CN104701115B - Field emission cathode with double-layer nano-carbon coating and preparation method - Google Patents
Field emission cathode with double-layer nano-carbon coating and preparation method Download PDFInfo
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Abstract
The invention provides a field emission cathode with double-layer nano-carbon coating and a preparation method. The preparation method includes the steps: firstly, coating nano-diamond on a substrate by an electrophoretic deposition method to form a nano-diamond coating; coating a nano-carbon tube on the nano-diamond coating by the electrophoretic deposition method to form a nano-carbon tube coating; finally, performing heat treatment in a hot filament chemical vapor deposition system, and performing chemical bonding reaction of the substrate and the nano-diamond coating to obtain a chemical bonding layer. The field emission cathode is provided with a four-layer structure with the substrate, the chemical bonding layer, the nano-diamond coating and the nano-carbon tube coating, simultaneously has the advantages of the nano-carbon tube and the nano-diamond, and has fine field emission characteristics and field emission stability.
Description
Technical field
The present invention relates to the cathode of field emission display in electronic display technology field, it particularly relates to a kind of with double
The field-transmitting cathode and preparation method of layer nanometer carbon coating.
Background technology
CNT has low threshold voltage, big field enhancement factor, and big Flied emission electric current, is a kind of preferable
Filed emission cathode material.But thermally contacting between CNT and base material is poor so as to cause the steady of its emission current
It is qualitative poor, limit its application in Flied emission field.Nano diamond has very high thermal conductivity, and Nano diamond
Possess relatively low work function and negative electron affinity (NEA), be also a kind of outstanding filed emission cathode material.In substrate and CNT
Between add Nano diamond, thermally contacting between substrate and CNT can be improved, improve its field emission stability.
At present most field-transmitting cathodes with CNT or diamond as emitter are all adopted in substrate directly
The route of deposition growing carbon nanotube film or diamond thin is preparing.Although the Characteristics of Field Emitter Array is excellent, thin film
Growth course is complex, and growth area is restricted, and is unfavorable for realizing field-transmitting cathode to inexpensive, large-area practicality
Change direction to develop.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the present invention to provide a kind of have substrate --- chemical bonding
The field-transmitting cathode of the four-layer structure of layer --- nano diamond coating --- nano-carbon tube coating, i.e., apply with double-layer nanometer carbon
The field-transmitting cathode of layer (i.e. nano diamond coating and nano-carbon tube coating) structure.
Another object of the present invention is to a kind of preparation method of the field-transmitting cathode with double-layer nanometer carbon coating is provided,
Simply and efficiently preparing can take into account the field-transmitting cathode of field emission characteristic and field emission stability.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical scheme that and is achieved：
A kind of field-transmitting cathode with double-layer nanometer carbon coating, described field-transmitting cathode includes substrate, sinks in substrate
Product has nano diamond coating, and a stratification bonded layer is defined between substrate and nano diamond coating, and Nano diamond is applied
Deposition has nano-carbon tube coating on layer.
Field-transmitting cathode with double-layer nanometer carbon coating as above, described substrate is titanium substrate, described
Chemical bonding layer be TiC chemical bonding layers.
A kind of preparation method of the field-transmitting cathode with double-layer nanometer carbon coating as above, the method will be received first
Rice diamond is coated in substrate by the method for electrophoretic deposition, forms nano diamond coating；
Then CNT is coated on nano diamond coating by the method for electrophoretic deposition, forms CNT and apply
Layer；
Finally make substrate that chemical bonding reaction occur with nano diamond coating, obtain chemical bonding layer.
Preparation method as above, described substrate is titanium substrate, and described chemical bonding layer is TiC chemical bonds
Close layer.
The method specifically includes following steps：
Step one, selects metal titanium sheet as substrate, the one side of metal titanium sheet is ground, polish after be placed in acetone it is super
Sound is cleaned, Jing ethanol dehydrations after then deionized water is rinsed；
Step 2, configures Nano diamond electrophoresis liquid：It is Nano diamond from mass ratio：Iodine=1：2 mixture is
Solute；It is deionized water from volume ratio：Acetone：Isopropanol=1：1：20 mixed liquor is solvent, makes Nano diamond content
For 0.23mg/ml；
Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, 30 DEG C of ultrasonic temperature will be carried out after solute and solvent mixing
～40 DEG C, form the nano-diamond powder electrophoresis liquid of mix homogeneously；
Step 3, used as negative electrode, used as anode, two-plate spacing is 1cm to stainless steel substrates to the one side that metal titanium sheet is polished,
Electrophoretic voltage 60V, electrophoresis time 2min, in the one side of metal titanium sheet polishing nano diamond coating is deposited；
Step 4, configures CNT electrophoresis liquid：With CNT as solute, isopropanol is solvent, and both are mixed, and is made
The content of CNT is 0.2mg/ml；Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, ultrasound are carried out to mixture
30 DEG C～40 DEG C of temperature, forms the CNT electrophoresis liquid of mix homogeneously；
Step 5, metal titanium sheet has been had been coated with the one side of nano diamond coating as negative electrode, and stainless steel substrates are used as sun
Pole, two-plate spacing is 1cm, electrophoretic voltage 60V, electrophoresis time 8min, continues to deposit nanometer on nano diamond coating surface
Carbon pipe coating；
Step 6, by the metal titanium sheet that deposited nano diamond coating and nano-carbon tube coating vacuum heat system is inserted
Heat treatment is carried out in system, the vacuum of vacuum heat system is 3 × 10 during heat treatment-3Pa, temperature is 700 DEG C, process time
For 10min, chemical bonding is formed between substrate and nano-carbon material, obtain double-layer nanometer carbon coating field-transmitting cathode.
The present invention compared with prior art, has the following technical effect that：
The electrophoretic deposition process of the present invention is simple, is easily controlled, and negative electrode prepares yield height, with low cost, is adapted to batch raw
Produce；Can large area prepare, meet the large screen display requirement of flat faced display.
Double-layer nanometer carbon coating field-transmitting cathode proposed by the present invention has substrate --- chemical bonding layer --- nanometer gold
The four-layer structure of hard rock coating --- nano-carbon tube coating, wherein chemical bonding layer realize substrate and nano-carbon material coating it
Between secure bond, and provide electric transmission path from substrate to material with carbon element, nano diamond coating can not only improve substrate
With thermally contacting for CNT, also can be used as the second field emission body in addition to CNT.The field-transmitting cathode has both nanometer
The advantage of carbon pipe and Nano diamond, with good field emission characteristic (big Flied emission electric current, low threshold voltage) and field
Launch stability.
Description of the drawings
Fig. 1 is the structural representation of double-layer nanometer carbon coating field-transmitting cathode proposed by the present invention.
Fig. 2 is the SEM image of the titanium substrate used in embodiment.
Fig. 3 is the SEM image in embodiment after electrophoretic deposition Nano diamond in titanium substrate.
Fig. 4 is the SEM image in embodiment after electrophoretic deposition CNT on nano diamond coating.
Fig. 5 is the XRD figure that deposited the metal titanium sheet of nano diamond coating and nano-carbon tube coating after heat treatment
Spectrum.
Fig. 6 is the Flied emission J-E characteristic curves of embodiment.
Fig. 7 is the Flied emission F-N curves of embodiment.
Fig. 8 is the field emission stability test curve of embodiment.
Explanation is further explained in detail to the particular content of the present invention below in conjunction with drawings and Examples.
Specific embodiment
Defer to above-mentioned technical proposal, the specific embodiment of the present invention given below, it should be noted that the present invention not office
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
Enclose.
Embodiment：
The present embodiment provides a kind of preparation method of the field-transmitting cathode with double-layer nanometer carbon coating as above, should
Method specifically includes following steps：
Step one, selects metal titanium sheet as substrate, the one side of metal titanium sheet is ground, polish after be placed in acetone it is super
Sound is cleaned, Jing ethanol dehydrations after then deionized water is rinsed；
Step 2, configures Nano diamond electrophoresis liquid：It is Nano diamond from mass ratio：Iodine=1：2 mixture is
Solute；It is deionized water from volume ratio：Acetone：Isopropanol=1：1：20 mixed liquor is solvent, makes Nano diamond content
For 0.23mg/ml；
Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, 30 DEG C of ultrasonic temperature will be carried out after solute and solvent mixing
～40 DEG C, form the nano-diamond powder electrophoresis liquid of mix homogeneously；
Step 3, used as negative electrode, used as anode, two-plate spacing is 1cm to stainless steel substrates to the one side that metal titanium sheet is polished,
Electrophoretic voltage 60V, electrophoresis time 2min, in the one side of metal titanium sheet polishing nano diamond coating is deposited；
Step 4, configures CNT electrophoresis liquid：With CNT as solute, isopropanol is solvent, and both are mixed, and is made
The content of CNT is 0.2mg/ml；Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, ultrasound are carried out to mixture
30 DEG C～40 DEG C of temperature, forms the CNT electrophoresis liquid of mix homogeneously；
Step 5, metal titanium sheet has been had been coated with the one side of nano diamond coating as negative electrode, and stainless steel substrates are used as sun
Pole, two-plate spacing is 1cm, electrophoretic voltage 60V, electrophoresis time 8min, continues to deposit nanometer on nano diamond coating surface
Carbon pipe coating；
Step 6, by the metal titanium sheet that deposited nano diamond coating and nano-carbon tube coating Hot Filament Chemical Vapor is inserted
Heat treatment is carried out in depositing system, the vacuum of hot-wire chemical gas-phase deposition system is 3 × 10 during heat treatment-3Pa, temperature is 700
DEG C, process time is 10min, and chemical bonding is formed between substrate and nano-carbon material, obtains double-layer nanometer carbon coating field and sends out
Penetrate negative electrode.
The vacuum heat system that the present embodiment is adopted for hot-wire chemical gas-phase deposition system, i.e. HFCVD systems.
Fig. 1 is a kind of field-transmitting cathode with double-layer nanometer carbon coating obtained in the present embodiment, and described Flied emission is cloudy
Pole includes substrate, and deposition has nano diamond coating in substrate, and a stratification is defined between substrate and nano diamond coating
Bonded layer, deposition has nano-carbon tube coating on nano diamond coating.Send out field with double-layer nanometer carbon coating as above
Negative electrode is penetrated, described substrate is titanium substrate, and described chemical bonding layer is TiC chemical bonding layers.
As shown in figure 1, in the present embodiment substrate is Titanium；Chemical bonding layer is TiC, and substrate can be made to apply with material with carbon element
Layer strong bond, and the electric transmission path from substrate to material with carbon element is provided；Nano diamond coating can improve CNT with
The thermo-contact of substrate, while Nano diamond also can be used as field emission body；Nano-carbon tube coating is main field emission body.
Fig. 2 is the SEM image (amplifying 5000 times) of the titanium substrate used in the present embodiment, and Fig. 3 is in metal titanio
SEM image (amplifying 10000 times) after basal surface electrophoretic deposition Nano diamond.Contrast Fig. 2 and Fig. 3, it can be seen that in gold
Nano diamond in category titanium substrate surface-coated, because Nano diamond granule is very little, and easily reunites, so in figure
It is difficult to it was observed that single Nano diamond granule.Fig. 4 is on nano diamond coating after electrophoretic deposition CNT
SEM image (amplifies 10000 times), it can be seen that sample surfaces are applied and have been covered with CNT.Fig. 5 is sample through 700 DEG C of vacuum
XRD spectrum after heat treatment, occurs in that the diffraction maximum of TiC in figure.This declaratives Nano diamond reacts to be formed with substrate titanium
TiC, that is, define chemical bonding layer.
Properties of product are tested：
When testing the field emission characteristic of this embodiment, negative electrode (field-transmitting cathode) and anode (ITO electro-conductive glass) spacing
For 400 μm, vacuum is 10-4Pa magnitudes.Its Flied emission is can be seen that from the Flied emission J-E characteristic curves of embodiment open electricity
Field is 1.37V/ μm, and the emission under 2.625V/ μm of field intensity is 180 μ A/cm2(Fig. 6).The Flied emission F- of embodiment
N curves (Fig. 7) then confirm that its electron emission meets field-emission mechanics.
Field emission stability test is carried out to this embodiment of double-layer nanometer carbon coating field-transmitting cathode, test field intensity is
2.5V/ μm, as a result as shown in Figure 8.As can be seen that the embodiment has good field emission stability, during the test of 120min
Between internal field emission electric current rate of change for initial current 6.4%.
Claims (1)
1. a kind of preparation method of the field-transmitting cathode with double-layer nanometer carbon coating, it is characterised in that：Described Flied emission is cloudy
Pole includes substrate, and deposition has nano diamond coating in substrate, and a stratification is defined between substrate and nano diamond coating
Bonded layer, deposition has nano-carbon tube coating on nano diamond coating；
Chemical bonding layer can make substrate and material with carbon element coating strong bond, and provide the electric transmission road from substrate to material with carbon element
Footpath；Nano diamond coating can improve thermally contacting for CNT and substrate, while Nano diamond also can be used as field emission body；
Nano-carbon tube coating is main field emission body；
Described nano diamond coating is Nano diamond granule composition；
Nano diamond is coated in substrate by the method for electrophoretic deposition first, forms nano diamond coating；
Then CNT is coated on nano diamond coating by the method for electrophoretic deposition, forms nano-carbon tube coating；
Finally make substrate that chemical bonding reaction occur with nano diamond coating, obtain chemical bonding layer；
Described substrate is titanium substrate, and described chemical bonding layer is TiC chemical bonding layers；
The method specifically includes following steps：
Step one, selects metal titanium sheet as substrate, the one side of metal titanium sheet is ground, polish after be placed in acetone ultrasound clearly
Wash, Jing ethanol dehydrations after then deionized water is rinsed；
Step 2, configures Nano diamond electrophoresis liquid：It is Nano diamond from mass ratio：Iodine=1：2 mixture is solute；
It is deionized water from volume ratio：Acetone：Isopropanol=1：1：20 mixed liquor is solvent, makes the Nano diamond content be
0.23mg/ml；
Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, ultrasonic temperature 30 DEG C～40 will be carried out after solute and solvent mixing
DEG C, form the nano-diamond powder electrophoresis liquid of mix homogeneously；
Step 3, used as negative electrode, used as anode, two-plate spacing is 1cm to stainless steel substrates to the one side that metal titanium sheet is polished, electrophoresis
Voltage 60V, electrophoresis time 2min, in the one side of metal titanium sheet polishing nano diamond coating is deposited；
Step 4, configures CNT electrophoresis liquid：With CNT as solute, isopropanol is solvent, and both are mixed, and makes nanometer
The content of carbon pipe is 0.2mg/ml；Ultrasonic disperse, ultrasonic power 99W, ultrasonic time 30min, ultrasonic temperature are carried out to mixture
30 DEG C～40 DEG C, form the CNT electrophoresis liquid of mix homogeneously；
Step 5, sheet metal has been had been coated with the one side of nano diamond coating as negative electrode, and stainless steel substrates are used as anode, the two poles of the earth
Plate spacing is 1cm, electrophoretic voltage 60V, electrophoresis time 8min, continues to deposit CNT painting on nano diamond coating surface
Layer；
Step 6, the metal titanium sheet that deposited nano diamond coating and nano-carbon tube coating is inserted in vacuum heat system
Heat treatment is carried out, the vacuum of vacuum heat system is 3 × 10 during heat treatment-3Pa, temperature is 700 DEG C, and process time is
10min, forms chemical bonding between substrate and nano-carbon material, obtains double-layer nanometer carbon coating field-transmitting cathode.
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| KR100545354B1 (en) * | 2003-08-04 | 2006-01-24 | 일진다이아몬드(주) | Emitter composition using Diamond, manufacturing method and Field Emission cell comprising composition |
| JP2006045008A (en) * | 2004-08-05 | 2006-02-16 | Kobe Steel Ltd | Diamond film-carbon thread composite material and its manufacturing method |
| KR20060032402A (en) * | 2004-10-12 | 2006-04-17 | 삼성에스디아이 주식회사 | Carbon nanotube emitter and manufacturing method thereof and field emission device and manufacturing method thereof |
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