CN104198380B - Equipment and method for observing grapheme grain boundary on line - Google Patents
Equipment and method for observing grapheme grain boundary on line Download PDFInfo
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- CN104198380B CN104198380B CN201410476770.3A CN201410476770A CN104198380B CN 104198380 B CN104198380 B CN 104198380B CN 201410476770 A CN201410476770 A CN 201410476770A CN 104198380 B CN104198380 B CN 104198380B
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Abstract
The invention discloses equipment and method for observing a grapheme grain boundary on line. The equipment comprises a grapheme processing main body mechanism and an observing mechanism; the grapheme processing main body mechanism comprises a processing cavity, a conveying belt, a plurality of cleaning boxes and an ultraviolet lamp; the conveying belt is positioned at the bottom of the processing cavity; the cleaning boxes are arranged on the conveying belt and are conveyed by the conveying belt; the ultraviolet lamp is arranged on the inner wall of the top of the processing cavity; and the observing mechanism comprises a microscope. According to the invention, the grapheme grain boundary of a large area of grapheme thin film can be observed on line; the production line design can save time cost; the grapheme grain boundary is more rapidly observed; and the integral equipment has a simple structure, is low in cost, is convenient to operate and is beneficial to production operation of the industrial production line.
Description
Technical field
The present invention relates to a kind of equipment of online observation Graphene crystal boundary and its observation procedure.
Background technology
Graphene is that novoselov and geim of 2004 Nian Man Chester universities finds, it has good physics, change
The excellent properties of each side such as, electricity, mechanics, have extensively in numerous areas such as new forms of energy, new material and electronic devices and components
Application prospect.The current preparation method of Graphene mainly has: (1) microcomputer stripping method, this method can only production quantity few
Graphene, predominantly stay on laboratory level；(2) epitaxy, this method major defect be relatively costly and silicon chip relatively
Its large-scale application of little size limitation；(3) oxidation-reduction method, the Graphene defect that the method produces is more；(4) solvent stripping
From method, the method is main be shortcoming be production efficiency than its business application of lower limit；(5) chemical vapour deposition technique, i.e. cvd
Method, the crystal structure of graphite that this method produces is relatively complete, and quality is higher, can be used for transparency electrode, Flat panel touch display screen etc..Chemical gas
The principle of phase sedimentation is that one or more gaseous material is imported to generation chemical reaction in a reaction chamber, and in substrate
Deposit a kind of material.The matrix material of Graphene preparation is usually various metals, including Copper Foil, nickel foil, platinum etc., wherein due to
Copper Foil low price and preferably and the number of plies is relatively easy to control and can be used for large-scale production for the Graphene quality that grows.Depositing operation is complete
Cheng Hou, needs to transfer graphene to reuse on required substrate by rotor technique.
During industrialized mass production Graphene, generally adopt the cvd preparation method of diffusion furnace, deposition life on Copper Foil
Long large-area graphene film.Sheet resistance and transmitance are the important indicators characterizing the Graphene quality prepared.Graphene crystal grain
Size has close associating with Graphene sheet resistance.In Graphene forming core growth stage, Graphene island slowly grows formation graphite
Alkene crystal grain, has the crystal boundary of Graphene between crystal grain and crystal grain.By observing Graphene crystal boundary, can be calculated by statistics
Go out the size of the Graphene crystallite dimension of growth, such that it is able to adjust production technology, prepare higher-quality graphene film.
But although the information that on Graphene crystal boundary, atom is recombinated can be obtained by tem and stm observation, but with regard to large area stone
On black alkene thin film, the distributed intelligence of Graphene crystal boundary is but difficult to obtain by instrument at this stage.And shown by research, graphite
Alkene crystal boundary also contributes to the properties of Graphene and related product attribute.
The existing method observing Graphene crystal boundary rests essentially within laboratory stage, complicated using certain operations, price
High laboratory equlpment, such as tem, sem, uv analyzer etc. are observed, and need the complicated technique of multiple tracks, such as
Graphene is transferred to liquid crystal, the method using optical birefringence observes Graphene crystal boundary.However, this kind of method also can be seen simultaneously
Measure the crystal boundary at cuprio bottom, and Graphene crystal boundary extraordinary image, it is difficult to differentiate, and time-consuming very long, it is highly detrimental to industrial metaplasia
Product demand.For synthesis, the defect that existing observation exists is: the Graphene crystal boundary that (1) observes graphene film rests on reality
Test the room stage it is impossible to online observation；(2) observe the Graphene crystal boundary complex process of graphene film, take longer；(3) observe
The equipment price that Graphene crystal boundary uses is high；(4) complex operation, and the graphene film of minimum area can only be observed.
Content of the invention
First purpose of the present invention is to solve the problems, such as prior art, provides one kind being capable of online observation large area
The equipment of the Graphene crystal boundary of graphene film.
The technical scheme realizing first purpose of the present invention is a kind of equipment of online observation Graphene crystal boundary, including graphite
Alkene processes main body mechanism and observation element；Described Graphene process main body mechanism include processing chamber, conveyer belt, multiple clean box and
Burdick lamp；Described conveyer belt is located at the bottom of processing chamber；Described clean box is arranged on a moving belt, is transmitted by conveyer belt；Institute
State on the inwall at the top that Burdick lamp is arranged on processing chamber；Described observation element includes microscope.
In order to obtain more preferable effect, the ultraviolet wavelength of described Burdick lamp transmitting is 187～400nm, power of lamp tube
Not less than 100w.
The processing chamber that described Graphene processes main body mechanism is semi-closed structure that side is opened wide or carry can folding
The full-closed structure of door.Such enclosed construction not only contributes to the formation of wet environment, and can freely put into Graphene
Film sample.
Due to quartz burner heating, temperature is higher, needs to take waste heat away, makes to be maintained at one in cavity suitably
Temperature, therefore described Graphene processes main body mechanism and also includes taking out hot channel；Described hot channel of taking out is arranged in processing chamber, with place
The connection of reason intracavity portion.
In order to allow graphene film surface low-level oxidation, thus the observation of crystal boundary of being more convenient for, online observation Graphene crystal boundary
Equipment also includes Graphene pretreatment mechanism；Described Graphene pretreatment mechanism is baking platform.
In order to can determine that time and the temperature of pretreatment, described baking platform setting intervalometer and incubator.
In order to manufacture wet environment in cavity, described Graphene processes main body mechanism and also includes being arranged in processing chamber
Humidifier.Described Graphene processes the humidity inductive probe that main body mechanism also includes being arranged in processing chamber.
Described observation element also includes the computer being connected with microscope；Described microscope is metallurgical microscope.
Described conveyer belt adopts the crawler belt of the Teflon material high temperature resistant, ultraviolet will not deform under irradiating.
Second object of the present invention is the method providing a kind of line of convenient and reliable operation to observe Graphene crystal boundary, adopts
The equipment of aforesaid online observation Graphene crystal boundary；Comprise the following steps:
Step one: the graphene film prepared carries out toasting pre- place by the baking platform of Graphene pretreatment mechanism
Reason, between 100 DEG C～250 DEG C, the time is 5-10min to temperature control；
Step 2: graphene film is put into clean box；Open Burdick lamp to be irradiated；Set the operation speed of conveyer belt
Spend, for this clean box, 5-25min is needed by whole processing chamber；Control process chamber interior humidity is 20%～80%；Described ultraviolet
The ultraviolet wavelength of line lamp transmitting controls in 187～400nm；
Step 3: observed by microscope, observed result is analyzed and is shown by computer.
Employ technique scheme, the present invention has a following beneficial effect:
(1) present invention is capable of the Graphene crystal boundary of online observation large-area graphene film, and the pipeline design can be saved
Time cost, more rapidly observes Graphene crystal boundary, and whole device framework is simple, low cost, easy to operate, beneficial to industrialization
The production operation of streamline.
(2) present invention is additionally provided with pretreatment mechanism, and graphene film is carried out with roasting pretreatment, thus can be to Graphene
Film surface low-level oxidation is so that the crystal boundary that wet environment ultraviolet irradiates lower Graphene is more prone to observe, particularly with original
Just there is the graphene film of growth defect even more extremely beneficial.
(3) processing chamber of the present invention is used for integrated various equipment, and semiclosed or full closeding state is conducive to wet environment
Formation, and semiclosed or switching door then can freely put into graphene film sample.
(4) humidifier of the present invention and humidity inductive probe can manufacture wet environment in cavity, and real-time monitoring
Humidity in cavity is it is ensured that humidity is 20%～80%.
(5) present invention radiates ultraviolet using quartz burner, for providing energy, so that reaction is carried out, reaction
The hydrone in wet environment is enable to be cracked into oxygen and hydroxide groups, then oxygen and hydroxide groups can pass through Graphene
Crystal boundary optionally spreads, and Strong oxdiative grows the metal substrate of graphene film.Metal substrate after oxidation serves as a contrast compared to original
The crystallite dimension at bottom is bigger.Change with substrate crystal boundary is big, and at this moment Graphene crystal boundary just can show elongated black line shape, permissible
Clear observation, and ultraviolet wavelength is shorter, and energy is higher, and the ultraviolet of upper wavelength cannot complete the transition of energy, unfavorable
Hydrone in wet environment is cracked into oxonium ion and hydroxide ion group.
(5) the conveyor materials Teflon of the present invention, can be high temperature resistant, and ultraviolet will not deform under irradiating.
(6) present invention, using the metallurgical microscope being connected with computer, can conveniently observe Graphene crystal boundary, and
Tem and stm high with respect to price, can not only observe large-area graphene film and price is relatively cheap a lot.
Brief description
In order that present disclosure is easier to be clearly understood, below according to specific embodiment and combine accompanying drawing, right
The present invention is described in further detail, wherein
Fig. 1 is the structural representation of the present invention.
It is numbered in accompanying drawing:
Graphene processes main body mechanism 1, processing chamber 11, conveyer belt 12, clean box 13, Burdick lamp 14, takes out heat pipe
Road 15, humidifier 16, humidity inductive probe 17, observation element 2, microscope 21, computer 22, Graphene pretreatment mechanism
3；Graphene film 4.
Specific embodiment
(embodiment 1)
See Fig. 1, a kind of equipment of online observation Graphene crystal boundary of the present embodiment, including Graphene process main body mechanism 1,
Observation element 2 and Graphene pretreatment mechanism 3.Graphene processes main body mechanism 1 and includes processing chamber 11, conveyer belt 12, Duo Gejie
Net box 13, Burdick lamp 14, take out hot channel 15, humidifier 16 and humidity inductive probe 17.Processing chamber 11 open wide for side half
Enclosed construction or with can folding door full-closed structure.Conveyer belt 12 is located at the bottom of processing chamber 11, using Teflon
Material；Clean box 13 is arranged on the conveyor belt 12, is transmitted by conveyer belt 12；Burdick lamp 14 is arranged on the top of processing chamber 11
On inwall, the ultraviolet wavelength of Burdick lamp 14 transmitting is 187～400nm, and power of lamp tube is not less than 100w；Take out hot channel 15 to set
Put in processing chamber 11, connect with processing chamber 11 inside；Humidifier 16 and humidity inductive probe 17 are arranged in processing chamber 11.
Observation element 2 includes connected microscope 21 and computer 22, and microscope 21 is metallurgical microscope.Graphene pretreatment mechanism 3 is
Baking platform, baking platform setting intervalometer and incubator.
Carry out according to the following steps during detection: step one: the graphene film prepared passes through Graphene preprocessor
The baking platform of structure 3 carries out toasting pretreatment, and between 100 DEG C～250 DEG C, the time is 5-10min to temperature control；
Step 2: graphene film 4 is put into clean box 13；Open Burdick lamp 14 to be irradiated；Set conveyer belt 12
The speed of service for this clean box 13,5-25min is needed by whole processing chamber 11；Control process chamber 11 interior humidity is 20%
～80%；The ultraviolet wavelength of Burdick lamp 14 transmitting controls in 187～400nm.
Step 3: observed by microscope 21, observed result is analyzed and is shown by computer 22.
Particular embodiments described above, has carried out detailed further to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail bright, be should be understood that the specific embodiment that the foregoing is only the present invention, be not limited to the present invention, all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvement done etc., should be included in the guarantor of the present invention
Within the scope of shield.
Claims (11)
1. a kind of equipment of online observation Graphene crystal boundary it is characterised in that: include Graphene process main body mechanism (1) and observe
Mechanism (2)；Described Graphene processes main body mechanism (1) and includes processing chamber (11), conveyer belt (12), multiple clean box (13) and purple
Outside line lamp (14)；Described conveyer belt (12) is located at the bottom of processing chamber (11)；Described clean box (13) is arranged on conveyer belt (12)
On, transmitted by conveyer belt (12)；Described Burdick lamp (14) is arranged on the inwall at top of processing chamber (11)；Described observation machine
Structure (2) includes microscope (21)；Described Graphene processes the humidifier that main body mechanism (1) also includes being arranged in processing chamber (11)
(16).
2. a kind of online observation Graphene crystal boundary according to claim 1 equipment it is characterised in that: described Burdick lamp
(14) ultraviolet wavelength launched is 187～400nm, and power of lamp tube is not less than 100w.
3. a kind of online observation Graphene crystal boundary according to claim 2 equipment it is characterised in that: at described Graphene
Reason main body mechanism (1) processing chamber (11) be side open wide semi-closed structure or carry can folding door totally-enclosed knot
Structure.
4. a kind of online observation Graphene crystal boundary according to claim 3 equipment it is characterised in that: at described Graphene
Reason main body mechanism (1) also includes taking out hot channel (15)；Described hot channel (15) of taking out is arranged in processing chamber (11), with processing chamber
(11) internal connection.
5. a kind of online observation Graphene crystal boundary according to claim 4 equipment it is characterised in that: also include Graphene
Pretreatment mechanism (3)；Described Graphene pretreatment mechanism (3) is baking platform.
6. a kind of online observation Graphene crystal boundary according to claim 5 equipment it is characterised in that: described baking platform
Setting intervalometer and incubator.
7. a kind of online observation Graphene crystal boundary according to claim 6 equipment it is characterised in that: at described Graphene
Reason main body mechanism (1) also includes humidity inductive probe (17) being arranged in processing chamber (11).
8. a kind of online observation Graphene crystal boundary according to claim 7 equipment it is characterised in that: described observation element
(2) also include the computer (22) being connected with microscope (21)；Described microscope (21) is metallurgical microscope.
9. a kind of online observation Graphene crystal boundary according to claim 8 equipment it is characterised in that: described conveyer belt
(12) adopt the crawler belt of Teflon material.
10. a kind of method of online observation Graphene crystal boundary it is characterised in that: using the online observation stone described in claim 9
The equipment of black alkene crystal boundary；Comprise the following steps:
Step one: the graphene film prepared carries out toasting pretreatment by the baking platform of Graphene pretreatment mechanism (3),
Between 100 DEG C～250 DEG C, the time is 5-10min to temperature control；
Step 2: graphene film (4) is put into clean box (13)；Open Burdick lamp (14) to be irradiated；Set conveyer belt
(12) the speed of service needs 5-25min for this clean box (13) by whole processing chamber (11)；
Step 3: observed by microscope (21), observed result is analyzed and is shown by computer (22).
A kind of 11. methods of online observation Graphene crystal boundary according to claim 10 it is characterised in that: described step 2
In, control process chamber (11) interior humidity is 20%～80%；The ultraviolet wavelength that described Burdick lamp (14) is launched controls
187～400nm.
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| CN201410476770.3A CN104198380B (en) | 2014-09-17 | 2014-09-17 | Equipment and method for observing grapheme grain boundary on line |
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| CN201410476770.3A CN104198380B (en) | 2014-09-17 | 2014-09-17 | Equipment and method for observing grapheme grain boundary on line |
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| CN104198380B true CN104198380B (en) | 2017-01-25 |
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| CN107024431A (en) * | 2016-08-31 | 2017-08-08 | 无锡东恒新能源科技有限公司 | A kind of graphene crystal boundary observation and analysis equipment |
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Effective date of registration: 20190911 Address after: 213149 Jiangsu province west of the city of Changzhou Taihu science and Technology Industrial Park orchid Road No. 8 Patentee after: Changzhou two-dimensional warm ene Technology Co., Ltd. Address before: 213000 No. 6 Xiangyun Road, Wujin Economic Development Zone, Jiangsu, Changzhou Patentee before: 2D CARBON (CHANGZHOU) TECH INC., LTD. |