CN101966987A - Fractal graphene material with negative electron affinity as well as preparation method and application thereof - Google Patents
Fractal graphene material with negative electron affinity as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a fractal graphene material with negative electron affinity as well as a preparation method and application thereof. The fractal graphene material is prepared by adopting a superhigh temperature chemical vapor deposition process and comprises monolayer fractal flake graphene and multilayer fractal flake graphene which are deposited on a substrate and vertically grow in a staggered way; along with the increase of the temperature of the substrate, the crystal state of a graphene nanosheet trends to vertical growth, which directly decides the electrical property orientation of the graphene nanosheet; and the negative electron affinity is generated due to the existence of a large-curvature strip-shaped bulging structure of the flake graphene so that the local field is enhanced, therefore, the fractal graphene material has stronger field electron emission capacity and high structure stability, is very suitable for manufacturing a cathode material of a field emission device and has wide application prospects in the fields of field emission display, cold cathode electric light sources, X-ray sources, electron beam welding and cold cathode electron source devices, and the like.
Description
Technical field
The present invention relates to field of novel, particularly a kind of fractal grapheme material (Fractal Graphene with NEA is called for short FGN) with negative electron affinity (NEA), this material can be used for the negative electrode of fabricating yard ballistic device.
Background technology
Graphene (Graphene) is a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape crystalline network.The scientist Geim A of Univ Manchester UK in 2004 peels off method by micromechanics and peels off and observe monolayer carbon atomic plane structure, it is the existence of Graphene, broken the thermodynamics traditional concept that two-dimension single layer atomic crystal structure can not Individual existence, caused the research boom of the whole world grapheme material.Because its unique two dimensional crystal structure, make it show some novel rerum naturas at aspects such as electricity, calorifics and mechanics, being expected to obtain widespread use in fields such as high-performance micro-nano electron device, field emmision material, matrix material, gas sensor and energy storages, is another landmark new carbon behind soccerballene and carbon nanotube.
The method for preparing at present Graphene has micromechanics to peel off method, epitaxy method, heating SiC method and chemical Vapor deposition process etc., wherein chemical Vapor deposition process also is the main method that realizes two-dimentional Graphene field emission body preparation at present as deposition technique the most commonly used in the semi-conductor industry.The grapheme material of chemical Vapor deposition process preparation mostly is the graphene nanometer sheet film greatly, it is made up of numerous graphene nano monolithics of stochastic distribution, discrete growth, by regulating stand density, spacing and the pattern that parameters such as substrate temperature, depositing time can remote effect graphene nano monolithic.The field emission is as a kind of key property of graphene nanometer sheet, proved by the graphene nanometer sheet film of hot filament CVD (HF-CVD) preparation as far back as 2002, but so far, research to the grapheme material field emission performance still is in the laboratory exploratory stage, and Shang Weijian has report to prepare the Graphene field emmision material of practical use.
Its depositing temperature of existing chemical Vapor deposition process is many below 1200 ℃, the density of the graphene nanometer sheet that comprises in the graphene film of preparation, pattern and orientation have very big-difference, and the crystalline orientation of graphene nanometer sheet has directly determined its electrical properties, is good electron field emission materials being close to the graphene nanometer sheet of growing under the erectility.The tangleweed that graphene nanometer sheet is arranged in the existing graphene film causes the efficient of its emission low, emission uniformity is poor.How to realize the optimization growth based on the grapheme material of upright graphene nanometer sheet, improve the field emission performance of grapheme material, the Graphene field emmision material of preparing practical use is the current a great problem that faces.
Summary of the invention
One of purpose of the present invention provides a kind of fractal grapheme material with negative electron affinity (NEA), this material adopts 1300 ℃ of ultrahigh-temperature (〉) chemical vapor deposition method (UT-CVD) preparation, constitute by the individual layer and the fractal sheet Graphene of multilayer that are deposited on the upright staggered growth on the substrate, have good electronic field emission ability, can satisfy novel electron device counter electrode emission efficiency, emissive porwer and homogeneity and stability requirement; Two of purpose of the present invention provides a kind of preparation method with fractal grapheme material of negative electron affinity (NEA); Three of purpose of the present invention provides aforesaid application with fractal grapheme material of negative electron affinity (NEA) in fields such as making Field Emission Display, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source devices.
One of purpose of the present invention is achieved through the following technical solutions:
Fractal grapheme material with negative electron affinity (NEA) of the present invention is made of the individual layer and the fractal sheet Graphene of multilayer that are deposited on the upright staggered growth on the substrate.
Further, described substrate is selected one or more in copper, chromium, gold, iron, cobalt or the nickel for use, or contains metal-doped semiconductor material;
Further, flake graphite alkene and the angle between the substrate surface normal in the described material are less than or equal to 20 °, and the surface of single flake graphite alkene is arc and has wrinkle Zhe that the edge is open fault structure, length is between 0.3 um～20um, and height is between 0.1 um～10 um;
Further, the D frequency band (1320～1370cm of the Raman spectrum of described grapheme material
-1) peak strength and G frequency band (1540～1580 cm
-1) ratio of peak strength is not less than 0.10.
Two of purpose of the present invention is achieved through the following technical solutions:
This preparation method with fractal grapheme material of negative electron affinity (NEA) may further comprise the steps:
1) selects to be fit to the base material that Graphene is grown, and base material is carried out physics and matting, reach the required cleaning surfaces state of deposition;
2) cleaned base material loaded is gone in the magnetron sputtering reaction chamber, feed rare gas element, starting electrode after waiting to reach working vacuum, form plasma body, by the plasma bombardment target, on base material deposition different two to three-layer metal as substrate, deposit thickness is chosen 100 ~ 200 nanometers;
3) substrate that will be deposited on the base material changes in the ultrahigh-temperature chemical vapour deposition reactor furnace, open heating unit, make Reaktionsofen temperature increase to 600 ~ 800 ℃, feed the gas mixture and the rare gas element of reactant gases and carrier gas then, and formation plasma body, quicken by electrode, make reactive ion carry out physical bombardment and chemical reaction treating processes, at the substrate surface uniform carbon nano-particle layer of growing substrate;
Wherein, this reactant gases is selected carbon based gas for use, and one or more mixed gass in hydrogen, ammonia, the nitrogen are selected in described carrier gas for use.
4) promote Reaktionsofen temperature to 1000 ~ 1400 ℃, promote the carrier gas ratio, reduce carbon based gas concentration, the carbon atom sedimentation rate is reduced, deposit the fractal Graphene that has negative electron affinity (NEA) uniformly at substrate surface;
5) keep Reaktionsofen temperature to 1000 ~ 1400 ℃, only feed carrier gas in the Reaktionsofen, to grapheme material reform, purifying.
Further, in step 1), select semi-conductor, metal or stupalith as base material; In step 2) in, described substrate is selected one or more the combination in copper, chromium, gold, iron, cobalt, the nickel for use;
Further, in the step 3), the ratio that keeps reactant gases and carrier gas is in the scope of 1:1 ~ 8;
Further, in the step 4), the ratio of reactant gases and carrier gas is adjusted in the scope of 1:10 ~ 20;
Further, in step 3), 4) deposition process in all add or selectivity adds doped element, element can be III, V group element or the metallic element on the mendeleev periodic table of elements.
Three of purpose of the present invention is that aforesaid fractal grapheme material with negative electron affinity (NEA) is used to make associated components on Field Emission Display, cold cathode electric light source, x-ray source and the cold-cathode electron source device, especially for the negative electrode of fabricating yard ballistic device.
The present invention has the following advantages:
1. there is the strip projected parts structure of the deep camber that forms because of the graphene film gauffer in the fractal grapheme material with negative electron affinity (NEA) of the present invention, this structure causes the Graphene energy band structure to change, produced negative electron affinity (NEA), on the other hand, deep camber has caused the formation of high-density electron distributions, local fields is enhanced, thereby make the easier effusion of electronics surface, therefore, this material has good electronic field emission ability, can satisfy novel electron device counter electrode emission efficiency, emissive porwer and homogeneity and stability requirement.Early-stage Study shows, about 2.0 microns * 2.0 microns of the average area of flake graphite alkene structure; About 3 microns of list structure mean length; Starting the field intensity threshold value is 0.22-0.40 volt/micron.
2. the growth technique that the preparation method with fractal grapheme material of negative electron affinity (NEA) of the present invention passes through to improve temperature of reaction, optimizes Graphene, realized the controllable growth of Graphene submicrometer structure, overcome the traditional chemical vapour deposition process and prepared upright graphene nanometer sheet ratio low shortcoming in the grapheme material that, realized the density of graphene nanometer sheet, the controllable growth of pattern and orientation greatly improves and has promoted grapheme material low, the lack of homogeneity of emissive power, the insufficient problem of structural stability in actual applications.
3. grapheme material of the present invention can controllably be produced in batches, thereby has effectively widened the application of grapheme material in a plurality of fields such as Field Emission Display, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source devices.
Description of drawings
In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing, wherein:
Fig. 1 is for implementing apparatus structure synoptic diagram of the present invention (wherein, 1-magnetron sputtering reaction chamber; The 2-under meter; The 3-starting electrode; The 6-heating unit; The 12-mixing chamber; The 13-starting electrode; The 15-transfer robot; 16,17-vacuum unit; 18-ultrahigh-temperature chemical vapor deposition reaction chamber);
Fig. 2 is a method flow synoptic diagram of the present invention;
Fig. 3 is grapheme material of the present invention (FGN) sample stereoscan photograph (500 times in electron microscope);
Fig. 4 is grapheme material of the present invention (FGN) sample stereoscan photograph (5000 times in electron microscope);
Fig. 5 is the Raman spectrogram of grapheme material of the present invention (FGN) sample;
Fig. 6 is film height and the long limit of Graphene monolithic and the angle synoptic diagram between the substrate surface normal of grapheme material of the present invention (FGN) sample.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.Should be appreciated that preferred embodiment only for the present invention is described, rather than in order to limit protection scope of the present invention.
Present method is to improve on traditional chemical Vapor deposition process basis and improve, and proposes a kind of new preparation method, is defined as ultrahigh-temperature chemical Vapor deposition process (being called for short UT-CVD).
As shown in Figure 1, starting electrode 3 is arranged on the inside of magnetron sputtering reaction chamber 1, under meter 2 is arranged on the input channel of rare gas element, vacuum unit 16 is arranged on magnetron sputtering reaction chamber 1 outside and is connected with magnetron sputtering reaction chamber 1, heating unit 6 and starting electrode 13 are arranged on the inside of ultrahigh-temperature chemical vapor deposition reaction chamber 18, under meter 7,8,9,10,11 are arranged on the gas inlet pipe road of mixing chamber 12, the gas output tube road of mixing chamber 12 is connected with ultrahigh-temperature chemical vapor deposition reaction chamber 18, and vacuum unit 17 is arranged on ultrahigh-temperature chemical vapor deposition reaction chamber 18 outsides and is connected with ultrahigh-temperature chemical vapor deposition reaction chamber 18; Transfer robot 15 is arranged between the sealed door of the sealed door of magnetron sputtering reaction chamber 1 and ultrahigh-temperature chemical vapor deposition reaction chamber 18.
Embodiment one
As shown in Figure 2, method of the present invention may further comprise the steps:
1) copper that select to be fit to the Graphene growth is as base material, and base material is carried out physics and matting, reaches the required clean surface state of deposition;
2) cleaned base material loaded is gone in the magnetron sputtering reaction chamber 1, start vacuum unit 16 and 17, treat that vacuum tightness reaches 8 * 10
-4During Pa, feed rare gas element by under meter 2, make vacuum tightness rise to 1Pa and also keep stable, starting electrode 3 forms plasma body 4, and by plasma bombardment base material 5, three layers of nickel metal of deposition are as substrate on base material;
3) after deposition finishes, treat that vacuum tightness returns to 10
-3During Pa, send in the ultrahigh-temperature chemical vapor deposition reaction chamber 18 by the substrate that transfer robot 15 will be deposited on the base material; Question response chamber 18 vacuum tightnesss reach 5 * 10
-4During Pa, start heating unit 6, make Reaktionsofen temperature increase to 800 ℃, by under meter 7,8,9,10,11 with reactant gases, carrier gas and rare gas element by a certain percentage (1:7:1) feed mixing chamber 12, after treating that gas mixes, enter in the reaction chamber 18 starting electrode 13, form plasma body 14, at the substrate surface uniform carbon nano-particle layer of growing;
Wherein, this reactant gases is selected carbon based gas for use, and carrier gas can be selected the mixed gas of one or more and they in hydrogen, ammonia, the nitrogen for use;
4) start heating unit 6, promote Reaktionsofen temperature to 1400 ℃, by under meter 7,8,9,10,11 reactant gases and carrier gas ratio are adjusted to 1:18, reduce concentrations of reactant gas, carbon laydown speed is reduced, to transfer the sheet deposition to by unformed deposition, in the scope of height of deposition between 0.1 um～10 um;
5) keep the Reaktionsofen temperature at 1400 ℃,, only feed carrier gas by under meter 7,8,9,10,11 control off-response other inert gases, to grapheme material reform, purifying;
Embodiment two
Present embodiment may further comprise the steps:
1) selects to be fit to Graphene grown semiconductor material (as silicon) as base material, and base material is carried out physics and matting, reach the required cleaning surfaces state of deposition;
2) cleaned base material loaded is gone in the magnetron sputtering reaction chamber 1, start vacuum unit 16 and 17, treat that vacuum tightness reaches 8 * 10
-4During Pa, feed rare gas elementes by under meter 2, make vacuum tightness rise to 1Pa and keep stable, starting electrode 3 forms plasma body 4, by plasma bombardment base material 5, on base material successively deposit cobalt nickel metal as substrate;
3) after deposition finishes, treat that vacuum tightness returns to 10
-3During Pa, send in the ultrahigh-temperature chemical vapor deposition reaction chamber 18 by the substrate that transfer robot 15 will be deposited on the base material; Question response chamber 18 vacuum tightnesss reach 5 * 10
-4During Pa, start heating unit 6, make Reaktionsofen temperature increase to 700 ℃, by under meter 7,8,9,10,11 with reactant gases, carrier gas and rare gas element by a certain percentage (1:5:1) feed mixing chamber 12, after treating that gas mixes, enter in the reaction chamber 18 starting electrode 13, form plasma body 14, at the substrate surface uniform carbon nano-particle layer of growing;
Wherein, this reactant gases is selected carbon based gas for use, and carrier gas can be selected the mixed gas of one or more and they in hydrogen, ammonia, the nitrogen for use;
4) start heating unit 6, promote Reaktionsofen temperature to 1200 ℃, by under meter 7,8,9,10,11 reactant gases and carrier gas ratio are adjusted to 1:15, reduce concentrations of reactant gas, carbon laydown speed is reduced, to transfer the sheet deposition to by unformed deposition, in the scope of height of deposition between 0.1 um～10 um;
5) keep the Reaktionsofen temperature at 1200 ℃,, only feed carrier gas by under meter 7,8,9,10,11 control off-response other inert gases, to grapheme material reform, purifying;
Embodiment three
Present embodiment may further comprise the steps:
1) pottery that select to be fit to the Graphene growth is as base material, and base material is carried out physics and matting, reaches the required clean surface state of deposition;
2) cleaned base material loaded is gone in the magnetron sputtering reaction chamber 1, start vacuum unit 16 and 17, treat that vacuum tightness reaches 8 * 10
-4During Pa, feed rare gas elementes by under meter 2, make vacuum tightness rise to 1Pa and keep stable, starting electrode 3 forms plasma body 4, by plasma bombardment base material 5, on base material successively deposit cobalt chromium nickel metal as substrate;
3) after deposition finishes, treat that vacuum tightness returns to 10
-3During Pa, send in the ultrahigh-temperature chemical vapor deposition reaction chamber 18 by the substrate that transfer robot 15 will be deposited on the base material; Question response chamber 18 vacuum tightnesss reach 5 * 10
-4During Pa, start heating unit 6, make Reaktionsofen temperature increase to 600 ℃, by under meter 7,8,9,10,11 with reactant gases, carrier gas and rare gas element by a certain percentage (1:2:1) feed mixing chamber 12, after treating that gas mixes, enter in the reaction chamber 18 starting electrode 13, form plasma body 14, at the substrate surface uniform carbon nano-particle layer of growing;
Wherein, this reactant gases is selected carbon based gas for use, and carrier gas can be selected the mixed gas of one or more and they in hydrogen, ammonia, the nitrogen for use;
4) start heating unit 6, promote Reaktionsofen temperature to 1000 ℃, by under meter 7,8,9,10,11 reactant gases and carrier gas ratio are adjusted to 1:11, reduce concentrations of reactant gas, carbon laydown speed is reduced, to transfer the sheet deposition to by unformed deposition, in the scope of height of deposition between 0.1 um～10 um;
5) keep the Reaktionsofen temperature at 1000 ℃,, only feed carrier gas by under meter 7,8,9,10,11 control off-response other inert gases, to grapheme material reform, purifying;
In the step of above each embodiment, can be in step 3), 4) deposition process in add doped element, element can be III, V group element and the metallic element on Mendelyeev's periodic table of chemical element, purpose is the electron emissivity that promotes material.
In addition, the material that the selection of substrate is not limited to mention in the foregoing description, in fact, this substrate can be selected one or more the combination in copper, chromium, gold, iron, cobalt or the nickel for use, or contains the semiconductor material of doping metals.
Utilize the correlation properties of the fractal grapheme material that the operational condition of embodiment (1) makes such as Fig. 3 to shown in Figure 6 with negative electron affinity (NEA).As Fig. 3, Fig. 4 and shown in Figure 6, this grapheme material is made of the individual layer and the fractal sheet Graphene of multilayer that are deposited on the upright staggered growth on the substrate, flake graphite alkene and the angle between the substrate surface normal in the described material are less than or equal to 20 °, the surface of single flake graphite alkene is arc and has wrinkle Zhe, the edge is that (so-called open fault structure is that single flake graphite alkene is the two dimensional crystal structure to open fault structure, its leaf growth end does not seal), length is between 0.3 um～20um, and height is between 0.1 um～10 um.
As shown in Figure 5, the D frequency band (1320～1370cm of the Raman spectrum of grapheme material
-1) peak strength and G frequency band (1540～1580 cm
-1) ratio of peak strength is not less than 0.10.The 2D peak has Lorentz lorentz's symmetry of height, shows that FGN is the quite complete single-layer graphene of structure.Simultaneously, D peak heights symmetry, peak shape are sharp-pointed, halfwidth is very little, can belong to the Geometrical Bending for Graphene, but not textural defect.What deserves to be mentioned is that The above results shows that in the test result height unanimity of the different positions of FGN sample this material growth is very even.
Grapheme material of the present invention can controllably be produced in batches, the grapheme material that makes can be widely used in a plurality of fields such as Field Emission Display, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source devices, particularly has special advantages aspect the negative electrode of fabricating yard ballistic device.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the aim and the scope of the technical program, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. have the fractal grapheme material of negative electron affinity (NEA), it is characterized in that: described material is made of the individual layer and the fractal sheet Graphene of multilayer that are deposited on the upright staggered growth on the substrate.
2. as claims 1 described fractal grapheme material with negative electron affinity (NEA), it is characterized in that: described substrate is selected one or more in copper, chromium, gold, iron, cobalt or the nickel for use, or contains metal-doped semiconductor material.
3. the fractal grapheme material with negative electron affinity (NEA) as claimed in claim 1 or 2, it is characterized in that: flake graphite alkene and the angle between the substrate surface normal in the described material are less than or equal to 20 °, the surface of single flake graphite alkene is arc and has wrinkle Zhe, the edge is open fault structure, length is between 0.3 um～20um, and height is between 0.1 um～10 um.
4. the fractal grapheme material with negative electron affinity (NEA) as claimed in claim 3 is characterized in that: the D frequency band (1320～1370cm of the Raman spectrum of described grapheme material
-1) peak strength and G frequency band (1540～1580 cm
-1) ratio of peak strength is not less than 0.10.
5. have the preparation method of the fractal grapheme material of negative electron affinity (NEA), it is characterized in that: may further comprise the steps:
1) selects to be fit to the base material that Graphene is grown, and base material is carried out physics and matting, reach the required cleaning surfaces state of deposition;
2) cleaned base material loaded is gone in the magnetron sputtering reaction chamber, feed rare gas element, starting electrode after waiting to reach working vacuum, form plasma body, by the plasma bombardment target, on base material deposition different two to three-layer metal as substrate, deposit thickness is chosen 100 ~ 200 nanometers;
3) substrate that will be deposited on the base material changes in the ultrahigh-temperature chemical vapour deposition reactor furnace, open heating unit, make Reaktionsofen temperature increase to 600 ~ 800 ℃, feed the gas mixture and the rare gas element of reactant gases and carrier gas then, and formation plasma body, quicken by electrode, make reactive ion carry out physical bombardment and chemical reaction treating processes, at the substrate surface uniform carbon nano-particle layer of growing substrate;
Wherein, this reactant gases is selected carbon based gas for use, and one or more mixed gass in hydrogen, ammonia, the nitrogen are selected in described carrier gas for use;
4) promote Reaktionsofen temperature to 1000 ~ 1400 ℃, promote the carrier gas ratio, reduce carbon based gas concentration, the carbon atom sedimentation rate is reduced, deposit the fractal Graphene that has negative electron affinity (NEA) uniformly at substrate surface;
5) keep Reaktionsofen temperature to 1000 ~ 1400 ℃, only feed carrier gas in the Reaktionsofen, to grapheme material reform, purifying.
6. the preparation method with fractal grapheme material of negative electron affinity (NEA) according to claim 5 is characterized in that: in step 1), select semi-conductor, metal or stupalith as base material; In step 2) in, described substrate is selected one or more the combination in copper, chromium, gold, iron, cobalt, the nickel for use.
7. the preparation method with fractal grapheme material of negative electron affinity (NEA) according to claim 5 is characterized in that: in the step 3), the ratio that keeps reactant gases and carrier gas is in the scope of 1:1 ~ 8.
8. the fractal grapheme material with negative electron affinity (NEA) according to claim 5 the preparation method, it is characterized in that: in the step 4), the ratio of reactant gases and carrier gas is adjusted in the scope of 1:10 ~ 20.
9. the fractal grapheme material with negative electron affinity (NEA) according to claim 5 the preparation method, it is characterized in that: in step 3), 4) deposition process in all add or selectivity adds doped element, element can be III, V group element or the metallic element on the mendeleev periodic table of elements.
10. the application with fractal grapheme material of negative electron affinity (NEA) as claimed in claim 4 is characterized in that: the cathode material in fields such as Field Emission Display, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source devices as the fabricating yard ballistic device.
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