CN109830413A - GaN micron bar array/graphene field emission cathode composite material and preparation method thereof - Google Patents
GaN micron bar array/graphene field emission cathode composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereofs, specific step is as follows: step 1, to silicon substrate plating platinum film, then making annealing treatment the silicon substrate of plated platinum film, room temperature is naturally cooled to after annealing, obtains substrate A；Step 2, the substrate A that step 1 obtains is heat-treated together with reaction source, certain distance is kept between substrate A and reaction source, naturally cools to room temperature after the reaction was completed, obtain substrate B；Step 3, the substrate B that step 2 obtains is heat-treated, is naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphene field emission cathode composite material.There is excellent field emission characteristic by GaN micron bar array/graphene field emission cathode composite material that this method is prepared.
Description
Technical field
The invention belongs to composite material and preparation method thereof technical fields, and in particular to a kind of GaN micron bar array/graphene field
Emitting cathode composite material and preparation method thereof.
Background technique
Flied emission is also known as cold cathode emission or from electron emission, is body surface under forceful electric power field action, launches electronics
The phenomenon that, it is to constrain surface potential barrier with external strong electrical field, reduces potential barrier highest point, and barrier width is made to narrow, either
So that electronics is entered dielectric layer from base with internal strong electrical field, and accelerate in the dielectric layer to obtain large energy, to cause
Interior of articles electronics is not required to the phenomenon that obtaining additional energy, that is, not needing by exciting electronics that can escape.Along with vacuum
Microelectronics has become an important subject in the continuous development for showing application field, field emission display (FED) technology.
The key of FED research is filed emission cathode material preparation, and filed emission cathode material decides therefore service life and the quality of FED is drawn
The upsurge of the preparation of research filed emission cathode material and field emission characteristic is played.
Field emission electron source material is that field emission flat panel display develops one of the problem that faces, obtain have high stability and
The cold cathode of long-life is an urgent demand of Field Emission Display functionization.Have to the basic demand of practical application cathode material:
Work function is small, field enhancement factor is big, be easy to open and it is reliable and stable, material is economical and practical, easy to process.Reported type is numerous
In more filed emission cathode materials, GaN micron bar is attracting vast researcher competitively to study.With conventional high-temperature infusibility gold
Symbolic animal of the birth year ratio, GaN micron bar are received great attention due to excellent field emission characteristic.Compared with block GaN, GaN micron bar array
Performance it is more superior, be mainly shown as more big L/D ratio and higher stability.GaN micron bar has high-melting-point, highly thermally conductive
It is the advantages that rate, high-breakdown-voltage, small electron affinity, increasingly extensive in Flied emission application aspect, however there are high current transmittings
Difficult problem, and the performances such as current flow uniformity and stability are still to be improved.Influence GaN micron bar field emission characteristic because being known as very
It is more, including pattern, doping, cladding etc..It, can be by itself and other in order to improve the field emission characteristic of GaN micron bar array
Material cladding is desirably to obtain excellent field emission characteristic.In past few years, researchers are in order to effectively utilize GaN micron bar
Unique performance is answered it with various functional form nano materials (such as other semiconductors, metal, metal oxide)
It closes.With the continuous development that these are studied, currently used for preparing the common method of GaN base composite material, according to preparation route and
Material composition can be divided into Metalorganic Chemical Vapor Deposition, hydride transports vapor phase epitaxial growth, laser ablation method, oxidation
Object assisting growth method, sol-gel method and chemical vapour deposition technique (CVD) etc..CVD method is a kind of easy to operate and low in cost
Synthesizing mean, be suitble to large batch of materials synthesis.By being passed through gas reaction source, while presoma is heated, wherein precursor
It can be solid powder, liquid or gaseous state, make itself and gas source that sufficiently reaction, then at a certain temperature, gas phase point occur
After son reaches cohesion critical dimension, medium well is not long for nucleation, to obtain monodimension nanometer material.Under normal circumstances, it is only necessary to full
The certain experiment condition of foot, various crystalline materials can form one-dimensional nano structure.By using different gallium sources, nitrogen source, gas
The good regulation to GaN base composite material in size and shape may be implemented in flow, reaction time and temperature.
As a kind of typical semiconductor material with wide forbidden band, the success of GaN micron bar array and graphene is compound to drop
The work function of low GaN, and be conducive to accelerate electronics transfer, improve its Flied emission electric current and field emission stability.
Summary of the invention
The object of the present invention is to provide a kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof,
Have excellent Flied emission special by GaN micron bar array/graphene field emission cathode composite material that this method is prepared
Property.
The technical scheme adopted by the invention is that: GaN micron bar array/graphene field emission cathode composite material preparation side
Method, the specific steps are as follows:
Step 1, to silicon substrate plating platinum film, then the silicon substrate of plated platinum film is made annealing treatment, annealing terminates
After naturally cool to room temperature, obtain substrate A；
Step 2, the substrate A that step 1 obtains is heat-treated together with reaction source, is kept between substrate A and reaction source
Certain distance naturally cools to room temperature after the reaction was completed, obtains substrate B；
Step 3, the substrate B that step 2 obtains is heat-treated, it is micro- to get GaN is naturally cooling to room temperature after the reaction was completed
Rice stick array/graphene field emission cathode composite material.
It is a feature of the present invention that
Concrete operations in step 1, to silicon substrate plating platinum film are as follows: JFC-1600 type ion sputtering film coating instrument is used,
Vacuum degree is 8 × 10-3In the case where Pa, setting sputtering current is 40-60mA, sputtering time 40-80s, to silicon substrate platinum plating
Film.
In step 1, process that the silicon substrate of plated platinum film is annealed specifically: serving as a contrast the silicon of plated platinum film
Bottom is put into quartz boat, and plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, and setting annealing temperature is 800-1200
DEG C, ammonia flow 50-200sccm, annealing time is 5-30min, and 20min nitrogen is first led to before furnace body heating to remove boiler tube
In air, be then warming up to 800-1200 DEG C with 10 DEG C of heating rate per minute and made annealing treatment.
Heat treatment process in step 2 specifically: the substrate A for obtaining step 1 is moved into quartz boat, with ammonia and oxidation
Gallium is placed in quartz boat as nitrogen source and gallium source, then by reaction source, and substrate A is made to be placed on the quartz boat apart from reaction source 1-3cm
Downstream at, after the quartz boat for filling substrate A and reaction source is put into the quartz ampoule of controlling temperature with region tube furnace, being passed through flow is
The nitrogen 30min air-discharging of 200-400sccm, then rises to 900-1250 DEG C with the heating rate of 5-20 DEG C/min, then leads to
Inbound traffics are the argon gas 10min of 100-300sccm, close argon gas, are passed through the ammonia that flow is 100-400sccm again later and keep
10-30min。
Reaction source described in step 2 is carbon dust and gallium oxide, and wherein the mass ratio of carbon dust and gallium oxide is 1:1-3.
Heat treatment process in step 3 specifically: the substrate B that step 2 obtains is put into quartz boat, then sets quartz boat
In in the quartz ampoule of temperature control tube furnace, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 200-400sccm, is connect
Reaction temperature risen to 950-1250 DEG C with the heating rate of 5-20 DEG C/min, being then first passed through flow is 50-150sccm
After argon gas 5-20min, then it is passed through the methane that flow is 4-20sccm and keeps 5-25min.
The beneficial effects of the present invention are:
The present invention using gallium oxide is gallium source, ammonia is nitrogen source, methane for carbon source, with CVD method under specific process conditions,
Two steps prepare GaN micron bar array/graphene composite material；
GaN micron bar array/graphene composite material of the method for the present invention preparation has excellent field emission characteristic；
GaN micron bar array/graphene composite material of the method for the present invention preparation also has good field emission stability；
Preparation process of the present invention is simple, and experimental facilities is simple, at low cost, profitable, it is easy to accomplish commercialization.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image of Pt nanoparticle on a silicon substrate after annealing in the present invention；
Fig. 2 is the scanning electron microscope image of GaN micron bar array in the present invention；
Fig. 3 is GaN micron bar array/graphene composite material formation mechenism image that the method for the present invention is prepared.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The present invention provides a kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereofs, specific to walk
It is rapid as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is 40-60mA, sputtering time 40-80s, and to silicon substrate plating platinum film, the silicon substrate for sputtering platinum film is put into stone
Ying Zhouzhong, plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, setting annealing
Temperature is 800-1200 DEG C, ammonia flow 50-200sccm, and annealing time is 5-30min, first leads to 20min nitrogen before furnace body heating
Then gas is warming up to 800-1200 DEG C with 10 DEG C of heating rate per minute and carries out at annealing to remove the air in boiler tube
Reason, naturally cools to room temperature after annealing.Obtain substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:1-3, after by substrate A place under the quartz boat of carbon dust and gallium oxide 1-3cm
Trip.Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min that flow is 200-400sccm and empties
Gas, it is ensured that be oxygen-free environment in pipe.Then 900-1250 DEG C of reaction temperature is risen to the heating rate of 5-20 DEG C/min, then first
It is passed through the argon gas 10min that flow is 100-300sccm, closes argon gas, then being passed through flow is that 100-400sccm ammonia keeps 10-
30min.It is naturally cooling to room temperature after the reaction was completed, obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 200-400sccm, it is ensured that be oxygen-free environment in pipe.It connects
Rise to 950-1250 DEG C of reaction temperature with the heating rate of 5-20 DEG C/min, be then first passed through flow be 50-150sccm argon
After gas 5-20min, then be passed through flow be 4-20sccm methane keep 5-25min be naturally cooling to after the reaction was completed room temperature to get
GaN micron bar array/graphene field emission cathode composite material.
Fig. 1 is the scanning electron microscope image of the Pt nanoparticle that is prepared using the method for the present invention on a silicon substrate, from Fig. 1
It can be seen that Pt nanoparticle is uniformly distributed on a silicon substrate, and spherical shape is presented in Pt nanoparticle, and the diameter of Pt nanoparticle is about
50-100nm, this provides good support for growth GaN micron bar array.
Fig. 2 is the SEM image for the GaN micron bar array being prepared using the method for the present invention, it can be found that GaN micron bar
It is vertically arranged on substrate, about 1 micron of diameter of micron side, about several microns of length, this is compound for growth graphene above it
Material provides support well.
Fig. 3 is GaN micron bar array/graphene composite material formation mechenism figure, and the first step on silicon substrate first to sputtering
Platinum film forms Pt nanoparticle after the second step annealing, and third step is with Pt nanoparticle catalytic growth GaN micron bar, the 4th step
In GaN micron bar synthesizing graphite alkene, GaN micron bar array/graphene composite material is formed.
Embodiment 1
A kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, the specific steps are as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is that 40mA, sputtering time 40s are put into the silicon substrate for sputtering platinum film in quartz boat silicon substrate plating platinum film,
Plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, and setting annealing temperature is
800 DEG C, ammonia flow 50sccm, annealing time is 5min, and 20min nitrogen is first led to before furnace body heating to remove in boiler tube
Then air is warming up to 800 DEG C with 10 DEG C of heating rate per minute and is made annealing treatment, room is naturally cooled to after annealing
Temperature obtains substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:1, after substrate A placed into quartz boat downstream apart from carbon dust and gallium oxide 1cm.It will
Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min air-discharging that flow is 200sccm, it is ensured that pipe
Interior is oxygen-free environment.Then 900 DEG C of reaction temperature are risen to the heating rate of 5 DEG C/min, being then first passed through flow is 100sccm
Argon gas 10min, close argon gas, then be passed through flow be 100sccm ammonia keep 10min.It is naturally cooling to room after the reaction was completed
Temperature obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 200sccm, it is ensured that be oxygen-free environment in pipe.Then with 5
DEG C/heating rate of min rises to 950 DEG C of reaction temperature, after being then first passed through the argon gas 5min that flow is 50sccm, then it is passed through stream
Amount is that 4sccm methane keeps 5min to be naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphene Flied emission
Cathode composite.
Embodiment 2
A kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, the specific steps are as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is that 60mA, sputtering time 80s are put into the silicon substrate for sputtering platinum film in quartz boat silicon substrate plating platinum film,
Plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, and setting annealing temperature is
1200 DEG C, ammonia flow 200sccm, annealing time is 30min, and 20min nitrogen is first led to before furnace body heating to remove boiler tube
In air, be then warming up to 1200 DEG C with 10 DEG C of heating rate per minute and made annealing treatment, it is naturally cold after annealing
But room temperature is arrived.Obtain substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:3, after substrate A placed into quartz boat downstream apart from carbon dust and gallium oxide 3cm.It will
Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min air-discharging that flow is 400sccm, it is ensured that pipe
Interior is oxygen-free environment.Then 1250 DEG C of reaction temperature are risen to the heating rate of 20 DEG C/min, being then first passed through flow is
The argon gas 10min of 300sccm closes argon gas, then being passed through flow is that 400sccm ammonia keeps 30min.It drops naturally after the reaction was completed
It warms to room temperature, obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 400sccm, it is ensured that be oxygen-free environment in pipe.Then with
The heating rate of 20 DEG C/min rises to 1250 DEG C of reaction temperature, after being then first passed through the argon gas 20min that flow is 150sccm, then
Being passed through flow is that 20sccm methane keeps 25min to be naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphite
Alkene field-transmitting cathode composite material.
Embodiment 3
A kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, the specific steps are as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is that 50mA, sputtering time 50s are put into the silicon substrate for sputtering platinum film in quartz boat silicon substrate plating platinum film,
Plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, and setting annealing temperature is
1000 DEG C, ammonia flow 100sccm, annealing time is 20min, and 20min nitrogen is first led to before furnace body heating to remove boiler tube
In air, be then warming up to 900 DEG C with 10 DEG C of heating rate per minute and made annealing treatment, natural cooling after annealing
To room temperature.Obtain substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:2, after substrate A placed into quartz boat downstream apart from carbon dust and gallium oxide 2cm.It will
Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min air-discharging that flow is 300sccm, it is ensured that pipe
Interior is oxygen-free environment.Then 1000 DEG C of reaction temperature are risen to the heating rate of 15 DEG C/min, being then first passed through flow is
The argon gas 10min of 200sccm closes argon gas, then being passed through flow is that 300sccm ammonia keeps 20min.It drops naturally after the reaction was completed
It warms to room temperature, obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 300sccm, it is ensured that be oxygen-free environment in pipe.Then with
The heating rate of 15 DEG C/min rises to 1000 DEG C of reaction temperature, after being then first passed through the argon gas 15min that flow is 100sccm, then
Being passed through flow is that 15sccm methane keeps 20min to be naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphite
Alkene field-transmitting cathode composite material.
Embodiment 4
A kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, the specific steps are as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is that 60mA, sputtering time 70s are put into the silicon substrate for sputtering platinum film in quartz boat silicon substrate plating platinum film,
Plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, and setting annealing temperature is
1200 DEG C, ammonia flow 100sccm, annealing time is 5min, and 20min nitrogen is first led to before furnace body heating to remove in boiler tube
Air, be then warming up to 800 DEG C with 10 DEG C of heating rate per minute and made annealing treatment, naturally cooled to after annealing
Room temperature.Obtain substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:3, after substrate A placed into quartz boat downstream apart from carbon dust and gallium oxide 1cm.It will
Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min air-discharging that flow is 400sccm, it is ensured that pipe
Interior is oxygen-free environment.Then 1250 DEG C of reaction temperature are risen to the heating rate of 10 DEG C/min, being then first passed through flow is
The argon gas 10min of 100sccm closes argon gas, then being passed through flow is that 200sccm ammonia keeps 10min.It drops naturally after the reaction was completed
It warms to room temperature, obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 250sccm, it is ensured that be oxygen-free environment in pipe.Then with
The heating rate of 5-20 DEG C/min rises to 950 DEG C of reaction temperature, after being then first passed through the argon gas 5min that flow is 50sccm, then leads to
Inbound traffics are that 20sccm methane keeps 25min to be naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphene
Field-transmitting cathode composite material.
Embodiment 5
A kind of GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, the specific steps are as follows:
It step 1, is 8 × 10 in vacuum degree using JFC-1600 type ion sputtering film coating instrument-3In the case of Pa, setting sputtering
Electric current is that 50mA, sputtering time 60s are put into the silicon substrate for sputtering platinum film in quartz boat silicon substrate plating platinum film,
Plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, is made annealing treatment to silicon substrate, and setting annealing temperature is
800 DEG C, ammonia flow 100sccm, annealing time is 15min, and 20min nitrogen is first led to before furnace body heating to remove in boiler tube
Air, be then warming up to 800 DEG C with 10 DEG C of heating rate per minute and made annealing treatment, naturally cooled to after annealing
Room temperature.Obtain substrate A；
Step 2, substrate A step 1 obtained is moved into quartz boat, using ammonia and gallium oxide as nitrogen source and gallium source, first
Carbon dust and gallium oxide are placed in quartz boat by 1:2, after substrate A placed into quartz boat downstream apart from carbon dust and gallium oxide 2cm.It will
Quartz boat is put into the quartz ampoule of controlling temperature with region tube furnace, is passed through the nitrogen 30min air-discharging that flow is 400sccm, it is ensured that pipe
Interior is oxygen-free environment.Then 900 DEG C of reaction temperature are risen to the heating rate of 20 DEG C/min, being then first passed through flow is
The argon gas 10min of 300sccm closes argon gas, then being passed through flow is that 400sccm ammonia keeps 10min.It drops naturally after the reaction was completed
It warms to room temperature, obtains substrate B at this time；
Step 3, the substrate B that step 2 obtains is put into quartz boat, then quartz boat is placed in the quartz ampoule of temperature control tube furnace
It is interior, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 400sccm, it is ensured that be oxygen-free environment in pipe.Then with 5
DEG C/heating rate of min rises to 950 DEG C of reaction temperature, after being then first passed through the argon gas 5min that flow is 50sccm, then it is passed through stream
Amount is that 20sccm methane keeps 25min to be naturally cooling to room temperature after the reaction was completed to get GaN micron bar array/graphene field hair
Penetrate cathode composite.
Claims (6)
1.GaN micron bar array/graphene field emission cathode composite material and preparation method thereof, which is characterized in that specific step is as follows:
Step 1, to silicon substrate plating platinum film, then the silicon substrate of plated platinum film is made annealing treatment, after annealing certainly
It so is cooled to room temperature, obtains substrate A；
Step 2, the substrate A that step 1 obtains is heat-treated together with reaction source, keeps certain between substrate A and reaction source
Distance naturally cools to room temperature after the reaction was completed, obtains substrate B；
Step 3, the substrate B that step 2 obtains is heat-treated, is naturally cooling to room temperature after the reaction was completed to get GaN micron bar
Array/graphene field emission cathode composite material.
2. GaN micron bar array/graphene field emission cathode composite material and preparation method thereof according to claim 1, special
Sign is, the concrete operations in step 1, to silicon substrate plating platinum film are as follows: JFC-1600 type ion sputtering film coating instrument is used, true
Reciprocal of duty cycle is 8 × 10-3In the case where Pa, setting sputtering current be 40-60mA, sputtering time 40-80s, it is thin to silicon substrate platinum plating
Film.
3. GaN micron bar array/graphene field emission cathode composite material and preparation method thereof according to claim 1, special
Sign is, in step 1, process that the silicon substrate of plated platinum film is annealed specifically: serving as a contrast the silicon of plated platinum film
Bottom is put into quartz boat, and plated film is face-up, and quartz boat is then pushed into tube furnace flat-temperature zone, and setting annealing temperature is 800-1200
DEG C, ammonia flow 50-200sccm, annealing time is 5-30min, and 20min nitrogen is first led to before furnace body heating to remove boiler tube
In air, be then warming up to 800-1200 DEG C with 10 DEG C of heating rate per minute and made annealing treatment.
4. GaN micron bar array/graphene field emission cathode composite material and preparation method thereof according to claim 1, special
Sign is, the heat treatment process in step 2 specifically: the substrate A for obtaining step 1 is moved into quartz boat, with ammonia and oxidation
Gallium is placed in quartz boat as nitrogen source and gallium source, then by reaction source, and substrate A is made to be placed on the quartz boat apart from reaction source 1-3cm
Downstream at, after the quartz boat for filling substrate A and reaction source is put into the quartz ampoule of controlling temperature with region tube furnace, being passed through flow is
The nitrogen 30min air-discharging of 200-400sccm, then rises to 900-1250 DEG C with the heating rate of 5-20 DEG C/min, then leads to
Inbound traffics are the argon gas 10min of 100-300sccm, close argon gas, are passed through the ammonia that flow is 100-400sccm again later and keep
10-30min。
5. GaN micron bar array/graphene field emission cathode composite material and preparation method thereof according to claim 1, special
Sign is that reaction source described in step 2 is carbon dust and gallium oxide, and wherein the mass ratio of carbon dust and gallium oxide is 1:1-3.
6. GaN micron bar array/graphene field emission cathode composite material and preparation method thereof according to claim 1, special
Sign is, the heat treatment process in step 3 specifically: the substrate B that step 2 obtains is put into quartz boat, then sets quartz boat
In in the quartz ampoule of temperature control tube furnace, using methane as carbon source, it is passed through the nitrogen 30min air-discharging that flow is 200-400sccm, is connect
Reaction temperature risen to 950-1250 DEG C with the heating rate of 5-20 DEG C/min, being then first passed through flow is 50-150sccm
After argon gas 5-20min, then it is passed through the methane that flow is 4-20sccm and keeps 5-25min.
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| CN115108580A (en) * | 2022-05-11 | 2022-09-27 | 中国科学院长春光学精密机械与物理研究所 | Gallium oxide micron line preparation method, solar blind ultraviolet detector and preparation method thereof |
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| CN115108580A (en) * | 2022-05-11 | 2022-09-27 | 中国科学院长春光学精密机械与物理研究所 | Gallium oxide micron line preparation method, solar blind ultraviolet detector and preparation method thereof |
| CN115108580B (en) * | 2022-05-11 | 2024-03-05 | 中国科学院长春光学精密机械与物理研究所 | Gallium oxide micron line preparation method, solar blind ultraviolet detector and preparation method thereof |
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