CN110491751A - Vertical Launch GaAs nano-wire array photocathode and preparation method - Google Patents

Vertical Launch GaAs nano-wire array photocathode and preparation method Download PDF

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CN110491751A
CN110491751A CN201910443189.4A CN201910443189A CN110491751A CN 110491751 A CN110491751 A CN 110491751A CN 201910443189 A CN201910443189 A CN 201910443189A CN 110491751 A CN110491751 A CN 110491751A
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gaas
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emission layer
nano
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刘磊
刁煜
夏斯浩
陆菲菲
田�健
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Nanjing Tech University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
    • H01J1/02—Main electrodes
    • H01J1/34—Photo-emissive cathodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • 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
    • H01J9/12—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes

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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The present invention provides a kind of Vertical Launch GaAs nano-wire array photocathodes, including p-type GaAs substrate layer, p-type varying doping GaAs nano-wire array emission layer, Cs/O active coating；Wherein p-type GaAs substrate layer is set to bottom, p-type varying doping GaAs nano-wire array emission layer includes the p-type varying doping GaAs nano wire with light trapping structure of several uniform thickness for being set to p-type GaAs substrate layer upper bottom surface, and Cs/O active coating is several and is respectively arranged at corresponding p-type varying doping GaAs nano wire upper bottom surface.

Description

Vertical Launch GaAs nano-wire array photocathode and preparation method
Technical field
The present invention relates to a kind of vacuum photoemissive material technology, especially a kind of Vertical Launch GaAs nano-wire array light Electric cathode and preparation method.
Background technique
Photocathode is a kind of photoemissive material based on external photoeffect, by inhaling on p-type semiconductor material surface Attached Cs/O2Or Cs/NF3Equal low-work-function materials realize negative electron affinity (NEA) (NEA), improve the quantum efficiency of cathode.As photoelectricity The most typical representative of cathode, NEAGaAs photocathode is high by quantum efficiency, secretly emits small, emitted electron energy and angle point The medium numerous excellent performances of cloth collection, in image intensifier, high-speed photography, semiconductor devices, superlattices function element and high energy object The fields such as reason have been widely used.
GaAs photocathode common at present is all based on GaAs epitaxial film, although having, monocrystalline is high-quality, surface is equal Even characteristic, but the surface reflectivity of thin-film material is larger, it is longer that the photoelectron excited in vivo is transported to emitting surface distance. Using existing nanotechnology, researcher has successfully been prepared for GaAs nanowire array structure photocathode, has Surface light trapping structure and the emitting surface of surrounding can efficiently solve the deficiencies of conventional films photoelectric cathode materials, reduce Reflectivity and photoelectron transport distance.But quantum efficiency the experimental results showed that, the quantum efficiency of GaAs nanowire photodiode cathode is still In reduced levels, main cause is most of photoelectron escaped from line side face by adjacent nano wire double absorption, is caused The problem of electronics collects difficulty, exposes electron transport directionality difference and launching electronics dispersion.
Summary of the invention
The purpose of the present invention is to provide a kind of Vertical Launch GaAs nano-wire array photocathodes, including p-type GaAs to serve as a contrast Bottom, p-type varying doping GaAs nano-wire array emission layer, Cs/O active coating；Wherein p-type GaAs substrate layer is set to bottom, P-type varying doping GaAs nano-wire array emission layer includes several uniform thickness for being set to p-type GaAs substrate layer upper bottom surface with sunken The p-type varying doping GaAs nano wire of photo structure, Cs/O active coating is several and is respectively arranged at corresponding p-type varying doping GaAs and receives Rice noodles upper bottom surface.
Using above-mentioned photocathode, each p-type varying doping GaAs nano wire is cylinder, by the subelement of n equal thickness Layer is constituted, wherein n >=2, and with a thickness of 3 μm~15 μm, the doping concentration positioned at the subelement layer on nano wire top is 1 × 1018cm-3, the doping concentration for being located at the subelement layer that nano wire bottom end is connected with p-type GaAs substrate layer (1) is 1 × 1019cm-3, doping Concentration is distributed in the way of reducing from the bottom end of nano wire to top constant gradient, doped chemical Zn.
Using above-mentioned photocathode, the diameter of p-type varying doping GaAs nano-wire array is 100nm~450nm, adjacent nano The spacing of line is 150nm~450nm.
The object of the invention is also to provide a kind of preparation method of Vertical Launch GaAs nano-wire array photocathode, packets Include following steps:
Step 1, on GaAs substrate surface, the p-type varying doping GaAs transmitting layered of equal thickness unit is successively grown Layer；
It step 2, will be using the SiO of improved Stober method synthesis2Nanosphere is equably covered on varying doping GaAs transmitting Layer surface forms single layer SiO2Nanosphere mask layer；
Step 3, by reactive ion etching to mask layer SiO2Nanosphere is pre-processed, and coupled plasma etch is utilized Technology performs etching varying doping GaAs emission layer, cleaning removal SiO2Nanosphere exposure mask, obtains proper alignment on substrate layer P-type varying doping GaAs nano-wire array emission layer；
Step 4, p-type varying doping GaAs nano-wire array emission layer is removed into surface grease by chemical cleaning, be re-fed into Ultra-high vacuum system carries out high temperature purification processing, and varying doping GaAs nano-wire array emission layer is made to reach atomically clean surfaces, Further using ultrahigh vacuum activation technology in varying doping GaAs nano-wire array emission layer adsorption Cs/O active coating, finally Prepare varying doping GaAs nano-wire array photocathode.
Using the above method, Metallo-Organic Chemical Vapor deposition is selected in the growth of p-type varying doping GaAs emission layer in step 1 Method, p-type doping element are Zn.
Using the above method, the p-type varying doping GaAs emission layer is made of the subelement layer of n equal thickness, wherein n >=2, for total emission layer with a thickness of 3 μm~15 μm, the doping thickness positioned at emission layer top terminals elementary layer is 1 × 1018cm-3, it is located at Emission layer bottom end be connected with substrate layer subelement layer doping concentration be 1 × 1019cm-3, doping concentration is according to from emission layer Bottom end be distributed to the mode that top constant gradient reduces.
It is the tetraethoxysilance of 1:10 and anhydrous that using the above method, in step 2, improved Stober method, which is by volume ratio, It is 1 that alcohol mixed solution 1, which is added by the volume ratio that concentrated ammonia liquor (concentration 25%~30%), dehydrated alcohol and deionized water combine: Magnetic agitation is carried out in the mixed solution 2 of 2:3, wherein the volume ratio of mixed solution 1 and solution 2 is 1:1, and mixing speed is set as 1000rpm~1200rpm reacts 1min~2min, then reducing mixing speed is 350rpm~400rpm, is reacted 2 hours at room temperature It can get the SiO of partial size about 300nm~400nm afterwards2Nanosphere；
With the SiO of above-mentioned synthesis2Nanosphere calculates secondary addition tetraethoxysilance as seed solution, according to formula (1) Content, then tetraethoxysilance and ethyl alcohol are mixed according to the ratio of 1:4 and slowly instill seed solution, react 1 hour again by body Ammonium hydroxide and the percentage of deionized water revert to former ratio in system, and the reaction was continued can be obtained the SiO of designated diameter for 1 hour2It receives Rice ball；
Wherein, d2Indicate specified SiO2The diameter of nanosphere, d1Indicate seed particle size, V1Indicate the positive silicic acid being initially added The volume of second rouge, V2It is the volume of the tetraethoxysilance of second of addition.
Using the above method, pass through reactive ion etching technology in step 3 to mask layer SiO2Nanosphere is pre-processed, Reduce SiO2The diameter of nanosphere extremely, increases the distance between nanosphere, specific technological parameter are as follows: nanometer bulb diameter is 350nm ~500nm, using CF4With O2Gas performs etching, and flow value is respectively 40 sccm, 10sccm, radio-frequency power 150W, chamber Pressure is 4Pa, and etch period is 100s~200s.
Using the above method, coupled plasma etch technology is utilized in step 3, to SiO2The varying doping of mask layer GaAs emission layer starts to perform etching, response parameter are as follows: uses Cl2With BCl3Gas performs etching, and flow value is respectively 6sccm, 14sccm, radio-frequency power 100W, chamber pressure 4Pa, etch period are 100s~200s.
Using the above method, the chemical cleaning in step 4 is molten using 40%HF solution and HCl:IPA=1:10 mixing Liquid cleans p-type varying doping GaAs nano-wire array emission layer；High temperature purification be by GaAs nano-wire array emission layer 600 DEG C~ 15~30min is heated under the conditions of 700 DEG C；Ultrahigh vacuum activation technology is the active mode continuous using the source Cs, the source O is interrupted, is surpassed The vacuum degree of high vacuum environment is not less than 10-9Pa。
Compared with prior art, the present invention having the advantage that the nanowire photodiode cathode in (1) present invention uses doping Concentration, to the GaAs material of nano wire top change of gradient from high to low, is drawn from substrate layer in the vertical direction along nano wire Enter built in field, most of photoelectron excited in vivo under the action of built in field by spread and directional drift in a manner of to It transports and escapes at the top of line, significantly reduce the transverse electric transmitting of array, obtain the Vertical Launch efficiency of photocathode Enhancing further improves the photoelectronic effective collection efficiency of evolution；(2) GaAs nano-wire array is fabricated to light in the present invention Electric cathode, nanowire array structure have the characteristics that photon capture effect, can fully absorb incident photon and to reduce surface anti- It penetrates, is conducive to the photoemission efficiency for improving photocathode.
The invention will be further described with reference to the accompanying drawings of the specification.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Fig. 2~Fig. 7 is manufacturing process schematic diagram of the invention.
Specific embodiment
Embodiment one
In conjunction with Fig. 1, a kind of Vertical Launch GaAs nano-wire array photocathode, the cathode is served as a contrast by p type GaAs from bottom to top Bottom 1, GaAs nano-wire array emission layer 2 and Cs/O active coating 4 composition of p-type varying doping.
Nano wire in the nano-wire array at periodical proper alignment on substrate layer, sunken light that emission layer has Structure is finally absorbed after a series of absorptions, reflection and refraction after making most of incident photon enter nano-wire array, Since GaAs nano-wire array emission layer uses the grade doping structure with built in field, most of photoelectron is in built in field Under the action of transported along nano wire vertical direction to nano wire top, finally enter vacuum from emission layer top-emission, make The Vertical Launch efficiency of GaAs nano-wire array photocathode is enhanced.
Embodiment two
In conjunction with Fig. 2 to Fig. 6, a kind of preparation method of Vertical Launch GaAs nano-wire array photocathode, including following step It is rapid:
Prepare dislocation density first and is lower than 103cm-3And doping concentration is 1019cm-3P-type GaAs material as GaAs serve as a contrast Bottom 1；As shown in figure 3, utilizing MOCVD epitaxy technology (Metalorganic Chemical Vapor Deposition) and GaAs P-type Doping skill Art grows the p-type varying doping GaAs emission layer 2 that overall thickness is 10 μm on substrate 1, by unit of n (n >=2) a equal thickness Layer composition, the doping thickness positioned at the subelement layer on emission layer top are 1 × 1018cm-3, it is located at emission layer bottom end and substrate layer The doping concentration for the subelement layer being connected is 1 × 1019cm-3, doping concentration is according to from the bottom end of emission layer to top constant gradient Reduced mode is distributed, and all epitaxial layer foreign atoms are Zn；
The SiO for being 500nm using improved Stober method synthesis diameter2Nanosphere, concrete operations are the 4.5mL that will be configured Tetraethoxysilance and 45.5mL dehydrated alcohol mixed solution be added by 8.3mL concentrated ammonia liquor (28%), 16.7mL dehydrated alcohol and Magnetic agitation is carried out in the solution of 25mL deionized water mixing, and 1min is first reacted for 1000rpm~1200rpm with mixing speed, Reducing mixing speed again is 350rpm~400rpm, can get the SiO of diameter about 350nm after reacting 2 hours at room temperature2Nanosphere Seed solution, then to take the mixed solution of 8ml tetraethoxysilance and the dehydrated alcohol of 32ml slowly to instill in seed solution reaction 1 small When, continue to instill 4ml ammonium hydroxide and 10ml deionized water mixed liquor reacts the SiO that can be obtained that diameter is 500nm for 1 hour2Nanometer Ball；As shown in figure 4, the SiO for being synthesized preparation with sol evenning machine2Nanosphere is equably covered on varying doping GaAs emission layer 2, first Turn 10s with revolving speed 600rpm, then forms single layer SiO in transmitting layer surface after turning 4s with 1900rpm2Nanosphere mask layer 3；
As shown in figure 5, by reactive ion etching technology to mask layer SiO2Nanosphere is pre-processed, reaction chamber Pressure is 4Pa, and radio-frequency power supply power is 150W, and is passed through the CF that flow is respectively 40sccm, 10 sccm4And O2Gas, etching 150s, to reduce SiO2The diameter of nanosphere increases the distance between nanosphere；As shown in fig. 6, utilizing coupled plasma etch skill Art, to SiO2The varying doping GaAs emission layer 2 of mask layer starts to perform etching, and the pressure of reaction chamber is 4Pa, radio frequency Power supply is 100W, and is passed through the Cl that flow is respectively 6sccm, 14sccm2And BCl3Gas etches 150s, prepares and SiO2It receives The rice consistent array structure of ball mask diameter；As shown in fig. 7, SiO is contained at top2The varying doping GaAs of nanosphere mask layer receives Nanowire arrays emission layer is immersed in BOE solution (HF and NH3F mixed solution) in, 10min is impregnated, removal is adsorbed on a nanometer linear array The SiO in list face2Nanosphere, to prepare the p-type varying doping GaAs nano-wire array emission layer 2 of proper alignment；
P-type varying doping GaAs nano-wire array emission layer 4 is first cleaned into 5min with 40%HF solution, then uses HCl:IPA= 1:10 mixed solution cleans 5min, to remove the oxide and grease on photocathode surface, is re-fed into vacuum degree not less than 10-8Pa Ultra-high vacuum system in carry out high temperature purification processing, heating temperature be 700 DEG C, the time continues 20min, makes varying doping GaAs Nano-wire array emission layer 4 obtains atomically clean surfaces, finally uses in varying doping GaAs nano-wire array transmitting layer surface The ultrahigh vacuum activation technology that the source Cs is continuous, the source O is interrupted adsorbs Cs/O active coating 4, prepares varying doping as shown in Figure 1 GaAs nano-wire array photocathode.

Claims (10)

1. a kind of Vertical Launch GaAs nano-wire array photocathode, which is characterized in that including p-type GaAs substrate layer (1), p-type Varying doping GaAs nano-wire array emission layer (2), Cs/O active coating (4)；Wherein
P-type GaAs substrate layer (1) is set to bottom,
P-type varying doping GaAs nano-wire array emission layer (2) include it is several be set to p-type GaAs substrate layer (1) upper bottom surface etc. The thick p-type varying doping GaAs nano wire with light trapping structure,
Spacing between p-type varying doping GaAs nano wire is equal,
Cs/O active coating (4) is several and is respectively arranged at corresponding p-type varying doping GaAs nano wire upper bottom surface.
2. photocathode according to claim 1, which is characterized in that each p-type varying doping GaAs nano wire is cylinder, It is made of the subelement layer of n equal thickness, wherein n >=2, the subelement layer with a thickness of 3 μm~15 μm, positioned at nano wire top Doping concentration is 1 × 1018cm-3, it is dense to be located at the doping of subelement layer that nano wire bottom end is connected with p-type GaAs substrate layer (1) Degree is 1 × 1019cm-3, doping concentration by from the bottom end of nano wire to top constant gradient reduce in the way of be distributed, doped chemical For Zn.
3. photocathode according to claim 1, which is characterized in that the diameter of p-type varying doping GaAs nano-wire array is 100nm~450nm, the spacing of adjacent nanowires are 150nm~450nm.
4. a kind of method for preparing photocathode described in claim 1, which comprises the following steps:
Step 1, on GaAs substrate surface, equal thickness unit p-type varying doping GaAs emission layer layered is successively grown；
It step 2, will be using the SiO of improved Stober method synthesis2Nanosphere is equably covered on varying doping GaAs transmitting layer surface Form single layer SiO2Nanosphere mask layer；
Step 3, by reactive ion etching to mask layer SiO2Nanosphere is pre-processed, and coupled plasma etch technology is utilized Varying doping GaAs emission layer is performed etching, cleaning removal SiO2Nanosphere exposure mask obtains the p-type of proper alignment on substrate layer Varying doping GaAs nano-wire array emission layer；
Step 4, p-type varying doping GaAs nano-wire array emission layer is removed into surface grease by chemical cleaning, is re-fed into superelevation Vacuum system carries out high temperature purification processing, so that varying doping GaAs nano-wire array emission layer is reached atomically clean surfaces, into one Step is using ultrahigh vacuum activation technology in varying doping GaAs nano-wire array emission layer adsorption Cs/O active coating, final preparation Obtain varying doping GaAs nano-wire array photocathode.
5. according to the method described in claim 4, it is characterized in that, in step 1 p-type varying doping GaAs emission layer growth select Metalorganic Chemical Vapor Deposition, p-type doping element are Zn.
6. according to the method described in claim 4, it is characterized in that, the p-type varying doping GaAs emission layer is by n equal thickness Subelement layer constitute, wherein n >=2, total emission layer is with a thickness of 3 μm~15 μm, positioned at the doping of emission layer top terminals elementary layer With a thickness of 1 × 1018cm-3, the doping concentration for the subelement layer that is connected positioned at emission layer bottom end with substrate layer is 1 × 1019cm-3, mix Miscellaneous concentration is distributed in the way of reducing from the bottom end of emission layer to top constant gradient.
7. according to the method described in claim 4, it is characterized in that, it is 1 that improved Stober method, which is by volume ratio, in step 2: 10 tetraethoxysilance and dehydrated alcohol mixed solution 1 be added by concentrated ammonia liquor (concentration 25%~30%), dehydrated alcohol and go from Magnetic agitation is carried out in the mixed solution 2 that the volume ratio of sub- water combination is 1:2:3, wherein the volume ratio of mixed solution 1 and solution 2 For 1:1, mixing speed is set as 1000rpm~1200rpm reaction 1min~2min, then reduce mixing speed be 350rpm~ 400rpm can get the SiO of partial size about 300nm~400nm after reacting 2 hours at room temperature2Nanosphere；
With the SiO of above-mentioned synthesis2Nanosphere calculates containing for secondary addition tetraethoxysilance as seed solution, according to formula (1) Amount, then tetraethoxysilance and ethyl alcohol are mixed according to the ratio of 1:4 and slowly instill seed solution, reaction 1 hour again will be in system Ammonium hydroxide and the percentage of deionized water revert to former ratio, and the reaction was continued can be obtained the SiO of designated diameter for 1 hour2Nanosphere；
Wherein, d2Indicate specified SiO2The diameter of nanosphere, d1Indicate seed particle size, V1Indicate the tetraethoxysilance being initially added Volume, V2It is the volume of the tetraethoxysilance of second of addition.
8. according to the method described in claim 4, it is characterized in that, by reactive ion etching technology to mask layer in step 3 SiO2Nanosphere is pre-processed, and SiO is reduced2The diameter of nanosphere increases the distance between nanosphere, specific technological parameter are as follows: Nanometer bulb diameter is 350nm~500nm, and the distance between nanosphere is 150nm~450nm, using CF4With O2Gas performs etching, Flow value is respectively 40sccm, 10sccm, and radio-frequency power 150W, chamber pressure 4Pa, etch period is 100s~200s.
9. according to the method described in claim 4, it is characterized in that, coupled plasma etch technology is utilized in step 3, to having SiO2The varying doping GaAs emission layer of mask layer starts to perform etching, response parameter are as follows: uses Cl2With BCl3Gas is carved Erosion, flow value are respectively 6sccm, 14sccm, radio-frequency power 100W, chamber pressure 4Pa, etch period be 100s~ 200s。
10. according to the method described in claim 4, it is characterized in that, the chemical cleaning in step 4 be using 40%HF solution and HCl:IPA=1:10 mixed solution cleans p-type varying doping GaAs nano-wire array emission layer；High temperature purification is by GaAs nano wire Array emitter layer heats 15~30min under the conditions of 600 DEG C~700 DEG C；Ultrahigh vacuum activation technology is continuous, O using the source Cs The vacuum degree of the interrupted active mode in source, ultra-high vacuum environment is not less than 10-9Pa。
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Application publication date: 20191122