatered transmission titanium steel composite board | |
| CN104227000B (en) | A kind of production method of chromium target | |
| CN105458004A (en) | Low-plastic difficult-to-deform material slab rolling method and mold based on detachable cover | |
| CN108660375A (en) | A kind of application of metal powder material in 3D printing | |
| CN103498120B (en) | Utilize the preparation method of double-clad aluminium sheet rolling ultrathin magnesium alloy sheet or foil | |
| CN114068871A (en) | Composite belt with ultrathin lithium layers coated on two surfaces and preparation method thereof | |
| CN105887041B (en) | A kind of CVD method of inexpensive growing large-area graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |