CN105185673B - A kind of photoinduced electron emission source and its manufacturing method, electron emitting device - Google Patents
A kind of photoinduced electron emission source and its manufacturing method, electron emitting device Download PDFInfo
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- CN105185673B CN105185673B CN201510415969.XA CN201510415969A CN105185673B CN 105185673 B CN105185673 B CN 105185673B CN 201510415969 A CN201510415969 A CN 201510415969A CN 105185673 B CN105185673 B CN 105185673B
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Abstract
The embodiment of the invention discloses a kind of photoinduced electron emission source and its manufacturing method, electron emitting device, the manufacturing method includes：Choose the conductive substrates for being suitble to carbon nano tube growth；The deposit catalyst layers in the conductive substrates；Carbon nanotube is grown on the catalyst layer.The photoinduced electron emission source that the embodiment of the present invention is prepared by the deposit catalyst layers in conductive substrates and growth carbon nanotube, emission is big, photoemission is efficient, vacuum level requirements are low, stability is high, preparation method is simple, at low cost.
Description
Technical field
The present invention relates to a kind of electron emitting technology more particularly to a kind of photoinduced electron emission sources and its manufacturing method, electricity
Sub- emitter.
Background technology
Electron emission source has in fields such as display, illumination, microwave amplifier, electron microscope, material analysis and space flight
It is widely applied.Thermionic emission and Field Electron Emission are widely applied in national product and life, and with each application
The continuous development in field proposes in modulating performance, high-frequency emission performance, safe and portable etc. electron emission source higher
It is required that.
In general, electron electronics be electronics under certain effect, be detached from electron emission source constraint, to
Vacuum or the process of anode transmitting.There are many types, such as thermionic emission, photic hair for the process of electron electronics
Penetrate with field emission etc., the density of emission current mainly with the temperature of electron emission source, the work function of emissive material, electron emission
The geometry enhancement factor in source and additional electric field strength or electromagnetic field are closely related.These emission mechanisms be prepare it is efficient, controllable
The theoretical foundation of electron emitting device.
Traditional thermionic emission device mainly uses resistance heating manner, heats low-work-function material, reaches
1000 DEG C or more, and by applying grid voltage and accelerating field, realize the continuous transmitting of electronics.Due to this radiation pattern base
In thermionic emission pattern, electron emission source needs to maintain higher temperature for a long time, and electronics just can be achieved stablizes transmitting, from
And the response time is longer, can not be directly realized by electronic dither transmitting.Though Field Electron Emission has the characteristics that instant response,
High-frequency impulse transmitting can be achieved, but need high field strong (about several kilovolts every micron), in practical applications to high-voltage isulation, vacuum
Degree, job stability and safe operation etc. propose very high requirement.
Invention content
In view of this, an embodiment of the present invention provides a kind of photoinduced electron emission source and its manufacturing method, electron emission dresses
It sets, photoemission is efficient, vacuum level requirements are low, stability is high, preparation method is simple, at low cost；It can realize direct current or height
Frequency impulse ejection, and fast response time.
In a first aspect, an embodiment of the present invention provides a kind of manufacturing methods of photoinduced electron emission source, including：
Choose the conductive substrates for being suitble to carbon nano tube growth；
The deposit catalyst layers in the conductive substrates；
Carbon nanotube is grown on the catalyst layer.
Second aspect, the embodiment of the present invention additionally provide a kind of electron emission source for electron emitting device.
The third aspect, the embodiment of the present invention additionally provide a kind of electron emitting device, including：
Vacuum cavity, anode, electron emission source, cathode anchor, first can cut down, second can cut down, light source, light beam focus system
System, anode tap and cathode leg；
Anode, electron emission source and cathode anchor are equipped in the vacuum cavity；
Electron emission source is set on cathode anchor, and electron emission source and anode are opposite；
The anode tap can cut down by first and be connect with anode；The cathode leg can be cut down by second and cathode anchor
Connection；
The light source and light beam focusing system are set to the outside of vacuum cavity；
Light source, the light for providing irradiation electron emission source, so that electron electronics；
Light-resource fousing system, for being focused processing to the light that light source is sent out.
An embodiment of the present invention provides a kind of photoinduced electron emission source and its manufacturing method, electron emitting device, by
Deposit catalyst layers and photoinduced electron emission source prepared by carbon nanotube is grown in conductive substrates, emission current is close
Degree is big, photoemission is efficient, vacuum level requirements are low, stability is high, preparation method is simple, at low cost.
Description of the drawings
By reading a detailed description of non-restrictive embodiments in the light of the attached drawings below, of the invention other
Feature, objects and advantages will become more apparent upon：
Fig. 1 is that the embodiment of the present invention one provides a kind of manufacturing method flow chart of photoinduced electron emission source；
Fig. 2 a-2c are that each step of production method of the according to embodiments of the present invention one photoinduced electron emission source provided is corresponding
Structural section figure；
Fig. 3 is that the electron micrograph of carbon nanotube is completely covered in conductive substrates that the embodiment of the present invention one provides
Figure；
Fig. 4 is the flow diagram for the growth carbon nanotube method that the embodiment of the present invention one provides；
Fig. 5 a are a kind of structural schematic diagrams for photoinduced electron emission source that the embodiment of the present invention one provides；
Fig. 5 b are the structural schematic diagrams for another photoinduced electron emission source that the embodiment of the present invention one provides；
Fig. 6 is a kind of manufacturing method flow chart of photoinduced electron emission source provided by Embodiment 2 of the present invention；
Fig. 7a-7c is that each step of production method of the according to embodiments of the present invention two photoinduced electron emission sources provided is corresponding
Structural section figure；
Fig. 8 is the electron micrograph figure of Patterned Carbon Nanotube provided by Embodiment 2 of the present invention；
Fig. 9 a are a kind of structural schematic diagrams of photoinduced electron emission source provided by Embodiment 2 of the present invention；
Fig. 9 b are the structural schematic diagrams of another photoinduced electron emission source provided by Embodiment 2 of the present invention；
Figure 10 is that the embodiment of the present invention three provides a kind of structure chart of electron emitting device；
Figure 11 is that emission current is electric with anode when conductive substrates are completely covered in the carbon nanotube that the embodiment of the present invention three provides
The graph of relation of the variation of pressure；
Figure 12 is emission current and time when conductive substrates are completely covered in the carbon nanotube that the embodiment of the present invention three provides
Relation curve.
Specific implementation mode
The present invention is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining the present invention rather than limitation of the invention.It also should be noted that in order to just
In description, only some but not all contents related to the present invention are shown in the drawings.
Embodiment one
Fig. 1 shows that the embodiment of the present invention one provides a kind of manufacturing method flow chart of photoinduced electron emission source, such as Fig. 1 institutes
Show, the manufacturing method includes the following steps：
Step S11:Choose the conductive substrates for being suitble to carbon nano tube growth；
Step S12:The deposit catalyst layers in the conductive substrates；
Step S13:Carbon nanotube is grown on the catalyst layer.
Fig. 2 a-2c show each step pair of production method for the photoinduced electron emission source that according to embodiments of the present invention one provides
The structural section figure answered.
As shown in Figure 2 a, the conductive substrates 201 for being suitble to carbon nano tube growth are chosen.
The conductive substrates 201 are the silicon base, metallic substrates or two-dimentional conductive material substrate of doping.Wherein, doping
Silicon base is highly doped silicon base；Metallic substrates can be stainless steel substrates, molybdenum sheet or copper sheet etc.；Two-dimentional conductive material is novel
Two-dimentional conductive material, such as graphene or molybdenum disulfide.
As shown in Figure 2 b, the deposit catalyst layers 202 in the conductive substrates.
The catalyst layer 202 is deposited using iron, cobalt, nickel or the organic compound material containing iron-cobalt-nickel；It is described
The thickness of catalyst layer 202 is 0.5-20nm.Wherein, the organic compound material containing iron-cobalt-nickel is preferably ferrocene and iron egg
In vain.
As shown in Figure 2 c, carbon nanotube 203 is grown on the catalyst layer.
In the present embodiment, carbon nanotube is the carbon nanotube of growth in situ, a diameter of 1-30nm；Chemical gas may be used
It is prepared by phase sedimentation, arc discharge method, laser induced deposition etc..In the present embodiment, carbon nanotube can take for height
To vertical growth pattern, or the random growth pattern of random orientation.
In the present embodiment, the method for preferably chemical vapor deposition grows carbon nanotube, and carbon nanotube, which is completely covered, to be led
Electric substrate (as shown in Figure 3).Fig. 4 shows the flow diagram of growth carbon nanotube method, as shown in figure 4, in the catalysis
Carbon nanotube is grown in oxidant layer includes：
Step S111:There are the conductive substrates of catalyst layer to be put on the specimen holder of depositing device deposition, to depositing device
Carry out vacuum pumping；
Step S112:When the vacuum degree of depositing device is not more than 10-2When Pa, hydrogen is passed into depositing device, is controlled
The vacuum degree of depositing device heats between 10-500Pa, and to conductive substrates.
Wherein, the mass flow of the hydrogen is 50-1000sccm.
Step S113：After the temperature of conductive substrates reaches growth temperature, carbon-source gas is passed into depositing device, is passed through
After the outgrowth time, the conductive substrates that grown carbon nanotube are taken out in cooling.
Wherein, the carbon-source gas is preferably CH4、C2H2Or the mixed gas of the two；The mass flow of carbon-source gas
For 10-200sccm；The growth temperature is 550-850 DEG C；The growth time is 1-120min.
On the basis of the above embodiments, further include operating as follows in the conductive substrates before deposit catalyst layers：
Multiple metal layers are deposited in the conductive substrates.
Specifically, the multiple metal layer using the single metal materials such as antimony, copper, aluminium, gold, silver, molybdenum and tungsten and antimony,
One or more of copper, aluminium, gold, silver, the arbitrary alloy of molybdenum and tungsten, nitridation antimony, zinc oxide or silica be sequentially depositing and
At.For example, multiple metal layers can be Ti (100nm)/Cu (20nm)/Al (10nm)/Fe (2nm).The multiple metal layer
Thickness is 10-500nm, and the number of the multiple metal layer is 1-5；Correspondingly, catalyst layer uses iron, cobalt, nickel or iron cobalt
The alloy of nickel or organic compound material containing iron-cobalt-nickel deposit.Multiple metal layers are deposited in conductive substrates to be carried
The electric conductivity of the adhesiveness and guarantee conductive substrates of high carbon nanotube and conductive substrates.
Fig. 5 a show that a kind of structural schematic diagram for photoinduced electron emission source that the embodiment of the present invention one provides, application are above-mentioned
Manufacturing method prepared.As shown in Figure 5 a, the electron emission source includes：Conductive substrates 501, catalyst layer 502 and carbon
Nanotube 503.Wherein, carbon nanotube is the carbon nanotube of growth in situ, a diameter of 1-30nm；Chemical vapor deposition may be used
It is prepared by method, arc discharge method, laser induced deposition etc..Carbon nanotube can be highly oriented vertical growth pattern,
It can be the random growth pattern of random orientation.
Figure 5b shows that the structural schematic diagrams for another photoinduced electron emission source that the embodiment of the present invention one provides；Such as Fig. 5 b
Shown, the electron emission source includes：Conductive substrates 501, multiple metal layers 504, catalyst layer 502 and carbon nanotube 503,
Wherein, multiple metal layers 504 can improve the adhesiveness for improving carbon nanotube and conductive substrates and ensure leading for conductive substrates
Electrically.
The present embodiment one provides a kind of photoinduced electron emission source and its manufacturing method, is urged by being deposited in conductive substrates
Agent layer and the photoinduced electron emission source that is prepared of growth carbon nanotube, emission is big, photoemission efficiency
Height, vacuum level requirements are low, stability is high, preparation method is simple, at low cost.
Embodiment two
Fig. 6 shows a kind of flow chart of the manufacturing method of photoinduced electron emission source provided by Embodiment 2 of the present invention；Such as
Shown in Fig. 6, the method includes the following steps：
Step S61:Choose the conductive substrates for being suitble to carbon nano tube growth.
Step S62:Prepare patterned catalytic oxidant layer as needed in the conductive substrates.
Step S63:Carbon nanotube is grown on the catalyst layer.
Fig. 7a-7c shows each step pair of production method for the photoinduced electron emission source that according to embodiments of the present invention two provide
The structural section figure answered.
As shown in Figure 7a, the conductive substrates 701 for being suitble to carbon nano tube growth are chosen.
The conductive substrates 701 are the silicon base, metallic substrates or two-dimentional conductive material substrate of doping.Wherein, doping
Silicon base is highly doped silicon base；Metallic substrates can be stainless steel substrates, molybdenum sheet or copper sheet etc.；Two-dimentional conductive material is novel
Two-dimentional conductive material, such as graphene or molybdenum disulfide.
As shown in Figure 7b, patterned catalytic oxidant layer 702 is prepared as needed in the conductive substrates..
In the present embodiment, the catalyst layer 702 is using iron, cobalt, nickel or the organic compound material containing iron-cobalt-nickel
It deposits；The thickness of the catalyst layer 702 is 0.5-20nm.Wherein, the organic compound material containing iron-cobalt-nickel can be with
For ferrocene and ferritin.
In the present embodiment, patterned catalyst layer is prepared using ultraviolet photolithographic technology, specific operating method is：
Deposit catalyst layers in conductive substrates, are then coated with photoresist on catalyst layer, are carried out to photoresist by mask plate ultraviolet
Light irradiates, and the photoresist crossed by ultraviolet light is removed by developing process, and not being photo-etched glue by etching technics removal covers
The catalyst layer of lid finally removes the photoresist on catalyst layer, obtains patterned catalyst layer.
As shown in Figure 7 c, carbon nanotube 703 is grown on the catalyst layer.
In the present embodiment, carbon nanotube is the carbon nanotube of growth in situ, a diameter of 1-30nm；Chemical gas may be used
It is prepared by phase sedimentation, arc discharge method, laser induced deposition etc..In the present embodiment, carbon nanotube can take for height
To vertical growth pattern, or the random growth pattern of random orientation.=
Wherein, in the present embodiment, the method for preferably chemical vapor deposition grows carbon nanotube, grows carbon nanotube
Method follows the method described in embodiment one, and no longer this tires out and states.
In the present embodiment, by obtaining patterned carbon nanotube, the pattern of preparation on patterned catalyst layer
The carbon nanotube of change is as shown in figure 8, the carbon nanotube is the carbon nanotube of patterned vertical growth.
On the basis of the above embodiments, it can also adopt and prepare patterned carbon nanotube with other methods, to preparing
Method is not restricted.
Fig. 9 a are a kind of structure chart of photoinduced electron emission source provided by Embodiment 2 of the present invention；Using above-mentioned manufacturer
It is prepared by method.As illustrated in fig. 9, the electron emission source includes：Conductive substrates 901, catalyst layer 902 and carbon nanotube
903.Wherein catalyst layer 902 and carbon nanotube 903 are in the pattern form of setting.
On the basis of the above embodiments, the present embodiment two additionally provides the structure chart of another photoinduced electron emission source,
As shown in figure 9b, the electron emission source includes：Conductive substrates 901, multiple metal layers 904, catalyst layer 902 and carbon nanotube
903, wherein multiple metal layers 904, catalyst layer 902 and carbon nanotube 903 are in the pattern form of setting.
Second embodiment of the present invention provides a kind of manufacturing methods of photoinduced electron emission source, by being prepared in conductive substrates
Patterned catalytic oxidant layer obtains patterned carbon nanotube, passes through electron emission source obtained by the above method, emission
Greatly, photoemission is efficient, vacuum level requirements are low, stability is high, preparation method is simple, at low cost.
Embodiment three
Figure 10 shows a kind of electron emitting device structure chart that the embodiment of the present invention three provides, wherein arrow is light source
The light sent out；Photoinduced electron emission source prepared by above-described embodiment is applied in photoinduced electron emitter, such as Figure 10 institutes
Show, the electron emitting device, including：
Vacuum cavity 1001, anode 1002, electron emission source 1003, cathode anchor 1004, first can cut down 1005, second can
Cut down 1006, light source 1007, light beam focusing system 1008, anode tap 1009 and cathode leg 1010.
Anode 1002, electron emission source 1003 and cathode anchor 1004 are equipped in the vacuum cavity 1001；Wherein, vacuum
Glass or the stainless steel with incident window, such as 304 steel may be used in cavity 1001.
Electron emission source 1003 is set on cathode anchor 1004, and electron emission source 1003 and anode 1002 are opposite；Wherein, cloudy
Pole holder 1004 can be used metal, transparent conducting glass, transparent conductive polymer or other conductive materials and be made；Metal is preferably
Iron, molybdenum or nickel；Transparent conducting glass is preferably indium oxide tin glass.
The anode tap 1009 can cut down 1005 by first and be connect with anode 1002；The cathode leg 1010 passes through
Two can cut down 1006 connect with cathode anchor 1004；The light source 1007 and light beam focusing system 1008 are set to vacuum cavity 1001
It is external；Light source 1007, the light for providing irradiation electron emission source, so that 1003 launching electronics of electron emission source；Light source is poly-
Burnt system 1008, the light for being sent out to light source 1007 are focused processing.
In the present embodiment, light source be preferably laser, laser diode or the ordinary light source of high brightness.The electronics
Plane where emission source 1003 and cathode anchor 1004 and the angle of cathode leg 1010 or anode tap 1009 0-90 ° it
Between；The angle for 1003 exterior normal of incident direction and electron emission source that the light source 1007 emits beam is between 0-180 °.Institute
The output for stating the luminous power of light source is direct current output or the pulse way of output；Wherein, when the luminous power of the light source is that pulse is defeated
When going out mode, the pulse width of output is between 10fs-1s.
When being worked using above-mentioned photoinduced electron emitter, when the luminous power output of light source is direct current output mode
When, it is observed that apparent emission current, with the increase of anode voltage, emission current is presented under the effect of lower anode
The transmitting feature of saturation, in above process, the mode of electron electronics is thermionic emission；Continue growing anode
Voltage, emission current quickly increase, and the mode of launching electronics is changed into thermionic emission and the coefficient compound hair of Flied emission
Penetrate mode.Figure 11 shows that emission current is with the relation curve of the variation of anode voltage when conductive substrates are completely covered in carbon nanotube
Figure；As shown in figure 11, when anode voltage is 20V, apparent emission current can be observed；When anode voltage is in 1500V or less
When, emission current is in saturation emission feature, and electron emission mode is thermionic emission；When anode voltage is higher than 1500V, transmitting
Electric current continues to increase, and electron emission mode is thermionic emission and the coefficient composed emission mode of Flied emission.It can be seen that
By the electron emitting device of application photoinduced electron emission source, emission is big, and photoelectric emissivity is high.
When the output of the luminous power of light source is the pulse way of output, electron emitting device works in a pulsed fashion, hair
Radio stream and time are in the relationship of pulse.The pulse frequency and pulse width of emission current with depend on light source.Figure 12 is shown
The relation curve of emission current and time when conductive substrates are completely covered in carbon nanotube, as shown in figure 12, emission current and time
In the relationship of pulse, wherein the pulse width of emission current is 8ms, pulse frequency 40HZ.
The embodiment of the present invention three provides a kind of electron emitting device, is sent out using the photoinduced electron manufactured in above-described embodiment
Source is penetrated, has the advantages that emission is big, photoemission is efficient, and the output side by regulating and controlling the luminous power of light source
Formula realizes the direct current of electronics or the transmitting of pulse, fast response time, stability height.
Note that above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that
The present invention is not limited to specific embodiments described here, can carry out for a person skilled in the art it is various it is apparent variation,
It readjusts and substitutes without departing from protection scope of the present invention.Therefore, although being carried out to the present invention by above example
It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also
May include other more equivalent embodiments, and the scope of the present invention is determined by scope of the appended claims.
Claims (9)
1. a kind of electron emitting device, which is characterized in that including：
Vacuum cavity anode, electron emission source, cathode anchor, first can cut down, second can cut down, light source, light beam focusing system, sun
Pole lead and cathode leg；
Anode, electron emission source and cathode anchor are equipped in the vacuum cavity；
Electron emission source is set on cathode anchor, and electron emission source and anode are opposite；
The anode tap can cut down by first and be connect with anode；The cathode leg can be cut down by second to be connected with cathode anchor
It connects；
The light source and light beam focusing system are set to the outside of vacuum cavity；
Light source, the light for providing irradiation electron emission source, so that electron electronics；
Light-resource fousing system, for being focused processing to the light that light source is sent out；
Wherein, the output of the luminous power of the light source is direct current output or the pulse way of output；When the luminous power of the light source is
When the pulse way of output, the pulse width of output is between 10fs-1s；The mode of the electron electronics is thermoelectricity
Sub- radiation pattern；
When using electron emitting device work, if the luminous power output of the light source is direct current output mode, in anode
Under the action of voltage, emission current is generated, with the increase of anode voltage, emission current is in the transmitting feature being saturated；
The electron emission source is photoinduced electron emission source；The photoinduced electron emission source is manufactured based on following method：
Choose the conductive substrates for being suitble to carbon nano tube growth；
The deposit catalyst layers in the conductive substrates；
Carbon nanotube is grown on the catalyst layer, wherein the carbon nanotube is vertical growth mode.
2. the apparatus according to claim 1, which is characterized in that plane where the electron emission source and cathode anchor with
The angle of cathode leg or anode tap is between 0-90 °；Outside the incident direction and electron emission source that the light source emits beam
The angle of normal is between 0-180 °.
3. the apparatus according to claim 1, which is characterized in that in the conductive substrates before deposit catalyst layers, also
Including：
Multiple metal layers are deposited in the conductive substrates.
4. device according to claim 1 or 3, which is characterized in that deposit catalyst layers include in the conductive substrates：
Prepare patterned catalytic oxidant layer as needed in the conductive substrates.
5. the apparatus according to claim 1, which is characterized in that the conductive substrates are the silicon base of doping, metallic substrates
Or two-dimentional conductive material substrate.
6. the apparatus according to claim 1, which is characterized in that the catalyst layer is using iron, cobalt, nickel or contains iron-cobalt-nickel
Organic compound material deposit；The thickness of the catalyst layer is 0.5-20nm.
7. device according to claim 3, which is characterized in that
The thickness of the multiple metal layer is 10-500nm, and the number of the multiple metal layer is 2-5；
Catalyst layer is deposited using the alloy of iron, cobalt, nickel or iron-cobalt-nickel or the organic compound material containing iron-cobalt-nickel.
8. the apparatus according to claim 1, which is characterized in that described to grow carbon nanotube, packet on the catalyst layer
It includes：
There are the conductive substrates of catalyst layer to be put on the specimen holder of depositing device deposition, depositing device is carried out to vacuumize behaviour
Make；
When the vacuum degree of depositing device is not more than 10-2When Pa, hydrogen is passed into depositing device, controls the vacuum of depositing device
Degree heats between 10-500Pa, and to conductive substrates；
After the temperature of conductive substrates reaches growth temperature, carbon-source gas is passed into depositing device, by growth time it
Afterwards, the conductive substrates that grown carbon nanotube are taken out in cooling.
9. device according to claim 8, which is characterized in that the mass flow of the hydrogen is 50-1000sccm；It is described
The mass flow of carbon-source gas is 10-200sccm；The growth temperature is 550-850 DEG C；The growth time is 1-
120min。
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| WO2009013677A1 (en) * | 2007-07-24 | 2009-01-29 | Philips Intellectual Property & Standards Gmbh | Thermionic electron emitter and x-ray source including same |
| US8837678B2 (en) * | 2011-08-12 | 2014-09-16 | Creative Electron, Inc. | Long-lasting pulseable compact X-ray tube with optically illuminated photocathode |
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| CN103227082A (en) * | 2012-12-22 | 2013-07-31 | 深圳先进技术研究院 | X-ray emitting device and X-ray generating method |
| CN103311089A (en) * | 2013-04-12 | 2013-09-18 | 李鹏 | Photoelectric-effect ion source based on carbon nano-tubes |
| CN104124122A (en) * | 2014-07-31 | 2014-10-29 | 国家纳米科学中心 | Method for improving carbon nanotube field emitting performance through diamond-like carbon film |
| CN104176701A (en) * | 2014-08-18 | 2014-12-03 | 中国科学院上海应用物理研究所 | Gold nanoparticle thin film wrapped by organic ligand and field electron emission device of gold nanoparticle thin film |
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Inventor after: Dai Qing Inventor after: Li Zhenjun Inventor after: Li Chi Inventor after: Bai Bing Inventor before: Li Zhenjun Inventor before: Li Chi Inventor before: Bai Bing Inventor before: Dai Qing |
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| GR01 | Patent grant | ||
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