CN101787589B - Preparation method of graphene film strip with linear section - Google Patents
Preparation method of graphene film strip with linear section Download PDFInfo
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- CN101787589B CN101787589B CN2010101045497A CN201010104549A CN101787589B CN 101787589 B CN101787589 B CN 101787589B CN 2010101045497 A CN2010101045497 A CN 2010101045497A CN 201010104549 A CN201010104549 A CN 201010104549A CN 101787589 B CN101787589 B CN 101787589B
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Abstract
The invention relates to a preparation method of a graphene film strip with a linear section. The method comprises the following steps: in the dry jet wet spinning process of polyacrylonitrile precursors, arranging a hot roll calendering process before steam drafting and after drying densification, wherein the surface temperature of the calendered hot rolls is controlled at 150-200 DEG C, the interval between every two hot rolls is controlled at 0.3-0.55 mm; calendering the precursor with a round section; carrying out steam drafting and thermoforming to prepare a graphene film strip precursor with a linear section; and preoxidating and carburizing to prepare the graphene film strip. The invention has the advantage of simple process; the prepared graphene film strip has outstanding properties, and the tensile strength exceeds 5000 MPa; and the graphene film strip has better orientation structure, the graphene layers of the graphene film strip are more compactly arranged and select preferred orientation in the axial direction, the consistency of every two adjacent graphene layers is good, and several graphene layers are compactly arranged to form a long ordered orientation structure.
Description
Technical field
The present invention relates to a kind of preparation of graphene film band, specially refer to the preparation method of cross sectional shape, belong to technical field of function materials for " one " font polyacrylonitrile-radical graphene film band.
Background technology
Graphene is rated as the highest material of human known strength; It can not only be developed ultra light aircraft material thin as the scraps of paper, make the tough and tensile bulletproof jacket of excess of export; Even also opened one for the manufacturing of " space elevator " cable and fanned the door of " Alibaba ", U.S. scientist confirms that " Graphene " is fit to be used for making space elevator cable fully.And the Graphene reinforced composite materials can not only be made flexible conductive film material; Be applied to the stealth material that the defence and military field prepares antistatic coating, radar absorbing and submarine aircraft; And aspect the energy, has unique two-dimension plane structure owing to Graphene; Make it have very big specific area, thereby be suitable as very much hydrogen storage material.Therefore grapheme material is with a wide range of applications and has the application prospect of potentiality, is becoming material science and Condensed Matter Physics field hot research in recent years rapidly.
Along with people's deepens continuously and preparation method's improvement to Graphene research, and people need the high-quality grapheme material of a large amount of structural integrities.At present, the preparation method that grapheme material is commonly used mainly contains mechanical stripping method, graphite oxide reducing process, solwution method, chemical method etc.Yet the Graphene based on the micromechanics stripping means makes not only yields poorly, and efficient is also very low.Though the graphite oxide reducing process can be prepared a large amount of Graphenes with relatively low cost; Yet the electronic structure of Graphene and perfection of crystal all receive the serious destruction of strong oxidizer; Its electronic property is affected, to a certain degree limit its application at accurate microelectronic.The chemically grown method can be prepared large tracts of land continuously and the graphene film semi-conducting material of excellent performance, however present stage technology immature and higher cost all limited its large-scale application.Realize the final application and the further investigation of Graphene, at first the mass preparation Graphene is realized the control to its pattern and composition simultaneously, and how a large amount of, low cost is prepared high-quality grapheme material and remained a challenging job so far.
In theory, in the Graphene lamella, carbon atom is arranged with short covalent bond, has very strong adhesion.Have very high elastic modelling quantity along Graphene lamella direction, can reach 1000GPa in theory, and be connected with Van der Waals force between graphene film and the graphene film, interfloor distance is longer, is about 0.335nm, a little less than the adhesion.People such as Lee have measured the mechanical property (Lee, C.et al.Science 321,385 (2008)) of single-layer graphene film, and their result of study shows that graphene film is the highest material of present known strength.Therefore infer, equally with sp
2The graphene nanobelt that key combines also should have very excellent mechanical property.Existing patent (U.S. Pat 7071258; US7150840) and document (Takashi K.et al.Nature 331,331 (1988); Herald, R.et al.Carbon 48,964 (2010); Donnet J.B.et al.Carbon 30,787 (1992) shows that the cross section is that the high strength and the high-modulus of circular polyacrylonitrile (PAN) carbon fiber is based on the preferred orientation of thick aromatic ring aspect molecule along fiber axis, and the carbon net length of high bond energy between aspect.Find that simultaneously carbon fiber is made up of height-oriented Graphene lamella, and have tangible anisotropy, high along the fiber axial strength, modulus is high, and lateral performance is poor, intensity is very low.Researched and proposed bar band model (Perret R.et al.Journal ofApplied Crystallography 3 (6) based on polyacrylonitrile-based carbon fiber structural; 525 (1970) and the two-dimensional structure model (Bennett S.C.et al.Carbon 17 (1), 25 (1979)) that proposes based on the ribbon structure model: the elementary cell of bar band model is sp
2The carbon of hydridization is that 5～7nm, average length are that the banded graphene layer of hundreds of nanometer is formed by mean breadth.
Up to now; Domestic do not see adopt calendering technology to make the presoma of circular cross-section process " one " font graphene film band presoma after, adopt the organic and inorganic method for transformation to process the graphene film presoma through pre-oxidation, carbonization the report of high-performance polyacrylonitrile-based graphene film band again.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of cross sectional shape for the graphene film band of " one " font.
A kind of cross sectional shape is the preparation method of the graphene film band of " one " font, comprises the steps:
(1) preparation of graphene film band presoma: the PAN spinning solution is carried out spinning with the dry-jet wet spinning technology; PAN spinning solution thread is first air layer through one section drying after extruding spinnerets; Then through three grades of coagulating bath drawing-offs; Washing, boiling water drawing-off again, oil, compacting by drying gets the cross section and is circular presoma; Then this forerunner's body heat roll-in is prolonged, obtain the graphene film band presoma of cross sectional shape through the drawing-off of secondary saturated vapor, steam heat typing, the dry silk of receiving again for " one " font;
(2) with cross sectional shape be graphene film band presoma pre-oxidation in pre-oxidation furnace of " one " font, the graphene film band of cross sectional shape for " one " font processed in carbonization in middle low temperature carbonization furnace and high temperature carbonization furnace.
Described hot-rolling calendering is rolled hot rod surface temperature range at 150 ℃-200 ℃ for the calendering of two-stage three hot-rollings, and the clearance control between hot-rolling and the hot-rolling is at 0.3-0.05mm.
Described saturated vapor degree of draft is 150 ℃-190 ℃ of 150%-250%, saturated vapor drawing temperatures.
Described steam heat setting temperature is 100 ℃.
Described cross sectional shape is that the graphene film band presoma thickness of " one " font is at the 5-10 mu m range.
Described pre-oxidation temperature is 180-280 ℃, and carburizing temperature is 300-1500 ℃, and the total draft rate is 3%-5% in pre-oxidation and the carbonization, and wire travelling speed is about 0.3m/min.
Technology of the present invention is simple; Be suitable for the production of extensive high-performance graphene film band, preparation be the graphene film band excellent performance of " one " font, met and exceeded the TENSILE STRENGTH of 5000MPa; Structural analysis shows that the graphene film band has reasonable orientation texture; The graphene layer of graphene film band is arranged densification and axially preferred orientation, and adjacent graphene layer continuity is better, and several graphene layers are closely arranged and formed long orderly orientation texture.Stack thickness (the L of graphene layer
c) and the width (L of graphene layer
a) respectively in 1.0～2.7nm and 2.4～5.2nm scope; The interlamellar spacing of graphene layer is between 0.34～0.35nm.G peak and D peak, G (1580-1600cm have all appearred in Raman spectrum
-1) peak is carbon atom (sp in the graphene film layer plane
2Hydridization) stretching vibration peak, D (1350-1370cm
-1) peak is the stretching vibration peak of Graphene lamella edge carbon atom, G peak right flank 1620cm simultaneously
-1Near also have a satellite peak, this is because the variation of Graphene surface carbon atom causes, the distortion of the Graphene plane of networks of carbon atoms, the distance on the network plane between the carbon atom reduces.
Description of drawings
Fig. 1 is calendering technology structural model figure among the present invention (from pipe, dripping to water between the hot-rolling and be temperature greater than 95 ℃ deionized water);
Fig. 2 is the section S EM figure of polyacrylonitrile-radical graphene film band presoma among the present invention;
Fig. 3 is the Raman spectrum of polyacrylonitrile-radical graphene film band (BM1 and BM2) among the present invention;
Fig. 4 is polyacrylonitrile-radical graphene film band (BM1 and BM2) XRD diffracting spectrum among the present invention;
Fig. 5 (a) is the low power image for the HRTEM image of polyacrylonitrile-radical graphene film band among the present invention, and the white arrow direction is the direction of principal axis of graphene film band; (f) for scheming the high power image at F place in (a).
The specific embodiment
Cross sectional shape is the preparation method of the graphene film band of " one " font:
At first adopting the aqueous phase precipitation polymerization to obtain viscosity average molecular weigh is 200,000; Molecular weight distribution is the polyacrylonitrile powder of 1.5-2.0; The polyacrylonitrile powder is at 60 ℃ down after washing, the vacuumize, according to a certain ratio (polyacrylonitrile powder quality concentration 20%, dimethyl sulfoxide (DMSO) mass concentration are 80%) and dimethyl sulfoxide (DMSO) under the pure nitrogen gas protection in polymeric kettle obtain solution; Solution temperature is 60 ℃, through vacuum defoamation, filter that to obtain temperature be 60 ℃ spinning solution.Spinning solution arrives spinnerets after the measuring pump metering of 1.2CC, spinnerets adopts 100 ℃ of water jacket insulations with the pipeline of carrying spinning solution.The platinum-rhodium alloy The hole diameter of spinneret is that 0.01mm, hole count are 1000, carries out spinning with the dry-jet wet spinning technology.PAN spinning solution thread remains on the air layer of 10mm earlier through the thickness of one section drying after extruding spinnerets; Then through three grades of coagulating bath drawing-offs; Washing, boiling water drawing-off, oil, compacting by drying (three grades of coagulating bath drawing-offs, washing, boiling water drawing-offs, oil, the compacting by drying operation is prior art), hot-rolling calendering, the drawing-off of secondary saturated vapor, steam heat typing, the dry silk of receiving obtain the graphene film band presoma that cross sectional shape is " one " font; Wherein the drawing-off of secondary saturated vapor is preceding with being provided with calendering technology behind the compacting by drying; The hot rod surface temperature range of control calendering is at 150 ℃, and the clearance control between hot-rolling and the hot-rolling is at 0.2mm.The graphene film band presoma of cross sectional shape for " one " font processed in steam drafting (the steam drafting rate is 150%, and the steam drafting temperature is 170 ℃) and steam heat typing (temperature is 100 ℃), and the section thickness of this graphene film band presoma is 12 μ m.
Graphene film band presoma carries out pre-oxidation and carbonization in pre-oxidation furnace and carbide furnace; The pre-oxidation temperature in 10 stove districts is 195 ℃, 210 ℃, 215 ℃, 225 ℃, 235 ℃, 245 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ successively; Middle low temperature carbonization furnace and high temperature carbonization furnace are horizontal chamber furnace (oven); 4 and 2 warm areas are respectively arranged, and middle low temperature is 350～700 ℃, and high temperature is 1500 ℃.The carbonization protective gas adopts nitrogen content up to 99.9999% high pure nitrogen.Graphene film band presoma total draft rate in pre-oxidation furnace and carbide furnace is 3%, and wire travelling speed is about 0.3m/min.Processed the graphene film band of cross sectional shape for " one " font, promptly cross sectional shape is the polyacrylonitrile-radical graphene film band of " one " font.。
The cross sectional shape of preparation is 5000MPa for the TENSILE STRENGTH of " one " font polyacrylonitrile-radical graphene film band.
Embodiment 2
Cross sectional shape is the preparation method of the graphene film band of " one " font:
At first adopting the aqueous phase precipitation polymerization to obtain viscosity average molecular weigh is 250,000; Molecular weight distribution is the polyacrylonitrile powder of 1.5-2.0; The polyacrylonitrile powder is at 60 ℃ down after washing, the vacuumize, according to a certain ratio (polyacrylonitrile powder quality concentration 20%, dimethyl sulfoxide (DMSO) mass concentration are 80%) and dimethyl sulfoxide (DMSO) under the pure nitrogen gas protection in polymeric kettle obtain solution; Solution temperature is 60 ℃, through vacuum defoamation, filter that to obtain temperature be 60 ℃ spinning solution.Spinning solution arrives spinnerets after the measuring pump metering of 1.2CC, spinnerets adopts 100 ℃ of water jacket insulations with the pipeline of carrying spinning solution.The platinum-rhodium alloy The hole diameter of spinneret is that 0.01mm, hole count are 1000, carries out spinning with the dry-jet wet spinning technology.PAN spinning solution thread remains on the air layer of 10mm earlier through the thickness of one section drying after extruding spinnerets; Then through three grades of coagulating bath drawing-offs; Washing, boiling water drawing-off again, oil, compacting by drying, hot-rolling calendering, the drawing-off of secondary saturated vapor, steam heat typing, the dry silk (three grades of coagulating bath drawing-offs, washing, boiling water drawing-offs, oil, the compacting by drying operation is prior art) of receiving obtain the graphene film band presoma of cross sectional shape for " one " type; Wherein the drawing-off of secondary saturated vapor is preceding with being provided with calendering technology behind the compacting by drying; The hot rod surface temperature range of control calendering is at 165 ℃, and the clearance control between hot-rolling and the hot-rolling is at 0.1mm.(the saturated vapor degree of draft is 200% in the saturated vapor drawing-off; The saturated vapor drawing temperature is 180 ℃) and steam heat typing (temperature is 100 ℃) processed the graphene film band presoma of cross sectional shape for " one " font, the section thickness of this graphene film band presoma is 10 μ m.Cross sectional shape carries out pre-oxidation and carbonization for the graphene film band presoma of " one " font in pre-oxidation furnace and carbide furnace, the pre-oxidation temperature in 10 stove districts is 185 ℃, 205 ℃, 220 ℃, 225 ℃, 235 ℃, 245 ℃, 255 ℃, 260 ℃, 265 ℃, 280 ℃ successively; Middle low temperature is 350～700 ℃, and high temperature is 1500 ℃.The carbonization protective gas adopts nitrogen content up to 99.9999% high pure nitrogen.Graphene film band presoma total draft rate in pre-oxidation furnace and carbide furnace is 4%, and wire travelling speed is about 0.3m/min.Processed the graphene film band of cross sectional shape for " one " font, promptly cross sectional shape is the polyacrylonitrile-radical graphene film band of " one " font.
The cross sectional shape of preparation is 5100MPa for the TENSILE STRENGTH of the polyacrylonitrile-radical graphene film band of " one " font.
Embodiment 3
Cross sectional shape is the preparation method of the graphene film band of " one " font:
At first adopting the aqueous phase precipitation polymerization to obtain viscosity average molecular weigh is 300,000; Molecular weight distribution is the polyacrylonitrile powder of 1.5-2.0; The polyacrylonitrile powder is at 60 ℃ down after washing, the vacuumize, according to a certain ratio (polyacrylonitrile powder quality concentration 20%, dimethyl sulfoxide (DMSO) mass concentration are 80%) and dimethyl sulfoxide (DMSO) under the pure nitrogen gas protection in polymeric kettle obtain solution; Solution temperature is 60 ℃, through vacuum defoamation, filter that to obtain temperature be 60 ℃ spinning solution.Spinning solution arrives spinnerets after the measuring pump metering of 1.2CC, spinnerets adopts 100 ℃ of water jacket insulations with the pipeline of carrying spinning solution.The platinum-rhodium alloy The hole diameter of spinneret is that 0.01mm, hole count are 1000, carries out spinning with the dry-jet wet spinning technology.PAN spinning solution thread after extruding spinnerets earlier through the thickness of one section drying remain on behind the air layer of 10mm through three grades of coagulating bath drawing-offs, washing, boiling water drawing-off, oil, compacting by drying, hot-rolling calendering, the drawing-off of secondary saturated vapor, steam heat typing, the dry silk (three grades of coagulating bath drawing-offs, washing, boiling water drawing-offs, oil, compacting by drying is operated is prior art) of receiving obtain graphene film band presoma; Wherein the drawing-off of secondary saturated vapor is preceding with being provided with calendering technology behind the compacting by drying; The hot rod surface temperature range of control calendering is at 175 ℃, and the clearance control between hot-rolling and the hot-rolling is at 0.1mm.(secondary saturated vapor degree of draft is 250% to the drawing-off of secondary saturated vapor; The saturated vapor drawing temperature is 190 ℃) and steam heat typing (temperature is 100 ℃) processed the graphene film band presoma of cross sectional shape for " one " font, the section thickness of this graphene film band presoma is at 7 μ m.Graphene film band presoma carries out pre-oxidation and carbonization in pre-oxidation furnace and carbide furnace, the pre-oxidation temperature in 10 stove districts is 195 ℃, 210 ℃, 215 ℃, 225 ℃, 230 ℃, 245 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ successively; Middle low temperature is 350～700 ℃, and high temperature is 1500 ℃.The carbonization protective gas adopts nitrogen content up to 99.9999% high pure nitrogen.Graphene film band presoma total draft rate in pre-oxidation furnace and carbide furnace is 3%, and wire travelling speed is about 0.3m/min.Processed the graphene film band of cross sectional shape for " one " font, promptly cross sectional shape is the polyacrylonitrile-radical graphene film band of " one " font.
The cross sectional shape of preparation is 5070MPa for the TENSILE STRENGTH of the polyacrylonitrile-radical graphene film band of " one " font.
Embodiment 4
Cross sectional shape is the preparation method of the graphene film band of " one " font:
At first adopting the aqueous phase precipitation polymerization to obtain viscosity average molecular weigh is 400,000; Molecular weight distribution is the polyacrylonitrile powder of 1.5-2.0; The polyacrylonitrile powder is at 60 ℃ down after washing, the vacuumize, according to a certain ratio (polyacrylonitrile powder quality concentration 20%, dimethyl sulfoxide (DMSO) mass concentration are 80%) and dimethyl sulfoxide (DMSO) under the pure nitrogen gas protection in polymeric kettle obtain solution; Solution temperature is 60 ℃, through vacuum defoamation, filter that to obtain temperature be 60 ℃ spinning solution.Spinning solution arrives spinnerets after the measuring pump metering of 1.2CC, spinnerets adopts 100 ℃ of water jacket insulations with the pipeline of carrying spinning solution.The platinum-rhodium alloy The hole diameter of spinneret is that 0.01mm, hole count are 1000, carries out spinning with the dry-jet wet spinning technology.PAN spinning solution thread remains on the air layer of 10mm earlier through the thickness of one section drying after extruding spinnerets; Then through three grades of coagulating bath drawing-offs, washing, boiling water drawing-off, oil, compacting by drying, hot-rolling calendering, the drawing-off of secondary saturated vapor, steam heat typing, the dry silk (three grades of coagulating bath drawing-offs, washing, boiling water drawing-offs, oil, the compacting by drying operation is prior art) of receiving obtain graphene film band presoma; Wherein the drawing-off of secondary saturated vapor is preceding with being provided with calendering technology behind the compacting by drying; The hot rod surface temperature range of control calendering is at 185 ℃, and the clearance control between hot-rolling and the hot-rolling is at 0.1mm.(the steam drafting rate is 200% in the saturated vapor drawing-off; The steam drafting temperature is 190 ℃) and steam heat typing (temperature is 100 ℃) processed the graphene film band presoma of cross sectional shape for " one " font, the section thickness of this graphene film band presoma is at 10 μ m.Graphene film band presoma carries out pre-oxidation and carbonization in pre-oxidation furnace and carbide furnace, the pre-oxidation temperature in 10 stove districts is 185 ℃, 200 ℃, 220 ℃, 230 ℃, 240 ℃, 245 ℃, 255 ℃, 260 ℃, 265 ℃, 280 ℃ successively; Middle low temperature is 350～700 ℃, and high temperature is 1500 ℃.The carbonization protective gas adopts nitrogen content up to 99.9999% high pure nitrogen.Graphene film band presoma total draft rate in pre-oxidation furnace and carbide furnace is 4%, and wire travelling speed is about 0.3m/min.Processed the graphene film band of cross sectional shape for " one " font, promptly cross sectional shape is the polyacrylonitrile-radical graphene film band of " one " font.
The cross sectional shape of preparation is 5100MPa for the TENSILE STRENGTH of the polyacrylonitrile-radical graphene film band of " one " font.
Claims (3)
1.
OnePlanting cross sectional shape is the preparation method of the graphene film band of " one " font, it is characterized in that comprising the steps:
(1) preparation of graphene film band presoma: the PAN spinning solution is carried out spinning with the dry-jet wet spinning technology; PAN spinning solution thread is first air layer through one section drying after extruding spinnerets; Then through three grades of coagulating bath drawing-offs; Washing, boiling water drawing-off again, oil, compacting by drying gets the cross section and is circular presoma; Then this forerunner's body heat roll-in is prolonged, described hot-rolling calendering is the calendering of two-stage three hot-rollings, and calendering hot-rolling surface temperature range is at 150 ℃-200 ℃; Clearance control between hot-rolling and the hot-rolling obtains the graphene film band presoma of cross sectional shape for " one " font through the drawing-off of secondary saturated vapor, steam heat typing, the dry silk of receiving again at 0.3-0.05mm;
(2) with cross sectional shape be graphene film band presoma pre-oxidation in pre-oxidation furnace of " one " font; Carbonization in middle low temperature carbonization furnace and high temperature carbonization furnace; Described pre-oxidation temperature is 180-280 ℃, and carburizing temperature is 300-1500 ℃, and the total draft rate is 3%-5% in pre-oxidation and the carbonization; Wire travelling speed is 0.3m/min, has processed the graphene film band of cross sectional shape for " one " font.
2. be the preparation method of the graphene film band of " one " font according to the described a kind of cross sectional shape of claim 1, it is characterized in that described steam heat setting temperature is 100 ℃.
3. be the preparation method of the graphene film band of " one " font according to the described a kind of cross sectional shape of claim 1, it is characterized in that described cross sectional shape is that the graphene film band presoma thickness of " one " font is at the 5-10 mu m range.
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| TW201431902A (en) * | 2012-11-16 | 2014-08-16 | 巴斯夫歐洲公司 | Polymeric precursors for producing graphene nanoribbons and suitable oligophenylene monomers for preparing them |
| CN104669597A (en) * | 2015-02-28 | 2015-06-03 | 浙江海轮绳网有限公司 | Wire drawing roller set and wire drawing machine applying same and wire drawing secondary-shaping method |
| CN106554006B (en) * | 2015-09-25 | 2019-07-02 | 国家纳米科学中心 | A kind of carbon material, preparation method and applications |
| CN106894113A (en) * | 2017-02-21 | 2017-06-27 | 东华大学 | A kind of graphene oxide dry-jet wet-spinning spinning process |
| CN109801758B (en) * | 2018-12-27 | 2020-08-28 | 中国科学院山西煤炭化学研究所 | Preparation process of graphene conductive film |
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