CN101966987B - 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 through micromechanics and peels off and observe monolayer carbon lattice plane structure; It is the existence of Graphene; Broken the thermodynamics traditional concept that two-dimension single layer atomic crystal structure can not exist singly, 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 is the graphene nanometer sheet film mostly; It is made up of numerous graphene nano monolithics of stochastic distribution, discrete growth, through parameters such as adjusting substrate temperature, depositing time can remote effect graphene nano monolithic stand density, spacing and pattern.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 at the graphene nanometer sheet that is close to growth 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.The optimization growth of the grapheme material of how realizing being the main body with upright graphene nanometer sheet improves the field emission performance of grapheme material, and the Graphene field emmision material of preparing practical use is the current a great problem that faces.
Summary of the invention
One of the object of the 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; Individual layer and the fractal sheet Graphene of multilayer by being deposited on the upright staggered growth on the substrate constitute; Have good electronic field emission ability, can satisfy novel electron device counter electrode emission efficiency, emissive porwer and homogeneity and stability requirement; Two of the object of the invention provides a kind of preparation method with fractal grapheme material of negative electron affinity (NEA); Three of the object of the invention provides aforesaid fractal grapheme material with negative electron affinity (NEA) in the application of making fields such as FED, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source device.
One of the object of the invention is realized through following technical scheme:
Fractal grapheme material with negative electron affinity (NEA) of the present invention is made up of the individual layer and the fractal sheet Graphene of multilayer that are deposited on the upright staggered growth on the substrate.
Further, said 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 said 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 said 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 the object of the invention is realized through following technical scheme:
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; Through the plasma bombardment target, deposition different two to three-layer metal is as substrate on base material, and deposit thickness is chosen 100 ~ 200 nanometers;
The substrate that 3) 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 through 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 said 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, said 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 alloying element, element can be III, V group element or the metallic element on the mendeleev periodic table of elements.
Three of the object of the invention is that aforesaid fractal grapheme material with negative electron affinity (NEA) is used to make associated components on FED, 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, and has 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 it is surperficial that electronics is overflowed more easily, 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 improve and promoted grapheme material in the practical application midfield low, the lack of homogeneity of emissive power, the insufficient problem of structural stability.
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 FED, 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 object of the invention, technical scheme and advantage clearer, will combine accompanying drawing that the present invention is made further detailed description below, wherein:
Fig. 1 is apparatus structure synoptic diagram (wherein, the 1-magnetron sputtering reaction chamber of embodiment of the present invention; 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
Below will carry out detailed description to the preferred embodiments of the present invention with reference to accompanying drawing.Should be appreciated that preferred embodiment has been merely explanation the present invention, rather than in order to limit protection scope of the present invention.
Present method is on traditional chemical Vapor deposition process basis, to improve 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, and heating unit 6 and starting electrode 13 are arranged on the inside of ultrahigh-temperature chemical vapor deposition reaction chamber 18, and under meter 7,8,9,10,11 is 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 sealed door and ultrahigh-temperature chemical vapor deposition reaction chamber 18 of magnetron sputtering reaction chamber 1.
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 cleaner 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 through under meter 2, make vacuum tightness rise to 1Pa and also keep stable, starting electrode 3 forms plasma body 4, and through 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 through 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 ℃; Through 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, get 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 ℃; Through 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 through 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 (like 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 through under meter 2, make vacuum tightness rise to 1Pa and keep stable, starting electrode 3 forms plasma body 4, through 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 through 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 ℃; Through 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, get 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 ℃; Through 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 through 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 cleaner 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 through under meter 2, make vacuum tightness rise to 1Pa and keep stable, starting electrode 3 forms plasma body 4, through 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 through 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 ℃; Through 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, get 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 ℃; Through 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 through 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 alloying 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.
Correlation properties such as Fig. 3 of utilizing the fractal grapheme material with negative electron affinity (NEA) that the operational condition of embodiment (1) makes are to shown in Figure 6.Like Fig. 3, Fig. 4 and shown in Figure 6; This grapheme material is made up 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 said material are less than or equal to 20 °; The surface of single flake graphite alkene is arc and has wrinkle Zhe that the edge is open fault structure (so-called open fault structure is that single flake graphite alkene is the two dimensional crystal structure, and 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, the D peak heights is symmetrical, peak shape is 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 is consistent at the test result height of the different positions of FGN sample, show that 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 FED, 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 with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and 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 present technique scheme, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (8)
1. the fractal grapheme material that has negative electron affinity (NEA); It is characterized in that: said material is made up 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 said 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 μ m～20 μ m, and height is between 0.1 μ m～10 μ m.
2. the fractal grapheme material with negative electron affinity (NEA) as claimed in claim 1, it is characterized in that: said substrate is selected one or more in copper, chromium, gold, iron, cobalt or the nickel for use, or contains metal-doped semiconductor material.
3. according to claim 1 or claim 2 the fractal grapheme material with negative electron affinity (NEA) is characterized in that: the D frequency band 1320～1370cm of the Raman spectrum of said grapheme material
-1Peak strength and G frequency band 1540～1580 cm
-1The ratio of peak strength is not less than 0.10.
4. 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; Through the plasma bombardment target, deposition different two to three-layer metal is as substrate on base material, and deposit thickness is chosen 100 ~ 200 nanometers;
The substrate that 3) 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 through 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 said carrier gas for use;
4) promote Reaktionsofen temperature to 1000 ~ 1400 ℃; Promote the carrier gas ratio, reduce carbon based gas concentration, said reactant gases and carrier gas ratio are adjusted to 1:10 ~ 20; 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.
5. the preparation method with fractal grapheme material of negative electron affinity (NEA) according to claim 4 is characterized in that: in step 1), select semi-conductor, metal or stupalith as base material; In step 2) in, said substrate is selected one or more the combination in copper, chromium, gold, iron, cobalt, the nickel for use.
6. the preparation method with fractal grapheme material of negative electron affinity (NEA) according to claim 4 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.
7. the fractal grapheme material with negative electron affinity (NEA) according to claim 4 the preparation method; It is characterized in that: in step 3), 4) deposition process in all add or selectivity adds alloying element, element can be III, V group element or the metallic element on the mendeleev periodic table of elements.
8. like the arbitrary described application of claim 1 to 3, it is characterized in that: at FED, cold cathode electric light source, x-ray source, electrons leaves welding and cold-cathode electron source devices field cathode material as the fabricating yard ballistic device with fractal grapheme material of negative electron affinity (NEA).
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