CN107731637B - It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method - Google Patents

It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method Download PDF

Info

Publication number
CN107731637B
CN107731637B CN201710851247.8A CN201710851247A CN107731637B CN 107731637 B CN107731637 B CN 107731637B CN 201710851247 A CN201710851247 A CN 201710851247A CN 107731637 B CN107731637 B CN 107731637B
Authority
CN
China
Prior art keywords
graphene
zno
graphene oxide
pmma
block
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
Application number
CN201710851247.8A
Other languages
Chinese (zh)
Other versions
CN107731637A (en
Inventor
陈海霞
丁继军
屈永锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Shiyou University
Original Assignee
Xian Shiyou University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Xian Shiyou University filed Critical Xian Shiyou University
Priority to CN201710851247.8A priority Critical patent/CN107731637B/en
Publication of CN107731637A publication Critical patent/CN107731637A/en
Application granted granted Critical
Publication of CN107731637B publication Critical patent/CN107731637B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
    • H01J1/02Main electrodes
    • H01J1/30Cold cathodes, e.g. field-emissive cathode
    • H01J1/304Field-emissive cathodes
    • H01J1/3042Field-emissive cathodes microengineered, e.g. Spindt-type
    • H01J1/3044Point emitters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02Manufacture of electrodes or electrode systems
    • H01J9/022Manufacture of electrodes or electrode systems of cold cathodes
    • H01J9/025Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Cathode-Ray Tubes And Fluorescent Screens For Display (AREA)
  • Cold Cathode And The Manufacture (AREA)

Abstract

The present invention is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method, can finely control to the Flied emission of miniature emitting area, while same emitter top can be realized the Flied emission of different current densities and intensity.The adjusted and controlled Flied emission includes silicon base, and the ZnO nano array of vertical arrangement growth on a silicon substrate is coated on the surface emitting layer on ZnO nano array top, the gold electrode of surface emitting layer two sides setting, the additional electrodes that surface emitting layer top is arranged;Surface emitting layer is in that the graphene oxide block being wholely set and graphene block form by structure;Graphene oxide block is filled in laterally and/or longitudinally interval setting, remaining area by graphene block;Graphene oxide block is alternate from the graphene block of different-thickness and different reducing degrees to form miniature emitting area;Voltage is driven in connecting on gold electrode, applied voltage is connected in additional electrodes, and silicon base connects ground wire.

Description

It is a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission And method
Technical field
The present invention relates to the regulations of the Flied emission of cold cathode structure, specially a kind of to be based on graphene oxide/graphene-ZnO The Flied emission of micro-structure is adjusted and controlled and method.
Background technique
The research work of cold-cathode material is concentrated mainly at present prepares the excellent new material of field emission performance, or grinds The person of studying carefully is modified existing emissive material by nanoparticle and forms new transmitting composite material, but after this preparation or modification Emitter material be only Flied emission electric current on the entire cold cathode of increase of macroscopic view, as shown in figure 5, and can not achieve at certain On one emitter in specific region emission current control, the emission current in region miniature on emitter can not also be realized Modulation.And in existing cold-cathode material test, it can only once emit the electric current of a kind of density and intensity, be unable to satisfy reality Demand, test efficiency is low;If carrying out a variety of tests, it can only be that parameter goes to test one by one one by one, entirely emit material It can not be also miniaturized in the field regulation of material, cannot achieve the cold cathode emitters material really in fine and smooth fine display technology Material.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of based on graphene oxide/micro- knot of graphene-ZnO The Flied emission of structure is adjusted and controlled and method, simple in sturcture, ingenious in design, can carry out to the Flied emission of miniature emitting area fine Control, while same emitter top can be realized the Flied emission of different current densities and intensity.
The present invention is to be achieved through the following technical solutions:
It is a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission, including silicon base, vertical row The ZnO nano array of column growth on a silicon substrate, is coated on the surface emitting layer on ZnO nano array top, surface emitting layer two The gold electrode of side setting, the additional electrodes that surface emitting layer top is arranged;
The surface emitting layer is in that the graphene oxide block being wholely set and graphene block form by structure;It is described Graphene oxide block laterally and/or longitudinally interval setting, remaining area by graphene block fill;Graphite oxide Alkene block is alternate from the graphene block of different-thickness and different reducing degrees to form miniature emitting area;
Voltage is driven in connecting on the gold electrode, applied voltage is connected in the additional electrodes, and silicon base connects ground wire.
Preferably, the graphene oxide block on the surface emitting layer and graphene block are arranged in checkerboard;Phase Neighbour is formed in criss-cross five graphene blocks, and intermediate graphene block thickness is minimum.
Preferably, the minimum 0.34nm of thickness difference between the alkene block of adjoining graphite two-by-two of the surface emitting layer, oxygen The thickness of graphite alkene block is identical, and surface emitting layer is with a thickness of 0.8-30nm.
Preferably, the interior voltage swing for driving voltage is less than 5V;The voltage swing of applied voltage is not higher than 300V.
It is a kind of that method is regulated and controled based on graphene oxide/graphene-ZnO micro-structure Flied emission, include the following steps,
Step 1 prepares graphene oxide/graphene-ZnO micro-structure;
Step 1, graphene oxide is coated to the ZnO nano array top grown on a silicon substrate;
Step 1.1, ZnO nanoarray structure is grown on a silicon substrate;
Step 1.2, PMMA is coated on ZnO array, so that ZnO array is entirely located in PMMA;
Step 1.3, the part PMMA on plasma etching ZnO array top forms PMMA-ZnO structure;
Step 1.4, GO-PMMA-ZnO structure is formed in PMMA-ZnO body structure surface cladding graphene oxide sheet;
Step 2, micro-pattern region is prepared in GO-PMMA-ZnO body structure surface, that is, forms GO/G-ZnO structure;
Step 2.1, laterally oxidation of the first strip Zn film of sputtering to the region for the first time in GO-PMMA-ZnO structure Graphene is restored to obtain the first strip graphene;
Step 2.2, the graphene for the first strip Zn film being etched using HCl and the region being thinned;
Step 2.3, second of the second strip Zn film of longitudinal sputtering is restored to obtain to the graphene oxide in the region Second strip graphene;
Step 2.4, continue the graphene for etching the second strip Zn film with HCl and the region being thinned;
Step 2.5, it is repeated several times and carries out above-mentioned steps 2.2 and 2.3, then laterally and longitudinally in alternation procedure form GO/G- PMMA-ZnO structure;
Step 2.6, it removes PMMA and forms GO/G-ZnO micro-structure;
Step 2 introduces driving electric field in GO/G-ZnO micro-structure;
In GO/G-ZnO structure, Au electrode is added in the both ends preparation using magnetron sputtering at GO/G layers, on Au electrode Voltage is driven in introducing;The additional electrodes of silicon base are arranged parallel in GO/G-ZnO structure upper, are introduced in additional electrodes outer Making alive;Silicon base is grounded;
Step 3 by driving voltage in adjusting, while adjusting applied voltage to micro- based on graphene oxide/graphene-ZnO The purpose that the Flied emission of structure is regulated and controled.
Preferably, in step 1.4, in aqueous solution and centrifugal treating is done for GO powder ultrasonic is evenly dispersed, is obtained uniformly The graphene oxide solution of dispersion, by the way that GO piece is evenly coated at PMMA-ZnO nanometers to graphene oxide solution electrophoretic deposition Array top forms GO-PMMA-ZnO structure.
Preferably, when sputtering strip Zn film, by mask lithography technology, in the GO layer of GO-PMMA-ZnO structure top end Upper to prepare thickness less than 20nm using magnetron sputtering, width is not more than the strip Zn film of 300nm.
Preferably, strip graphene area is formed using the HCl solution etching processing Zn film that molar concentration is 0.05-01M Domain.
Preferably, it in step 2.5, is repeated several times and carries out above-mentioned steps 2.2 and 2.3, then laterally and longitudinally in alternation procedure, It will be formed by the GO and graphene of the various different numbers of plies and different reducing degrees in the GO layer surface of GO-PMMA-ZnO structure top end The miniature emitting area of alternate composition obtains GO/G-PMMA-ZnO structure, removes PMMA and forms GO/G-ZnO structure.
Preferably, specific by driving voltage in adjusting in step 3, so that there are more electronics on miniature emitter region surface Vertical Launch is done, while adjusting applied voltage and substrate and the electronics of ZnO nano array bottom is made effectively to be transported to ZnO nano The top of array is simultaneously transferred to surface micro region, to realize to based on graphene oxide/graphene-ZnO micro-structure field Transmitting regulation.
Compared with prior art, the invention has the following beneficial technical effects:
Structure of the present invention, using the unique electrons transport property of graphene (G) and structure feature, with graphene oxide (GO) it is coated on ZnO nano array top for raw material, and thinned graphene number of plies, reduction treatment etc. form different zones It influences the electron emission density and intensity of the miniature emitting area in ZnO nano array top, regulates and controls electron emission process, must show up Emitting performance is excellent and is formed by graphene oxide (GO) is alternate from the graphene of the various different numbers of plies and different reducing degrees Miniature emitting area.In conjunction with the Two-dimensional electron emission characteristics of grapheme material, on the miniature emitting area of GO/G in design Electrode is driven, increases the Vertical Launch probability of electronics in conjunction with extra electric field, has further widened the regulation thinking of Flied emission electric current, Realize the steerable electron emission in micro-nano region.So as to carry out field emission performance test to resulting materials, tied according to experiment Zn film thickness, bar-shaped zone width, the factors such as number and miniature area size are thinned to field in fruit network analysis sputtering parameter The influence of emitting performance, while according to photoelectron image during Flied emission, the electron emission studied in different miniature regions is close The dependence of degree and intensity and above-mentioned influence factor.
Further, the interior drive voltage within 5V is used to increase the Vertical Launch probability of electronics, reduces parallel launch Electron amount;Applied voltage is to extract and be transported to ZnO nano battle array for the more electronics in substrate or nano-array bottom end Top is arranged, and can be reduced waving effect and can be transferred in surface micro region in Electronic Transport Processes, and it is traditional Up to several kilovolts of voltage of two pole field emission structures is compared, and the applied voltage in this structure can be reduced within 300V.
The present invention prepares GO layers using electrophoretic deposition technique on the method One-Dimensional ZnO nano-array top, utilizes magnetic control GO can be reduced into graphene by sputtering zinc oxide, and be combined also subtracting the number of plies of graphene during salt acid etch zinc This thin scientific thought, is sputtered and etching by multiple exposure mask, realizes that obtain GO/G on ZnO nano array top alternate miniature Region.Make these areas due to GO and G different design features and different electrology characteristics, and by multiple preparation process Graphene number of plies on domain is not also identical, so obtaining the alternate different miniature magnetic field emitter region of GO/G on ZnO nano array top Domain, by GO/G-ZnO structure utilize magnetron sputtering technique design preparation addition Au electrode, by introduce in drive electric field come Increase the Vertical Launch of graphene surface electronics, effectively to send out to modulate electronics during different miniature region internal field emissions The density and intensity penetrated realize the regulation of the different emission currents and emission process on the miniature region in emitter top, can be Really the process exploitation of fine and smooth fine display technology and production preparation provide experiment parameter.
Further, by being centrifuged Homogenization Treatments, evenly dispersed graphene oxide solution can be obtained, and pass through The size and the uniformity of graphene oxide sheet are realized and adjusted to centrifugal treating, ensure that and is coated in zinc oxide array in subsequent experimental On emission layer have good uniformity and lamellar structure.
Detailed description of the invention
Fig. 1 is the preparation flow figure of GO-PMMA-ZnO structure described in present example.
Fig. 2 is the preparation flow figure of GO/G-ZnO structure described in present example.
Fig. 3 is the SEM cross-section morphology figure of the GO clading ZnO nano array prepared in present example.
Fig. 4 is the structure scale-up model schematic diagram of ellipse circled in Fig. 3.
Fig. 5 is the adjusted and controlled and method schematic diagram of Flied emission in the prior art.
Fig. 6 is not add the interior Flied emission for driving voltage adjusted and controlled described in present example and method schematic diagram.
Fig. 7 is the adjusted and controlled and method schematic diagram of Flied emission described in present example.
Fig. 8 is miniature emission area structure schematic diagram described in present example.
Fig. 9 is the miniature partially enlarged electron emission schematic diagram of emitter region described in present example.
Figure 10 is the SEM shape appearance figure of the GO clading ZnO nano array prepared in present example.
Figure 11 is the model schematic of structure described in Figure 10.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
The present invention on GO layer prepared by One-Dimensional ZnO nano-array top by utilizing magnetron sputtering technique and lithographic technique The alternate miniature emitting area of GO/G is obtained, electrode is driven in design preparation Au on the surface micro region of emitter, so that graphite Alkene, which is driven inside under electric field action, effectively to inhibit the parallel launch of electronics to increase Vertical Launch, using drive electric field in adjusting and tied Extra electric field is closed to modulate the Flied emission size of current in GO/G-ZnO structure in different zones, is realized really for fine and smooth fine Cold cathode emitters material in display technology prepares novel graphite alkenyl cold cathode emitting devices for future and provides reference.
The present invention is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method, passes through The interior modulation for driving electric field to miniature region internal field emission processes different on the superficial layer of GO/G-ZnO structure;So as to by changing Become include interior drive voltage, GO thickness degree, Zn width and thickness and spacing, electrode spacing and applied voltage etc. main influence ginseng Some parameter in number, while constant other influences parameter, find out miniature regional Electronic emission current and running parameter according to Rely rule, successively find out the dependence of miniature region field emission performance Yu all main affecting parameters, probes into miniature region electricity The emission mechanism of son.
Specifically, it includes the following steps.
(1) preparation of GO clading ZnO nano array, as shown in Figure 1.
(a) preparation grows ZnO nano array in Si substrate, and specific practice is the quasi- magnetron sputtering that passes through in N-shaped Si substrate Upper preparation ZnO seed layer, by chemical water bath grow ZnO nano array, change growth parameter(s) come be arranged vertically and Away from suitable ZnO nanoarray structure;
(b) PMMA is coated in ZnO nano array using spin coating proceeding;
(c) PMMA on ZnO nano array top is removed by plasma etching again;Ensure PMMA and ZnO nano array Top is concordant, so that ZnO nano array can have good contact with the GO for being coated on top layer.
(d) on the surface PMMA-ZnO, cladding GO piece forms GO-PMMA-ZnO structure.It is received as shown in figure 3, coating ZnO for GO The SEM cross-section morphology of rice array, it can be seen that GO thin slice is successfully coated on the top of ZnO nano array, and the two well connects Protrusion transmitting point is formd in the GO layer on surface after touch.Fig. 4 is dashing forward for the latter two contact formation of GO clading ZnO nano array Rise launch point position model schematic, it can be seen that due to the GO on ZnO nano array and surface layer have it is good contact thus Apparent protrusion point is formed, these protrusion points can be used as effective field transmitting point under DC Electric Field.Applied voltage It is that and can be reduced to extract by the more electronics in substrate or nano-array bottom end and be transported to ZnO nano array top Waving effect and can be transferred in surface micro region in Electronic Transport Processes, the height with two traditional pole field emission structures It is compared up to several kilovolts of voltages, the applied voltage in this structure can be reduced within 300V.It is set in GO/G-ZnO structure upper The additional electrodes for being parallel to silicon base are set, applied voltage is introduced in additional electrodes;The circuit connecting relation of applied voltage is such as schemed It is the SEM pattern of GO clading ZnO nano array, it can be seen that the surface coated GO lamellar structure of ZnO nano array is equal shown in 10 It is even orderly, and relatively thin GO piece translucency is good, can clearly see lower layer's ZnO nanoarray structure profile.Figure 11 is The corresponding model schematic of Figure 10, the top of uniform sequential ZnO nanoarray structure are coated with ultra-thin GO piece, illustrate this The preliminary structure feature of the GO/ graphene-ZnO micro-structure prepared in invention.
Wherein, PMMA-- polymethyl methacrylate;GO-graphene oxide;G- graphene;ZnO-zinc oxide;Si— Silicon.
In experiment using the effect of PMMA other than forming the GO layer of uniform ground in support ZnO nano array, mainly Protect ZnO nano array from corrosion during subsequent HCl etching processing Zn film;Then GO powder ultrasonic is evenly dispersed It the processing such as in aqueous solution and is centrifuged, GO piece is evenly coated at by PMMA-ZnO nano-array top by electrophoretic deposition technique GO-PMMA-ZnO structure is formed, the deposition for studying ZnO nano array density, nanowire diameter, aspect ratio and GO coats ginseng The influence to its field emission performance such as number.
(2) the micro-pattern region for realizing GO-PMMA-ZnO body structure surface, that is, form GO/G-ZnO structure, such as Fig. 2 institute Show.
(a) laterally sputtering strip Zn film restores the GO in the region for the first time in GO-PMMA-ZnO structure,
(b) graphene for strip Zn film being etched using HCl and the region being thinned,
(c) second of longitudinal sputtering strip Zn film restores the GO in the region,
(d) continue to etch strip Zn film with HCl,
(e) it is repeatedly laterally and longitudinally alternately repeated above-mentioned technical process and forms GO/G-PMMA-ZnO structure,
(f) it removes PMMA and forms GO/G-ZnO structure.
Wherein, PMMA-- polymethyl methacrylate;GO-graphene oxide;G- graphene;ZnO-zinc oxide;Zn— Zinc;HCl--- hydrochloric acid;
On the basis of coating uniformity and emission stability of the ZnO to promote surface emitting point by GO, In order to which the different zones on cold cathode same in fine display technology surface realize different emissioies, in the present invention Cold cathode surface carries out micro-pattern processing, and specific practice is as follows: mask lithography technology is combined first, in GO-PMMA-ZnO The strip Zn film that thickness is less than 20nm is prepared using magnetron sputtering on the GO layer of structure top end, then using certain density HCl etching processing Zn film forms strip graphene region, while the thickness in graphene region is also thinned;Again to sample surfaces It carries out after being repeatedly laterally and longitudinally alternately repeated above-mentioned technical process, the GO layer surface of GO-PMMA-ZnO structure top end will be formed By the GO miniature emitting area formed alternate from the graphene of the various different numbers of plies and different reducing degrees, GO/G-PMMA- is obtained ZnO structure removes PMMA and forms GO/G-ZnO structure.Wherein, 1 is differed between the alkene block of adjoining graphite two-by-two of surface emitting layer Layer;The minimum value of thickness difference, that is, the minimum thickness of one layer of graphene block is 0.34nm, and the thickness of most thin graphene block Degree is 0.34nm;And the thickness of graphene oxide block is constant, the as thickness of surface emitting layer, and surface emitting layer at least wraps The identical graphene oxide block of one group of thickness and a graphene block are included, so the minimum that surface emitting layer is able to use is thick Degree is the thickness of graphene oxide, i.e. 0.8nm, and the maximum gauge being able to use takes the maximum gauge of graphene oxide block to be 30nm。
(3) modulation of the electric field to miniature region internal field emission processes different on the superficial layer of GO/G-ZnO structure is driven in.
Using magnetron sputtering technique design preparation addition Au electrode in GO/G-ZnO structure, it is less than in 5V by introducing Voltage is driven to increase the Vertical Launch probability of graphene surface electronics, effectively to modulate different miniature region internal field emissions The density and intensity of electron emission in the process, as shown in Figure 6 and Figure 7.By on different miniature regions in comparison emission process Optical imagery pattern, the density and intensity for studying electron emission in different miniature regions internally drive voltage and the interior dependence for driving electric current Relationship is analyzed and grasps interior drive electric field regulation to the affecting laws of Flied emission.
Fig. 5 illustrates under external electric field in ZnO array electronics and waves transmitting in non-uniform, shown in Fig. 6 by comparison GO-ZnO structure in wave effect reduction, the emission density and intensity of electronics increased compared to ZnO array shown in Fig. 5 Add, emission uniformity and improved stability.Simultaneously in GO/G-ZnO structure, using magnetron sputtering miniature emitter region GO/G Layer both ends preparation addition Au electrode, the interior drive voltage for being less than 5V is introduced on Au electrode, reduces the parallel hair of electronics in ZnO array It penetrates and increases its Vertical Launch probability, as shown in fig. 7, driving electric field in introducing in GO/G-ZnO structure realizes modulate emission body surface The emission density of electronics on the different miniature regions in face.
(4) miniature regional Electronic emission mechanism research
The electron emission approach on the two-dimensional graphene surface on ZnO nano array top is different from the electronics of conventional three-dimensional material Emission process, therefore the emission mechanism of GO/G-ZnO body structure surface is studied, the electron transport mechanism on the apparent miniature region of difference It is very important, different miniature regions power on after being illustrated in figure 8 micro-pattern region and partial enlargement shown in Fig. 9 The schematic diagram of son transmitting.The present invention is by Binding experiment as a result, research GO/G- as composed by the GO of different reducing degrees and thickness The similarities and differences of electronics radiation pattern on ZnO body structure surface probe into during Flied emission electronics tunnel vacuum barrier on miniature region Microcosmic mechanism meets the graphene-based novel cold cathode composite materials of actual techniques needs and provides correlative study to prepare from now on Basis.

Claims (9)

1. a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission, which is characterized in that including silicon substrate Bottom, the ZnO nano array of vertical arrangement growth on a silicon substrate, is coated on the surface emitting layer on ZnO nano array top, surface The gold electrode of emission layer two sides setting, the additional electrodes that surface emitting layer top is arranged;
The surface emitting layer is in that the graphene oxide block being wholely set and graphene block form by structure;The oxygen Graphite alkene block is filled in laterally and/or longitudinally interval setting, remaining area by graphene block;Graphene oxide area Block is alternate from the graphene block of different-thickness and different reducing degrees to form miniature emitting area;Different-thickness and different reduction The graphene block of degree by the graphene oxide to graphene block region restored to obtain graphene and etch, The graphene in the region is thinned to obtain;
Voltage is driven in connecting on the gold electrode, applied voltage is connected in the additional electrodes, and silicon base connects ground wire.
2. it is according to claim 1 a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission, It is characterized in that, the graphene oxide block and graphene block on the surface emitting layer are arranged in checkerboard;Adjacent shape In five graphene blocks of across, intermediate graphene block thickness is minimum.
3. it is according to claim 1 a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission, It is characterized in that, the minimum 0.34nm of thickness difference between the alkene block of adjoining graphite two-by-two of the surface emitting layer, aoxidizes stone The thickness of black alkene block is identical, and surface emitting layer is with a thickness of 0.8-30nm.
4. it is according to claim 1 a kind of adjusted and controlled based on graphene oxide/graphene-ZnO micro-structure Flied emission, It is characterized in that, the interior voltage swing for driving voltage is less than 5V;The voltage swing of applied voltage is not higher than 300V.
5. a kind of regulate and control method based on graphene oxide/graphene-ZnO micro-structure Flied emission, which is characterized in that including as follows Step,
Step 1 prepares graphene oxide/graphene-ZnO micro-structure;
Step 1, graphene oxide is coated to the ZnO nano array top grown on a silicon substrate;
Step 1.1, ZnO nanoarray structure is grown on a silicon substrate;
Step 1.2, PMMA is coated in ZnO nano array, so that ZnO nano array is entirely located in PMMA;
Step 1.3, pass through the PMMA on plasma etching ZnO nano array top, it is ensured that the top horizontal of PMMA and ZnO nano array Together, PMMA-ZnO structure is formed;
Step 1.4, GO-PMMA-ZnO structure is formed in PMMA-ZnO body structure surface cladding graphene oxide sheet;
Step 2, micro-pattern region is prepared in GO-PMMA-ZnO body structure surface, that is, forms GO/G-ZnO structure;
Step 2.1, the first strip Zn film is sputtered laterally for the first time in GO-PMMA-ZnO structure with the oxidation stone to the region Black alkene is restored to obtain the first strip graphene;
Step 2.2, the graphene for the first strip Zn film being etched using HCl and the region being thinned;
Step 2.3, second the second strip Zn film of longitudinal sputtering is restored to obtain the with the graphene oxide to the region Two strip graphenes;
Step 2.4, continue the graphene for etching the second strip Zn film with HCl and the region being thinned;
Step 2.5, it is repeated several times and carries out above-mentioned steps 2.1 to 2.4, form GO/G-PMMA- in laterally and longitudinally alternation procedure ZnO structure;
Step 2.6, it removes PMMA and forms GO/G-ZnO micro-structure;
Step 2 introduces driving electric field in GO/G-ZnO micro-structure;
In GO/G-ZnO structure, using magnetron sputtering in GO/G layers of both ends preparation addition Au electrode, introduced on Au electrode Interior drive voltage;The additional electrodes of silicon base are arranged parallel in GO/G-ZnO structure upper, outer power-up is introduced in additional electrodes Pressure;Silicon base is grounded;
Step 3 by driving voltage in adjusting, while adjusting applied voltage to based on graphene oxide/graphene-ZnO micro-structure Flied emission realize regulation purpose.
6. it is according to claim 5 it is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission regulate and control method, It is characterized in that, in step 1.4, in aqueous solution and centrifugal treating is done for GO powder ultrasonic is evenly dispersed, is obtained evenly dispersed Graphene oxide solution, by the way that GO piece is evenly coated at PMMA-ZnO nano-array to graphene oxide solution electrophoretic deposition Top forms GO-PMMA-ZnO structure.
7. it is according to claim 5 it is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission regulate and control method, It is characterized in that, by mask lithography technology, being adopted on the GO layer of GO-PMMA-ZnO structure top end when sputtering strip Zn film Thickness is prepared less than 20nm with magnetron sputtering, and width is not more than the strip Zn film of 300nm.
8. it is according to claim 5 it is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission regulate and control method, It is characterized in that, forming strip graphene region using the HCl solution etching processing Zn film that molar concentration is 0.05M.
9. it is according to claim 5 it is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission regulate and control method, It is characterized in that, be repeated several times in step 2.5 and carry out above-mentioned steps 2.1 to 2.4, in laterally and longitudinally alternation procedure, The GO layer surface of GO-PMMA-ZnO structure top end will be formed by the GO and graphene phase of the various different numbers of plies and different reducing degrees Between the miniature emitting area that forms, obtain GO/G-PMMA-ZnO structure, remove PMMA and form GO/G-ZnO structure.
CN201710851247.8A 2017-09-20 2017-09-20 It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method Active CN107731637B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710851247.8A CN107731637B (en) 2017-09-20 2017-09-20 It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710851247.8A CN107731637B (en) 2017-09-20 2017-09-20 It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method

Publications (2)

Publication Number Publication Date
CN107731637A CN107731637A (en) 2018-02-23
CN107731637B true CN107731637B (en) 2019-03-29

Family

ID=61206664

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710851247.8A Active CN107731637B (en) 2017-09-20 2017-09-20 It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method

Country Status (1)

Country Link
CN (1) CN107731637B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110184859B (en) * 2019-05-16 2021-08-27 西安石油大学 Multilayer graphene fiber paper and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102856139B (en) * 2012-09-07 2015-04-15 福州大学 Surface-conduction electron emission source based on graphene
CN104835708B (en) * 2015-05-12 2017-01-25 江苏师范大学 Preparation method of graphene oxide field emission flat plate display instrument
CN106847648B (en) * 2017-03-01 2019-01-08 杭州电子科技大学 A kind of preparation method of use for field emission graphene/zinc oxide/graphene sandwich structure composite cathode material

Also Published As

Publication number Publication date
CN107731637A (en) 2018-02-23

Similar Documents

Publication Publication Date Title
TW200305187A (en) Fed cathode structure using electrophoretic deposition and method of fabrication
US7319069B2 (en) Structure having pores, device using the same, and manufacturing methods therefor
Aghazadeh et al. Cathodic electrodeposition of Y (OH) 3 and Y2O3 nanostructures from chloride bath. Part II: Effect of the bath temperature on the crystal structure, composition and morphology
JP2004193524A (en) Columnar structure, electrode having columnar structure, and their manufacturing method
US20120161192A1 (en) Nitrogen-doped transparent graphene film and manufacturing method thereof
Liang et al. TiO2 nanotip arrays: anodic fabrication and field-emission properties
JP4403618B2 (en) Method for producing carbon nanotube
JP2004193523A (en) Nanostructure, electronic device, and its manufacturing method
CN107731637B (en) It is a kind of based on graphene oxide/graphene-ZnO micro-structure Flied emission is adjusted and controlled and method
Maurer et al. Field emission of copper nanowires grown in polymer ion-track membranes
KR20060032402A (en) Carbon nanotube emitter and manufacturing method thereof and field emission device and manufacturing method thereof
TWI254338B (en) Carbon-nanotube cold cathode and method for fabricating the same
Gautier et al. Enhanced field electron emission properties of hierarchically structured MWCNT-based cold cathodes
CN107731638B (en) Cold cathode structure and preparation method thereof based on the miniature emitting area of graphene oxide/graphene
TW505938B (en) Method of providing uniform emission current
Ma et al. Controllable preparation of silver nano-bowl coatings for suppressing secondary electron emission
TWI484061B (en) Diamond like film and method for fabricating the same
Lv et al. Tunable field emission properties of well-aligned silicon nanowires with controlled aspect ratio and proximity
KR101307538B1 (en) Nanoscale lithography method on graphene using oxidation and hydrogenation
CN115010122B (en) Method for preparing high-oxidation graphene
CN206244402U (en) A kind of graphene-based nanowire composite structures
KR102336107B1 (en) Bio sensor having piller-typed electrode suructure coated non-conductive material
WO2019109966A1 (en) Plasma generator electrode and manufacturing method thereof
TW480537B (en) Method for enhancing emission efficiency of carbon nanotube emission source field
Galperin et al. Effect of the morphology of CNT arrays on the current density of field-emitter matrices

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant