CN107818900A - A kind of NEA GaAs nano-cone arrays photocathode and preparation method - Google Patents
A kind of NEA GaAs nano-cone arrays photocathode and preparation method Download PDFInfo
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- CN107818900A CN107818900A CN201710975198.9A CN201710975198A CN107818900A CN 107818900 A CN107818900 A CN 107818900A CN 201710975198 A CN201710975198 A CN 201710975198A CN 107818900 A CN107818900 A CN 107818900A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- H01J1/02—Main electrodes
- H01J1/34—Photo-emissive cathodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- H01J9/00—Apparatus 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
- H01J9/02—Manufacture of electrodes or electrode systems
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Abstract
The invention discloses a kind of NEA GaAs nano-cone arrays photocathode and preparation method, the GaAs nano-cone arrays photocathode includes substrate layer and the nano-cone array emission layer positioned at substrate layer surface, the substrate is the insulation films such as Si or SiC, nano-cone array emission layer is made up of some p-type GaAs nanocones, and carries out Cs/O activation to the nano-cone array of growth.The effective refractive index of nano-cone array proposed by the present invention is gradual change, efficiently reduce due to air/GaAs cell interface refractive indexes it is discontinuous caused by light reflect, while GaAs photocathode quantum efficiencies are improved, influence of the incident angle of light for absorptivity is reduced.
Description
Technical field
The invention belongs to opto-electronics, and in particular to a kind of NEA-GaAs nano-cone arrays photocathode and preparation side
Method.
Background technology
Photocathode is a kind of photoemissive material that electric signal is converted light signals into using external photoeffect.GaAs makees
It is good with solar spectrum matching degree for direct band-gap semicondictor material, it is a kind of preferable photoelectric cathode materials.Negatron is affine
Gesture, i.e. cathode surface vacuum level are less than conduction band bottom energy level so that the escape probability of photo-excited electron greatly increases, therefore has
Quantum efficiency is high, dark current is small, emitted electron energy distribution collects medium particular advantages.
In general GaAs photocathodes are made of thin-film material, and thin-film material has growth technique ripe, into film quality
The advantages that having measured, but the emissivity of thin-film material is big, it is impossible to fully absorb the energy of incident light.Either reflection, the absorption of light
Or solar spectrum response, for thin film solar cell, the design of light trapping structure is all very important, especially in the moon
Under the development trend of very thin membranization, light trapping structure just seems more important, in addition for photocathode, the electronics of material
Transport distance is to the absorption depth of the thickness requirement and material of material to light to conflicting between the thickness requirement of material.
Nanocone is a kind of and the quite similar light trapping structure of nano wire.This pyramidal structure is by moth eye cornea
A kind of biomimetic features that periodic array of protrusions is inspired and prepared.The effective refractive index of nanocone structures is gradual change, can be with
Regard a kind of uniform dielectric from air to negative electrode with graded index as, effectively reduce due to air/GaAs negative electrodes circle
The discontinuous caused light reflection of face refractive index.The nanocone of identical size is compared with nano wire, and short circuit current will be higher by 10%,
And as the incident angle of incident light is converted into 90 ° from 0 °, the overall absorptivity of nanocone structures has almost no change, because
This is more outstanding compared to nano wire, the sunken light characteristic of nanocone.
Growth nano-cone array mainly has direct growth method, electrochemical erosion method, template etc. at present.Wherein, it is directly raw
Regular way uses microwave plasma body technique direct growth nanocone structures, and this nano-cone array has uniformity (orientation, cone angle
And distribution) it is poor, major diameter is smaller and top radius of curvature is larger the shortcomings of；Centrum draw ratio prepared by electrochemical erosion method is too
Small, top radius of curvature is too big, and preparation technology is complicated, and launch stability is poor, and sensitivity is low, and application prospect is little；Template
Be by substrate anisotropic etch go out inverted pyramid template, be subsequently filled emissive layer materials, template is fallen in final etching
Method.The centrum draw ratio and top radius of curvature of this structure are all undesirable, and preparation technology is complicated.Existing making nanocone
Technique there is make it is complicated, be difficult to that large area is realized, application is narrow and the defects of uniformity and poor controllability.Therefore
We need to find a kind of suitable nanocone growing method for preparing GaAs nano-cone array photocathodes.
The content of the invention
It is an object of the invention to provide a kind of NEA-GaAs nano-cone arrays photocathode and preparation method.
The technical scheme for realizing the object of the invention is：A kind of NEA-GaAs nano-cone arrays photocathode, including substrate layer
And the nano-cone array emission layer positioned at substrate layer surface；
The nano-cone array emission layer is made up of some p-type GaAs nanocones, and p-type GaAs nanometer poppet surfaces are adsorbed with
Cs/O active coatings.
A kind of method for preparing above-mentioned NEA-GaAs nano-cone arrays photocathode, step are as follows：
Step 1, substrate is cleaned, and backing material is sequentially cleaned using acetone, ethanol and deionized water；
Step 2, Ga drops are prepared on substrate surface after cleaning, preparation temperature is 600 DEG C -700 DEG C, and self-catalysis is given birth to
Long nano-pillar, self-catalysis temperature are 400 DEG C -600 DEG C；Temperature is reduced to 400 DEG C afterwards, solidifies Ga drops and grows to be formed
GaAs films；
Step 3, it is passed through hydrogen plasma and pre-etching is carried out to sample surfaces；Etching condition is as follows：It is passed through hydrogen, gas pressure
Power is 8Torr, and sample heating temperature is 800 DEG C -900 DEG C, is biased as 400V, bias current 100mA, time 25min；
Step 4, bias in CVD equipment is turned off, heater current is turned off, and vacuumizes 10 again-2Torr；
Step 5, carry out plasma etching and form surface nano tip array, the gaseous mixture of methane and hydrogen is passed through during etching
Body, the volume ratio of mixed gas is 5:100；When carrying out plasma etching using the mixed gas of hydrogen and argon gas, mixture
Product is than being 30:50.Sample heating temperature biases 400V, bias current 120mA, time 2 at 800 DEG C -950 DEG C, pressure 20Torr
Hour；
Step 6, with the grease and impurity of Chemical cleaning reagent etching away p-type GaAs nanometer poppet surfaces, ultravacuum is used
Activation technology is in p-type GaAs nano-cone array adsorption Cs/O active coatings.
Compared with prior art, its remarkable advantage is the present invention：
(1) GaAs nano-cone arrays of the invention are fabricated to photocathode, can pass through the transmitting between nanocone and folding
The energy for fully absorbing incident light is penetrated, overcomes the contradictory relation of photonic absorption depth and electron diffusion length；
(2) compared with nano-wire array, due to the unique structure of nanocone, no matter light is incident with which type of angle,
The photon of entrance can reflect and reflect between nanocone, finally thoroughly be absorbed by nano-cone array, form " photon capture " effect
Should, the loss of energy is reduced to minimum, so as to greatly improve the quantum efficiency of photocathode；
(3) surface nano tip array proposed by the present invention, there is high length-diameter ratio, small top radius of curvature, and has
Controllable draw ratio, cone angle and array density；
(4) preparation method of GaAs nano-cone arrays photocathode provided by the invention, is existed using ultravacuum activation technology
The adsorption of nanocone Cs/O active coatings so that photoelectron escape probability greatly increases, improve the quantum of photocathode
Efficiency, and the manufacture craft of nano-cone array is simple, workable, reduces the production cost of photocathode；
(5) when photon is absorbed inside nanocone, photoelectrons are excited, because the surrounding of nanocone is surface,
Therefore photoelectron escapes from the inside of nanocone to surrounding, the number of runaway electron is drastically increased, so as to increase photoelectricity
Stream, improve the quantum efficiency of photocathode.
Brief description of the drawings
Fig. 1 is GaAs nano-cone arrays photocathode schematic diagram of the present invention.
Fig. 2 (a), Fig. 2 (b), Fig. 2 (c) are the fabrication processings of the nano-cone array of the present invention, and wherein Fig. 2 (a) is lining
Bottom is placed on the schematic diagram in stainless steel circle support, and Fig. 2 (b) is that Pt fine metal mesh grid schematic diagrames are placed on substrate, and Fig. 2 (c) is etc.
Gas ions perform etching schematic diagram to GaAs.
In figure, 1- incident rays；2-GaAs nano-cone arrays；3- substrates；4-GaAs layers；5- stainless steel pallets；6-Pt is thin
Metallic mesh；7- plasma slabs.
Embodiment
With reference to Fig. 1, a kind of NEA-GaAs nano-cone arrays photocathode, including substrate layer 3 and positioned at substrate layer surface
Nano-cone array emission layer 2；
The nano-cone array emission layer 2 is made up of some p-type GaAs nanocones, and p-type GaAs nanometer poppet surfaces adsorb
There are Cs/O active coatings.
The substrate layer is Si or SiC insulation films, the p-type GaAs nanocones using plasma lithographic technique,
The array structure of nanocone is etched on the GaAs emission layers of substrate layer surface.
The draw ratio of nanocone is 50-5000, and sophisticated radius of curvature is in below 5nm, base diameter 200nm-
2000nm, cone angle are 20 ° -70 °, density 109cm-2-105cm-2.P-type doping concentration is 1 × 1019cm-3, doped chemical is
Zn。
The present invention also provides a kind of method for preparing NEA-GaAs nano-cone array photocathodes, and step is as follows：
Step 1, substrate is cleaned, and backing material is sequentially cleaned using acetone, ethanol and deionized water；
Step 2, Ga drops are prepared on substrate surface after cleaning, preparation temperature is 600 DEG C -700 DEG C, and self-catalysis is given birth to
Long nano-pillar, self-catalysis temperature are 400 DEG C -600 DEG C；Temperature is reduced to 400 DEG C afterwards, solidifies Ga drops and grows to be formed
GaAs films；
Step 3, it is passed through hydrogen plasma and pre-etching is carried out to sample surfaces；Etching condition is as follows：It is passed through hydrogen, gas pressure
Power is 8Torr, and sample heating temperature is 800 DEG C -900 DEG C, is biased as 400V, bias current 100mA, time 25min；
Step 4, bias in CVD equipment is turned off, heater current is turned off, and vacuumizes 10 again-2Torr；
Step 5, carry out plasma etching and form surface nano tip array, the gaseous mixture of methane and hydrogen is passed through during etching
Body, the volume ratio of mixed gas is 5:100；When carrying out plasma etching using the mixed gas of hydrogen and argon gas, mixture
Product is than being 30:50.Sample heating temperature biases 400V, bias current 120mA, time 2 at 800 DEG C -950 DEG C, pressure 20Torr
Hour；
Step 6, with the grease and impurity of Chemical cleaning reagent etching away p-type GaAs nanometer poppet surfaces, Chemical cleaning examination
Agent is that volume ratio is 2:2:1 sulfuric acid, hydrogen peroxide and deionized water mixed liquor；It is sent into high-temperature vacuum system and heat only
Change, heating-up temperature is 850 DEG C, the GaAs nanocones emission layer of p-type is obtained atomically clean surfaces；Work is activated using ultravacuum
Skill is in p-type GaAs nano-cone array adsorption Cs/O active coatings.
In step 2, Ga (CH3)3For gallium source, AsH3As As sources, ZnCl2For doped chemical Zn sources, with mole ratio
1000:1000：Reaction source is used as after 1 ratio mixing, reaction source is located at close to CVD reacting furnaces air inlet and apart from substrate 15cm
Position, substrate is located at the center heating location of CVD reacting furnaces；CVD reacting furnaces are first vacuumized before heating and are passed through argon purge
Boiler tube；To 850 DEG C, reaction source position heating-up temperature to 600 DEG C, deposition reaction time is substrate position heating-up temperature
100~120min.
When carrying out Surface Hydrogen ion etching, Pt metallic filaments grid mesh is placed on to the surface of GaAs layers, discharged using segmentation
Method enhancing for poorly conductive and the etching effect of the larger thin-film material of area, a diameter of the 0.2 of the metal grid mesh
Millimeter.
With reference to embodiment and accompanying drawing, the present invention is described in detail.
Embodiment
With reference to Fig. 2 (a), Fig. 2 (b), Fig. 2 (c), in the method for Si substrate surfaces growth GaAs films：
First have to Si substrates carrying out cleaning treatment, choose Si (111) substrate, ultrasonic cleaning two is carried out to it using acetone
It is secondary, each 4-6min, afterwards using EtOH Sonicate cleaning twice, each 4-6min, then cleaned twice with deionized water, use nitrogen
Dry up and be put into vacuum chamber.
Ga drops are prepared on Si (111) substrate after cleaning, preparation temperature is 630 DEG C, and Ga lines are 2 × 10-7Torr,
Growth time is 30min.Self-catalysis grows 1 μm of nano-pillar on Si (111) substrate, and self-catalysis temperature is 550 DEG C, Ga lines
For 1.5 × 10-7Torr, As line are 2 × 10-6Torr, growth time 15min.Cooling the temperature to 400 DEG C solidifies Ga drops,
Ga lines are 1.5 × 10-7Torr, As line are 2 × 10-6Torr, growth time 90min, growth form GaAs films 4.
The preparation method of GaAs nanocones：
The sample grown is placed in stainless steel circle support 5, is put into CVD equipment, is passed through hydrogen plasma to sample table
Face carries out pre-etching.Etching condition is as follows：High-purity hydrogen, gas pressure 8Torr are passed through, sample heating temperature is 850 DEG C, partially
Press as 400V, bias current 100mA, time 25min；Then bias in CVD equipment is turned off, heater current is turned off, and takes out again
Vacuum 10-2Torr；The mixed gas of methane and hydrogen is passed through, the volume ratio of mixed gas is 5:100；Using hydrogen and argon gas
When mixed gas carries out plasma etching, mixed volume ratio is 30:50.Sample heating temperature is 900 DEG C, and pressure is
20Torr, 400V, bias current 120mA are biased, the time is 2 hours；
When Surface Hydrogen ion etching 7 is carried out, Pt metallic filaments grid mesh 6 is placed on to the surface of sample, using segmentation
The method enhancing of electric discharge for poorly conductive and the etching effect of the larger thin-film material of area, the metal grid mesh it is a diameter of
0.2 millimeter.
Finally remove the grease and impurity of nanometer poppet surface by chemical attack, the reagent volume ratio of Chemical cleaning is 2:2:
1 sulfuric acid, hydrogen peroxide and deionized water.It is re-fed into high-temperature vacuum system and carries out heating purification, heating-up temperature is 850 DEG C, makes p
The GaAs nanocones emission layer of type obtains atomically clean surfaces；Send out p-type GaAs nanocones by ultravacuum activation technology again
Layer surface absorption Cs/O active coatings are penetrated, the process of Cs, O activation continues for Cs, and O sources are interrupted, and transmitting layer surface reaches negatron parent
And gesture, GaAs nano-cone array photocathodes as shown in Figure 1 are finally made.
Claims (9)
1. a kind of NEA-GaAs nano-cone arrays photocathode, it is characterised in that including substrate layer and positioned at substrate layer surface
Nano-cone array emission layer；
The nano-cone array emission layer is made up of some p-type GaAs nanocones, and p-type GaAs nanometer poppet surfaces are adsorbed with Cs/O
Active coating.
2. NEA-GaAs nano-cone arrays photocathode according to claim 1, it is characterised in that the substrate layer is Si
Or SiC insulation films.
3. NEA-GaAs nano-cone arrays photocathode according to claim 1 or 2, it is characterised in that the p-type GaAs
Nanocone using plasma lithographic technique, the array structure of nanocone is etched on the GaAs emission layers of substrate layer surface.
4. NEA-GaAs nano-cone arrays photocathode according to claim 1, it is characterised in that the draw ratio of nanocone
For 50-5000, sophisticated radius of curvature is 20 ° -70 ° in below 5nm, base diameter 200nm-2000nm, cone angle, and density is
109cm-2-105cm-2。
5. the GaAs nano-cone array photocathodes according to claim 1 or 4, it is characterised in that p-type doping concentration is 1
×1019cm-3, doped chemical Zn.
A kind of 6. method for preparing NEA-GaAs nano-cone arrays photocathode described in claim 1, it is characterised in that step is such as
Under：
Step 1, substrate is cleaned, and backing material is sequentially cleaned using acetone, ethanol and deionized water；
Step 2, Ga drops are prepared on substrate surface after cleaning, preparation temperature is 600 DEG C -700 DEG C, and self-catalysis growth is received
Meter Zhu, self-catalysis temperature are 400 DEG C -600 DEG C；Temperature is reduced to 400 DEG C afterwards, solidifies Ga drops and grows to form GaAs
Film；
Step 3, it is passed through hydrogen plasma and pre-etching is carried out to sample surfaces；Etching condition is as follows：Hydrogen is passed through, gas pressure is
8Torr, sample heating temperature are 800 DEG C -900 DEG C, are biased as 400V, bias current 100mA, time 25min；
Step 4, bias in CVD equipment is turned off, heater current is turned off, and vacuumizes 10 again-2Torr；
Step 5, carry out plasma etching and form surface nano tip array, the mixed gas of methane and hydrogen is passed through during etching,
The volume ratio of mixed gas is 5:100；When carrying out plasma etching using the mixed gas of hydrogen and argon gas, mixed volume ratio
For 30:50.Sample heating temperature biases 400V, bias current 120mA at 800 DEG C -950 DEG C, pressure 20Torr, and the time is 2 small
When；
Step 6, with the grease and impurity of Chemical cleaning reagent etching away p-type GaAs nanometer poppet surfaces, activated using ultravacuum
Technique is in p-type GaAs nano-cone array adsorption Cs/O active coatings.
7. the preparation method of NEA-GaAs nano-cone arrays photocathode according to claim 6, it is characterised in that step 2
In, Ga (CH3)3For gallium source, AsH3As As sources, ZnCl2For doped chemical Zn sources, with mole ratio 1000:1000：1 ratio
Reaction source is used as after mixing, reaction source is located at close to CVD reacting furnaces air inlet and is located at apart from substrate 15cm position, substrate
The center heating location of CVD reacting furnaces；CVD reacting furnaces are first vacuumized before heating and are passed through argon purge boiler tube；Substrate institute is in place
Heating-up temperature is put to 850 DEG C, for reaction source position heating-up temperature to 600 DEG C, the deposition reaction time is 100~120min.
8. the preparation method of NEA-GaAs nano-cone arrays photocathode according to claim 6, it is characterised in that carrying out
During Surface Hydrogen ion etching, Pt metallic filaments grid mesh is placed on to the surface of GaAs layers, a diameter of 0.2 milli of the metal grid mesh
Rice.
9. the preparation method of NEA-GaAs nano-cone arrays photocathode according to claim 6, it is characterised in that chemistry is clear
It is that volume ratio is 2 to wash reagent:2:1 sulfuric acid, hydrogen peroxide and deionized water mixed liquor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766857A (en) * | 2018-05-07 | 2018-11-06 | 东华理工大学 | A kind of GaAs nanocomposite opticals resonant structure photocathode electron source and preparation method thereof |
| CN110491751A (en) * | 2019-05-27 | 2019-11-22 | 南京理工大学 | Vertical Launch GaAs nano-wire array photocathode and preparation method |
| CN114927394A (en) * | 2022-04-26 | 2022-08-19 | 电子科技大学 | GaN photocathode with modified nanometer pyramid structure and preparation method thereof |
| CN116916722A (en) * | 2023-08-25 | 2023-10-20 | 华南理工大学 | GaAs surface micro-nano structure, preparation method thereof and heterojunction solar cell |
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| CN103594302A (en) * | 2013-11-19 | 2014-02-19 | 东华理工大学 | GaAs nanowire array photocathode and manufacturing method thereof |
| CN104112632A (en) * | 2014-07-23 | 2014-10-22 | 四川天微电子有限责任公司 | GaAs photoelectric cathode activating process beneficial for reduction of activation time |
| TW201701501A (en) * | 2015-05-21 | 2017-01-01 | 克萊譚克公司 | Photocathode including field emitter array on a silicon substrate with boron layer |
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| CN103594302A (en) * | 2013-11-19 | 2014-02-19 | 东华理工大学 | GaAs nanowire array photocathode and manufacturing method thereof |
| CN104112632A (en) * | 2014-07-23 | 2014-10-22 | 四川天微电子有限责任公司 | GaAs photoelectric cathode activating process beneficial for reduction of activation time |
| TW201701501A (en) * | 2015-05-21 | 2017-01-01 | 克萊譚克公司 | Photocathode including field emitter array on a silicon substrate with boron layer |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766857A (en) * | 2018-05-07 | 2018-11-06 | 东华理工大学 | A kind of GaAs nanocomposite opticals resonant structure photocathode electron source and preparation method thereof |
| CN110491751A (en) * | 2019-05-27 | 2019-11-22 | 南京理工大学 | Vertical Launch GaAs nano-wire array photocathode and preparation method |
| CN114927394A (en) * | 2022-04-26 | 2022-08-19 | 电子科技大学 | GaN photocathode with modified nanometer pyramid structure and preparation method thereof |
| CN116916722A (en) * | 2023-08-25 | 2023-10-20 | 华南理工大学 | GaAs surface micro-nano structure, preparation method thereof and heterojunction solar cell |
| CN116916722B (en) * | 2023-08-25 | 2024-03-15 | 华南理工大学 | GaAs surface micro-nano structure, preparation method thereof and heterojunction solar cell |
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