CN106229245A - A kind of explosion type Graphene electronic cathode and production method thereof - Google Patents

A kind of explosion type Graphene electronic cathode and production method thereof Download PDF

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CN106229245A
CN106229245A CN201610819504.5A CN201610819504A CN106229245A CN 106229245 A CN106229245 A CN 106229245A CN 201610819504 A CN201610819504 A CN 201610819504A CN 106229245 A CN106229245 A CN 106229245A
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graphene oxide
graphene
explosion type
cathode
electronic cathode
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CN106229245B (en
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柳建龙
杨锦标
曾葆青
宋林川
吴喆
黎晓云
傅文杰
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University of Electronic Science and Technology of China
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J23/00Details of transit-time tubes of the types covered by group H01J25/00
    • H01J23/02Electrodes; Magnetic control means; Screens
    • H01J23/04Cathodes
    • 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
    • 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

Abstract

This invention belongs to the explosion type Graphene electronic cathode in microwave vacuum electronic device and production method;Electronic cathode includes metal or graphite basis negative electrode and Graphene top layer: production method includes: producing of graphene oxide, produce containing the miscellaneous and suspension of powdery graphene oxide and graphene oxide suspension, graphene oxide powder, preparation graphene oxide electrophoresis liquid or slurry, explosion type Graphene electronic cathode idiosome processed, produces explosion type Graphene electronic cathode.This invention is owing to using Graphene as electronic cathode material, the thickness of its atom level and produce substantial amounts of emission edge and launch point is conducive to quickly, persistently forming plasma graphene oxide being carried out reduction sintering, and cover the emitting surface of whole negative electrode.Thus it is short to have the time that pulse toggle speed is fast, launch raising and lowering, pulse duration length and current waveform is good, impulse-free robustness, production technology is reliable, low cost, efficiency are high, it is easy to accomplish the features such as industrialized production.

Description

A kind of explosion type Graphene electronic cathode and production method thereof
Technical field
The invention belongs to microwave vacuum electronic device production technical field, particularly one and relate to Flied emission microwave vacuum device Explosion type Graphene electronic cathode in part and production method thereof, the electronic cathode using the method to be produced is alternatively arranged as projection The negative electrode of the related electronic devices such as pipe uses.
Background technology
Outburst field-transmitting cathode can produce strong current electron beam, the high current electricity that these negative electrodes produce in high-pressure pulse electric Son bundle, is referred to as Explosion electron emission, can apply to HIGH-POWERED MICROWAVES device such as relativistic magnetron, relativistic backward wave oscillator etc., High-power pulsed ion beams has important effect at electronic countermeasure and the field such as material modification, food safety.Cathode performance is Restrict these devices or the key factor of systematic function raising, great pulsed emission current intensity should be met and electric current is close Degree, keeps the pulse width of the cathode current emission and the stability of transmitting again in the case of the biggest electric current.
Traditional high-power microwave vacuum electronic device negative electrode, its cathode material typically uses metal (as rustless steel, tungsten close Gold etc.), graphite, velvet, CNT, carbon fiber etc..This type of negative electrode exists that emission effciency is low, operating temperature is high and needs The defects such as preheating time.For these defects, at " Research on An Improved Explosive Emission Cathode (research of a kind of modified model explosion type negative electrode) " (see " Journal of Physics D:Applied Physics " 2009,42,125204) document discloses a kind of follow-on graphite explosion type negative electrode, this explosion type negative electrode is first First negative electrode based on traditional graphite cathode is immersed in transformer oil, after heating in water bath, ultrasonic cleaning, then be placed in baking Dry in case, oil immersed type graphite cathode must be obtained;The experiment proved that the emitting performance of this oil immersed type graphite cathode is compared to biography System graphite cathode has obtained a certain degree of raising and has extended service life;But oil immersed type graphite cathode exists: first, if When using negative electrode based on other traditional materials (such as rustless steel etc.), the party's rule is invalid;Second, owing to anode and cathode gap is fast Speed Guan Bi and diode impedance change over, and its electron emission there is inhomogeneities and repeatability is poor, the repetition of pulse frequency The problems such as rate is not ideal enough with pulsewidth;The controllability that particularly electron beam is launched is poor, current waveform has relatively with voltage waveform The defects such as big difference, constrain the most again the application as high current electronic cathode of this explosion type negative electrode.
And for example at document " High Intensity, Pulsed Electron Beam from Carbon Nanotube Cathodes (high intensity pulses electron beam carbon nanotube cathod) " (seeing " Carbon " 2007,45,1471-1475) and document 《Mechanism of Explosive Electron Emission for Dielectric Fiber(velvet) Cathodes (the explosion type electron emission mechanism of media fibers (velvet) negative electrode) " (see " Journal of Applied Physics " 1998,84 (7), 3880-3889) in, disclose and be respectively adopted CNT and velvet material as blast Penetrate negative electrode (explosion type negative electrode).But this type of explosion type negative electrode exists, and launched impulse waveform is undesirable and the hair of impulse waveform Sting the defects such as more, to be unfavorable for electron beam modulation and application.
Summary of the invention
It is an object of the invention to the defect existed for background technology, a kind of explosion type Graphene electronic cathode of research and development And production method, short to reach work time pulse and rush that toggle speed is fast, to launch the time of raising and lowering, the pulse duration Long, pulse current waveform is good and impulse-free robustness, and production technology is reliable, low cost, efficiency height, it is easy to accomplish industrialized production etc. Purpose.
The solution of the present invention is by negative electrode based on the metal of direct for tradition divergent bundle, graphite cathode, so After on the surface at the electron emission position of this basis negative electrode, use the method such as electrophoresis, pulsed laser deposition, coating to lay equably (covering) one layer of graphene oxide or letter cover layer Han graphene oxide, after sinter through reduction thus make explosion type Graphene Electronic cathode.The present invention uses Graphene to launch electronic cathode material as explosion type, the thickness of its atom level and at oxidation stone Ink alkene carries out producing substantial amounts of tradition after reduction sinters the decomposition of its functional group and is considered emission edge and the launch point of defect, these Emission edge and launch point are particularly conducive to the emitting surface quickly forming and covering whole negative electrode of more plasma, Make this explosion type negative electrode have a faster toggle speed, fabulous impulse waveform and impulse-free robustness, launch raising and lowering time Between short, the persistent period is long.Thus, explosion type Graphene electronic cathode of the present invention includes that metal or graphite basis negative electrode, key exist Being additionally provided with a graphene layer in the surface at the electron emission position at basis negative electrode, this graphene layer is launched with basis cathode electronics Portion faces is fastened together thus constitutes explosion type Graphene electronic cathode.
The described surface at the electron emission position of basis negative electrode is additionally provided with a graphene layer, the thickness of graphene layer: when When using electrophoresis, pulsed laser deposition mode to arrange graphene layer, its thickness is 50-500 μm;And when the mode using coating sets When putting graphene layer, its thickness is 1-3mm.
The production method of explosion type Graphene electronic cathode of the present invention, including:
Producing of step 1. graphene oxide: expansible graphite is put in microwave oven or high temperature Muffle furnace 500~ 1000 DEG C are heated 5-30min, expansible graphite is sufficiently expanded, obtains the thickness < nano graphite flakes of 100nm;So After graphite flake is placed in agitator, and add strong oxidizer and strong acid, under agitation nano graphite flakes carried out intercalation Oxidation, intercalation oxidization time is 8-15 hour, obtains graphene oxide;
Step 2. is produced containing the miscellaneous and suspension of powdery graphene oxide: the graphene oxide of step 1 gained is spent from Sub-water removes remaining acid, and the graphene oxide after acid being removed is placed in the container with deionized water and carries out Ultrasonic Pulverization, Obtain containing the miscellaneous and suspension of powdery graphene oxide;
Step 3. produces graphene oxide suspension: step 2 gained suspension is put into centrifugal filtration in centrifuge, to remove Remove graphite flake and other solid impurity not having complete oxidation, obtain graphene oxide suspension;
Step 4. produces graphene oxide powder: use microporous filter membrane to carry out step 3 gained graphene oxide suspension Filter and separate, then microporous filter membrane is placed in baking oven drying together with the graphene oxide filtered on it, obtains graphene oxide Powder;
Step 5. prepares graphene oxide electrophoresis liquid or slurry:
5a. prepares graphene oxide electrophoresis liquid: by the graphene oxide powder of step 4 gained, by graphene oxide powder: After the weight ratio of slaine=1:0.8-1.5 adds slaine mix homogeneously, add in organic solution, be configured to concentration be 1~ The graphene oxide electrophoresis liquid of 100mg/ml is stand-by;Or
5b. prepares graphene oxide slurry: add industry silver slurry in the graphene oxide powder of step 4 gained, by oxygen Functionalized graphene powder: after the ratio of industry silver slurry=1:1-7 is uniformly mixed, be configured to graphene oxide slurry stand-by;
Step 6. explosion type processed Graphene electronic cathode idiosome:
Metal or graphite basis negative electrode are placed in by step 5a gained graphene oxide electrophoresis liquid as anode, at electric field Intensity is to carry out electrophoretic process under conditions of 10~100V/mm, makes the graphene oxide in solution adsorb in metal or graphite-based Plinth cathode electronics launches portion faces, and the electrophoretic process time is 10~120min, obtains the explosion type stone that top layer is graphene oxide Ink alkene electronic cathode idiosome;Or the electronics that step 5b gained graphene oxide slurry is coated on metal or graphite basis negative electrode sends out Penetrate portion faces, the explosion type Graphene electronic cathode idiosome of graphene oxide after cured process, must be contained;
Step 7. produces explosion type Graphene electronic cathode: by step 6 gained electronics after electrophoretic process or coating processing Negative electrode idiosome is placed in sintering furnace, carries out reduction and burn in vacuum condition or inert gas atmosphere and at a temperature of 300~1000 DEG C Knot, with the functional group removed in graphene oxide the adhesive force improving top layer and basis negative electrode, obtains explosion type Graphene electronics Negative electrode.
The most described strong oxidizer is potassium permanganate or high potassium phosphate, high sodium phosphate;Described strong acid is sulphuric acid or nitre Acid, hydrochloric acid;Wherein the weight ratio between graphite flake and strong oxidizer, strong acid is: graphite flake: strong oxidizer: strong acid=1:3-6: 80-120。
The most described microporous filter membrane is placed in baking oven drying together with the graphene oxide filtered on it, dries temperature Degree is 40-80 DEG C, the time is 1-5 hour;
It is magnesium nitrate or magnesium chloride, sodium chloride in slaine described in step 5a;And described machine solution is isopropanol or second Alcohol;And the most described industry silver slurry, its silver content (percentage by weight) is 70-90wt%.
Cured described in step 6, the temperature of cured: intermediate temperature setting is processed as 50~100 DEG C, hot setting processes It it is 100~200 DEG C.
Carrying out reduction sintering described in step 7, its sintering time is 1-10 hour.
The present invention is by negative electrode based on the metal of direct for tradition divergent bundle, graphite cathode, then at basis negative electrode The surface at electron emission position, one layer of graphene oxide be set equably, then through reduction sintering thus make emitting surface tool There is the explosion type Graphene electronic cathode of a large amount of emission edge and launch point;The inventive method is then to be processed into expanded graphite to receive Rice graphite flake, then obtain graphene oxide powder through intercalation oxidation, Ultrasonic Pulverization, drying and processing, owing to graphene oxide is to adopt Carrying out prepared by intercalation oxidation with strong acid and strong oxidizer, therefore there is substantial amounts of Guan Nengtuan in the surface at graphene oxide;This Invention uses Graphene to launch electronic cathode material as explosion type, the thickness of its atom level and carrying out graphene oxide also After former sintering, its functional group decompose and produce substantial amounts of emission edge and launch point, be more beneficial for occur dielectric surface flashover continue shape Become plasma, make substantial amounts of plasma quickly be formed and cover the emitting surface of whole negative electrode, it is ensured that emission current is steady Qualitative;The toggle speed of the present invention its explosion type pulse current compared with background technology improves about 3 times, pulse duration prolongation 8 times, and the good impulse-free robustness of pulse shape, beneficially wave filter is filtered.Thus the present invention has work time pulse and rushes toggle speed It is short hurry up, launch time of raising and lowering, and pulse duration length, pulse current waveform be good and impulse-free robustness, and production technology Reliably, low cost, efficiency height, it is easy to accomplish the features such as industrialized production.
Accompanying drawing explanation
Fig. 1 is the atomic force microscope images that the inventive method gained thickness is about the graphene oxide of 1nm;
Fig. 2 is the scanning electron microscope diagram sheet of the embodiment of the present invention 1 gained explosion type Graphene electronic cathode;In picture Demonstrate that its surface is evenly distributed with a large amount of emission edge and launch point;
Fig. 3 is embodiment 1 explosion type Graphene electronic cathode electrode structure schematic diagram;In figure, 1 is Graphene, and 2 is arc head Stainless steel base negative electrode;
Fig. 4 is that the embodiment of the present invention 1 carries out target practice contrast test curve chart with background technology;In figure 1 be conventional arched not The current waveform profile of rust steel negative electrode;2 is embodiment 1 current waveform profile.
Detailed description of the invention
Embodiment 1: the present embodiment is based on traditional stainless steel cathode as a example by negative electrode, and its method is:
Producing of step 1. graphene oxide: 1g expansible graphite is put in high temperature Muffle furnace and heat in 900 DEG C 10min, makes expansible graphite sufficiently expand, and obtains the thickness < nano graphite flakes of 100nm;Then graphite flake is placed in In agitator, and add potassium permanganate and concentrated sulphuric acid carries out intercalation oxidation, nano-graphite to nano graphite flakes under agitation Sheet: potassium permanganate: concentrated sulphuric acid=1.0g:4g:100ml;Intercalation oxidization time is 12 hours, obtains graphene oxide;
Step 2. is produced containing the miscellaneous and suspension of powdery graphene oxide: the graphene oxide of step 1 gained is spent from Sub-water removes remaining acid, is placed in the container with deionized water by the graphene oxide after deacidification and carries out Ultrasonic Pulverization, powder Broken power is 160W, obtains containing the miscellaneous and aaerosol solution of powdery graphene oxide;
Step 3. produces graphene oxide suspension: by step 2 gained containing the miscellaneous and aaerosol solution of powdery graphene oxide Put into and centrifuge is centrifuged filter, to remove graphite flake and other solid impurities not having complete oxidation, obtain oxidation stone Ink alkene suspension;
Step 4. produces graphene oxide powder: step 3 gained graphene oxide suspension is used filtering with microporous membrane Separate, leach moisture after, the microporous filter membrane with graphene oxide is placed in baking oven, at a temperature of 50 DEG C dry 3.5 hours, Obtain graphene oxide powder;
Step 5. prepares graphene oxide electrophoresis liquid or slurry: add magnesium nitrate to step 4 gained graphene oxide powder, After mix homogeneously, add in isopropanol, be configured to the graphene oxide electrophoresis liquid that concentration is 50mg/ml;Wherein: graphite oxide Alkene: magnesium nitrate=1:1;
Step 6. explosion type processed Graphene electronic cathode idiosome: be 30mm by overall diameter, interior diameter is 24mm, and height is The arc head stainless steel base negative electrode of 50mm inserts in graphene oxide electrophoresis liquid as negative electrode, and head inserts the degree of depth of solution and is 15mm, carries out electrophoretic process under conditions of electric field intensity is 40V/mm, makes the graphene oxide in solution adsorb at arc head Stainless steel cathode surface, the electrophoretic process time is 70min, obtains the explosion type Graphene electronic cathode embryo that top layer is graphene oxide Body;
Step 7. produces explosion type Graphene electronic cathode: be placed in very by the graphene oxide negative electrode idiosome of step 6 gained Under empty condition, at a temperature of 800 DEG C, reduction sintering 2 hours, carry out reduction treatment to graphene oxide, to remove graphene oxide In functional group and strengthen the adhesive force of Graphene and stainless steel base cathode surface simultaneously, obtain the explosion type that top layer is Graphene Graphene electronic cathode.
The present embodiment gained explosion type Graphene electronic cathode is arranged in the accelerator of the 500KV pulse power on an equal basis Under the conditions of carry out target practice contrast test with background technology;Fig. 4 is contrast test curve chart, in figure;1 is conventional arched rustless steel The current waveform of negative electrode, the rise time is 124ns, and the pulse duration is 10ns, and corresponding electric current is about 9700A;2 is this reality Executing the current waveform of example explosion type Graphene electronic cathode, the rise time is 48ns, and the pulse duration is 80ns, corresponding electricity Stream is about 10000A, and its toggle speed improves about 3 times, pulse persistance compared with the explosion type pulse current of tradition stainless steel cathode Time improves 8 times, and pulse shape is good, impulse-free robustness, beneficially wave filter are filtered.
Embodiment 2
The present embodiment is based on traditional graphite cathode as a example by negative electrode: step 1-4 all with embodiment 1 with;
The graphene oxide powder of step 4 gained is added magnesium nitrate by step 5., graphene oxide: magnesium nitrate=1:0.8, Add ethanol after mix homogeneously, be configured to the graphene oxide electrophoresis liquid that concentration is 60mg/ml;
Step 6. explosion type processed Graphene electronic cathode idiosome: be 24mm by overall diameter, interior diameter is 10mm, and height is In 20mm conventional graphite negative electrode inserting step 5 gained graphene oxide electrophoresis liquid, it is 20mm that negative electrode head inserts the degree of depth of solution, Under conditions of electric field intensity is 50V/mm, carries out electrophoretic process, makes the graphene oxide in solution adsorb at graphite cathode table Face, the electrophoretic process time is 60min, obtains the negative electrode idiosome that top layer is graphene oxide;
Step 7. produces explosion type Graphene electronic cathode: the graphene oxide negative electrode of step 6 gained is placed in indifferent gas In bromhidrosis atmosphere, at a temperature of 900 DEG C, reduction sintering 1.5 hours, carry out reduction treatment to graphene oxide, to remove graphite oxide Functional group in alkene and increase the adhesive force of Graphene and Graphene cathode surface, obtains the explosion type Graphene that top layer is Graphene Electronic cathode.
Embodiment 3
The present embodiment is based on traditional graphite cathode as a example by negative electrode: step 1-4 all with embodiment 1 with;
Step 5b. preparation graphene oxide slurry: adding silver content in the graphene oxide powder of step 4 gained is The conduction industry silver slurry being resistant to high temperature sintering of 75wt%, in graphene oxide powder: the ratio stirring of industry silver slurry=1:3 is mixed After closing uniformly, preparation graphene oxide slurry is stand-by;
Step 6. explosion type processed Graphene electronic cathode idiosome: step 5b gained graphene oxide slurry is coated on graphite The surface, electron emission position of basis negative electrode, cured 30 minutes at a temperature of 70 DEG C;
Step 7. produces explosion type Graphene electronic cathode: be placed in lazy by the graphene oxide negative electrode idiosome of step 6 gained Property gas atmosphere in, at a temperature of 900 DEG C reduction sintering 2 hours, to remove the functional group in graphene oxide, and increase coating Layer and the adhesive force on surface, graphite cathode electron emission position, obtain explosion type Graphene electronic cathode.

Claims (8)

1. an explosion type Graphene electronic cathode, including metal or graphite basis negative electrode, it is characterised in that at basis negative electrode The surface at electron emission position is additionally provided with a graphene layer, and this graphene layer is launched portion faces with basis cathode electronics and is tightened to One thus constitute explosion type Graphene electronic cathode.
2. explosion type Graphene electronic cathode as described in claim 1, it is characterised in that the described electron emission at basis negative electrode The surface at position is additionally provided with a graphene layer, the thickness of graphene layer: arrange graphite when using electrophoresis, pulsed laser deposition mode During alkene layer, its thickness is 50-500 μm;When the mode using coating arranges graphene layer, its thickness is 1-3mm.
3. the production method of explosion type Graphene electronic cathode as described in claim 1, including:
Producing of step 1. graphene oxide: expansible graphite is put in microwave oven or high temperature Muffle furnace at 500~1000 DEG C Middle heating 5-30min, sufficiently expands expansible graphite, obtains the thickness < nano graphite flakes of 100nm;Then by stone Ink sheet is placed in agitator, and adds strong oxidizer and strong acid, under agitation nano graphite flakes is carried out intercalation oxidation, inserts Layer oxidization time is 8-15 hour, obtains graphene oxide;
Step 2. is produced containing the miscellaneous and suspension of powdery graphene oxide: by the graphene oxide deionized water of step 1 gained Removing remaining acid, the graphene oxide after acid being removed is placed in the container with deionized water and carries out Ultrasonic Pulverization, obtains Containing the miscellaneous and suspension of powdery graphene oxide;
Step 3. produces graphene oxide suspension: step 2 gained suspension is put into centrifugal filtration in centrifuge, to remove not There are graphite flake and other solid impurity of complete oxidation, obtain graphene oxide suspension;
Step 4. produces graphene oxide powder: use microporous filter membrane to filter step 3 gained graphene oxide suspension Separate, then microporous filter membrane is placed in baking oven drying together with the graphene oxide filtered on it, obtains graphene oxide powder;
Step 5. prepares graphene oxide electrophoresis liquid or slurry:
5a. prepares graphene oxide electrophoresis liquid: by the graphene oxide powder of step 4 gained, by graphene oxide powder: metal After the weight ratio of salt=1:0.8-1.5 adds slaine mix homogeneously, add in organic solution, be configured to concentration be 1~ The graphene oxide electrophoresis liquid of 100mg/ml is stand-by;Or
5b. prepares graphene oxide slurry: add industry silver slurry in the graphene oxide powder of step 4 gained, by oxidation stone Ink alkene powder: after the ratio of industry silver slurry=1:1-7 is uniformly mixed, be configured to graphene oxide slurry stand-by;
Step 6. explosion type processed Graphene electronic cathode idiosome:
Metal or graphite basis negative electrode are placed in by step 5a gained graphene oxide electrophoresis liquid as anode, in electric field intensity It is to carry out electrophoretic process under conditions of 10~100V/mm, makes the graphene oxide absorption in solution cloudy at metal or graphite basis Surface, electron emission position, pole, the electrophoretic process time is 10~120min, obtains the explosion type Graphene that top layer is graphene oxide Electronic cathode idiosome;Or step 5b gained graphene oxide slurry is coated on metal or the electron emission part of graphite basis negative electrode Surface, position, must contain the explosion type Graphene electronic cathode idiosome of graphene oxide after cured process;
Step 7. produces explosion type Graphene electronic cathode: by step 6 gained electronic cathode after electrophoretic process or coating processing Idiosome is placed in sintering furnace, carries out reduction sintering in vacuum condition or inert gas atmosphere and at a temperature of 300~1000 DEG C, with Remove the functional group in graphene oxide and improve the adhesive force on top layer and basis negative electrode, obtaining explosion type Graphene electronic cathode.
4. the production method of explosion type Graphene electronic cathode as described in claim 3, it is characterised in that the most described by force Oxidant is potassium permanganate or high potassium phosphate, high sodium phosphate;Described strong acid is sulphuric acid or nitric acid, hydrochloric acid;Wherein graphite flake is with strong Weight ratio between oxidant, strong acid is: graphite flake: strong oxidizer: strong acid=1:3-6:80-120.
5. the production method of explosion type Graphene electronic cathode as described in claim 3, it is characterised in that the most described general Microporous filter membrane is placed in baking oven drying together with the graphene oxide filtered on it, dry temperature be 40-80 DEG C, the time be that 1-5 is little Time.
6. the production method of explosion type Graphene electronic cathode as described in claim 3, it is characterised in that described in step 5a Slaine is magnesium nitrate or magnesium chloride, sodium chloride;And described machine solution is isopropanol or ethanol;And the most described industry Silver slurry, its silver content (percentage by weight) is 70-90wt%.
7. the production method of explosion type Graphene electronic cathode as described in claim 3, it is characterised in that solidifying described in step 6 Processing, the temperature of cured: intermediate temperature setting is processed as 50~100 DEG C, hot setting is processed as 100~200 DEG C.
8. the production method of explosion type Graphene electronic cathode as described in claim 3, it is characterised in that enter described in step 7 Row reduction sintering, its sintering time is 1-10 hour.
CN201610819504.5A 2016-09-13 2016-09-13 A kind of explosion type graphene electronic cathode and its production method Expired - Fee Related CN106229245B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018217167A1 (en) * 2017-05-25 2018-11-29 National University Of Singapore Cathode structure for cold field electron emission and method of fabricating the same
CN109599313A (en) * 2018-12-06 2019-04-09 中国科学院兰州化学物理研究所 A kind of preparation method of Mxene flexible Field Emission cathode material
US20210222016A1 (en) * 2018-11-21 2021-07-22 Uduck Advanced Materials Graphene ink composition and method of preparing same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103346051A (en) * 2013-06-09 2013-10-09 中国科学院深圳先进技术研究院 Carbon nanometer tube negative electrode and method for preparing carbon nanometer tube negative electrode
CN104217907A (en) * 2014-09-12 2014-12-17 中国科学院深圳先进技术研究院 Preparation method for graphene field emitting cathode, and graphene field emitting cathode
US20150060757A1 (en) * 2013-09-02 2015-03-05 Kumoh National Institute Of Technology Field emission devices and methods of manufacturing gate electrodes thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103346051A (en) * 2013-06-09 2013-10-09 中国科学院深圳先进技术研究院 Carbon nanometer tube negative electrode and method for preparing carbon nanometer tube negative electrode
US20150060757A1 (en) * 2013-09-02 2015-03-05 Kumoh National Institute Of Technology Field emission devices and methods of manufacturing gate electrodes thereof
CN104217907A (en) * 2014-09-12 2014-12-17 中国科学院深圳先进技术研究院 Preparation method for graphene field emitting cathode, and graphene field emitting cathode

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HUA ZHAI等: "High Density Current Electron Emission from Graphene", 《VACUUM NANOELECTRONICS CONFERENCE (IVNC), 2016 29TH INTERNATIONAL》 *
JINBIAO YANG等: "Explosive field emission from graphene sheets", 《2015 28TH INTERNATIONAL VACUUM NANOELECTRONICS CONFERERNCE》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018217167A1 (en) * 2017-05-25 2018-11-29 National University Of Singapore Cathode structure for cold field electron emission and method of fabricating the same
CN110709959A (en) * 2017-05-25 2020-01-17 新加坡国立大学 Cathode structure for cold field electron emission and preparation method thereof
US11158479B2 (en) 2017-05-25 2021-10-26 National University Of Singapore Cathode structure for cold field electron emission and method of fabricating the same
CN110709959B (en) * 2017-05-25 2022-05-13 新加坡国立大学 Cathode structure for cold field electron emission and preparation method thereof
US20210222016A1 (en) * 2018-11-21 2021-07-22 Uduck Advanced Materials Graphene ink composition and method of preparing same
US11739228B2 (en) * 2018-11-21 2023-08-29 Uduck Advanced Materials Graphene ink composition and method of preparing same
CN109599313A (en) * 2018-12-06 2019-04-09 中国科学院兰州化学物理研究所 A kind of preparation method of Mxene flexible Field Emission cathode material

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