CN105428183A - Reflective NEA GaN nanowire array photoelectric negative electrode and manufacturing method therefor - Google Patents
Reflective NEA GaN nanowire array photoelectric negative electrode and manufacturing method therefor Download PDFInfo
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Abstract
The invention proposes a reflective NEA GaN nanowire array photoelectric negative electrode and a manufacturing method therefor. The reflective NEA GaN nanowire array photoelectric negative electrode is obtained by growing p-type GaN nanowires on the surface of an Si or SiC substrate and performing Cs/O activation on a grown nanowire array. The reflective NEA GaN nanowire array photoelectric negative electrode comprises a substrate layer and a nanowire array emission layer positioned on the surface of the substrate layer, wherein the nanowire array emission layer consists of a plurality of p-type GaN nanowires; Cs/O activation layers are adsorbed on the surfaces of the p-type GaN nanowires; and the substrate layer is Si or SiC. According to the reflective NEA GaN nanowire array photoelectric negative electrode, the photoelectron transmission distance can be reduced while the material emission rate is reduced; and photons are fully absorbed by controlling the diameters of the nanowires, so that the quantum efficiency of the GaN photoelectric negative electrode is improved.
Description
Technical field
The invention belongs to photoemissive material technical field, be specifically related to a kind of reflective NEAGaN nano-wire array photocathode and preparation method.
Background technology
Photocathode is a kind of photoemissive material utilizing external photoelectric effect light signal to be changed into the signal of telecommunication.There is the GaN photocathode of negative electron affinity, namely cathode surface vacuum level is lower than energy level at the bottom of conduction band, therefore in body, photo-excited electron only need run to surface, just be transmitted into vacuum by tunnelling, the potential barrier overcoming material surface is gone without the need to superfluous kinetic energy, the escape probability of photo-excited electron is increased greatly, therefore there is the particular advantages such as quantum efficiency is high, dark current is little, emitted electron energy distribution is concentrated.Its quantum efficiency is generally greater than 24%, is much higher than the quantum efficiency of traditional ultraviolet light photo negative electrode, and GaN material response, at below 400nm, is typical " day is blind " material, has good capability of resistance to radiation.
Current growing nano linear array mainly contains metal-organic chemical vapor deposition equipment method (MOCVD), dry lithography etc., and these growing methods all exist some inevitable shortcomings.Metal-organic chemical vapor deposition equipment method is due to its apparatus expensive, and reaction raw material are metallorganic the shortcoming such as not easily to preserve, and therefore repeatability is not high; And although dry lithography equipment is simple, cost is lower, easy realization, but because its reaction mechanism finally forms nano-wire array by corrosion resistant semiconductor material, therefore the lattice breakage of nanowire surface is comparatively serious, the surface formed is more coarse, and the diameter of nano wire does not reach the order of magnitude of nanowire photodiode cathode emission layer in addition, and therefore we need the nanowire growth method finding a kind of applicable preparation GaN nano wire array photoelectric negative electrode.
General GaN photocathode all adopts thin-film material to make, thin-film material has growth technique maturation, the advantages such as quality of forming film is good, but the emissivity of thin-film material is large, fully can not absorb the energy of incident light, in addition for reflective photocathode, the transport distance of the electronics of material to the thickness requirement of material and material to the absorption degree of depth of light to conflicting between the thickness requirement of material.
Summary of the invention
The object of the invention is to propose a kind of reflective NEAGaN nano-wire array photocathode and preparation method, can while reduction material emissivity, reduce photoelectronic transport distance, control the abundant absorb photons of diameter of nano wire, improve GaN photocathode quantum efficiency.
In order to solve the problems of the technologies described above, the invention provides a kind of reflective NEAGaN nano-wire array photocathode, comprising substrate layer, be positioned at the nano-wire array emission layer on substrate layer surface; Nano-wire array emission layer is made up of some p-type GaN nano wire, and p-type GaN nano wire surface is all adsorbed with Cs/O active coating.
Preferably, described substrate layer is Si or SiC; The diameter of described p-type GaN nano wire is 10 ~ 100nm, and length is 1 ~ 100 μm, and p-type doping content is 1 × 1019cm-3, and doped chemical is Zn.
The present invention also proposes a kind of method in substrate surface growth p-type GaN nano wire, and step is as follows:
Step 101, on substrate evaporated metal Al formed metal Al layer, the described substrate with metal Al layer is placed in oxalic acid solution and carries out electrochemical corrosion, thus substrate surface formed porous alumina membrane;
Step 102, the mixed liquor that described surface has the substrate of mesh structural porous aluminum oxide film to put into phosphoric acid and chromic acid to be soaked, to remove on aluminum oxide film bottom hole with the aluminium oxide of substrate contact, the mesh structural porous anodic aluminum oxide film of formation rule size;
Step 103, at described mesh structural porous anodic aluminum oxide film surface evaporation layer of metal Ni, then substrate is put into NaOH aqueous slkali and soak, remove the anodic aluminum oxide film of substrate surface, thus on substrate, form W metal nano particle dot matrix;
Step 104, substrate and reaction source are put into the quartz boat partition heating of CVD reacting furnace, after the temperature of substrate and reaction source region all reaches design temperature, ammonia and argon gas is passed into CVD reacting furnace, then the insulation of CVD reacting furnace carries out deposition reaction to 550 DEG C, and the p-type GaN nano wire array of Ni catalyst granules is arranged at obtained top.
Preferably, described substrate layer is Si or SiC; On substrate before evaporated metal Al, being first sulfuric acid and the hydrogen peroxide cleaning substrate of 1:1 by volume ratio, is then the hydrofluoric acid corrosion cleaning substrate of 5% with mass percent; Use electron beam evaporation methods evaporated metal Al on substrate to form Al layer in step 1, described Al layer thickness is 100 ~ 1000nm; Step 1 mesoxalic acid solution concentration is 0.5mol/L.
Preferably, in step 102, in described phosphoric acid and chromic acid mixture, phosphoric acid quality percentage is 4%, and chromic acid mass percent is 2%.
Preferably, use electron beam evaporation methods evaporation metal Ni layer in step 103, the thickness of W metal layer is 5 ~ 100nm; Described substrate put into mass percent be 5% NaOH aqueous slkali soak.
Preferably, in step 104, GaCl3 is gallium source, ZnCl2 is doped chemical Zn source, as reaction source after the mixing of the ratio of mole ratio 1000:1, reaction source is positioned near CVD reacting furnace air inlet and the position of distance substrate about 10cm, and substrate is positioned at the center heating location of CVD reacting furnace; First vacuumize CVD reacting furnace before heating and pass into argon purge boiler tube; Substrate position heating-up temperature to 850 DEG C, reaction source position heating-up temperature to 600 DEG C; Described argon flow amount is 200ml/min, ammonia flow be 30ml/min; The deposition reaction time is 100 ~ 120min.
The present invention also proposes a kind of method preparing reflective NEAGaN nano-wire array photocathode, is the Ni catalyst granules of the hydrochloric acid of 4%, the mixed acid solution removing p-type GaN nano wire array top of phosphoric acid and hydrofluoric acid with mass percent; Send in high-temperature vacuum system after cleaning and carry out adding thermal purification, make p-type GaN nano wire array obtain the surface of Atomically clean; Then in p-type GaN nano wire array surface absorption Cs/O active coating.
Preferably, with grease and the impurity on chemical cleaning reagent etching away p-type GaN nano wire surface, the sulfuric acid of chemical cleaning reagent to be volume ratio be 2:2:1, hydrogen peroxide and deionized water mixed liquor; Hot temperature degree in high-temperature vacuum system is 850 DEG C; Use ultravacuum activation technology in p-type GaN nano wire array surface absorption Cs/O active coating.
The present invention compared with prior art, its remarkable advantage is, GaN nano wire array is made into photocathode, fully can be absorbed the energy of incident light, and overcome the contradictory relation of the photonic absorption degree of depth and electron diffusion length by the transmitting between nano wire and refraction; When light incides nano-wire array with suitable angle, due to the structure of nano wire uniqueness, the photon entered can reflect and reflect between nano wire, finally thoroughly absorbed by nano-wire array, form " photon is caught " effect, the loss of energy is reduced to minimum, thus greatly improves the quantum efficiency of photocathode.In addition, when photon is when nano wire inside is by absorption, photoelectron is inspired, surrounding due to nano wire is surface, and therefore photoelectron is overflowed from the inside of nano wire to surrounding, drastically increases the number of runaway electron, thus increase photoelectric current, improve the quantum efficiency of photocathode.GaN nano wire array, due to the photoelectric characteristic of self excellence, becomes the NEAGaN photoelectric cathode materials of a new generation based on nanometer technology, has positive effect to expansion GaN photocathode application.
Accompanying drawing explanation
Fig. 1 is reflective NEAGaN nano-wire array photocathode schematic diagram of the present invention.
Fig. 2 is use anodic oxidation aluminium formwork method to generate on substrate in the present invention schematic flow sheet that proper alignment has the nano-wire array emission layer of nano-wire array.
CVD method is used to grow p-type GaN nano wire array schematic diagram in Fig. 3 the present invention.
Embodiment
Easy understand, according to technical scheme of the present invention, when not changing connotation of the present invention, one of ordinary skill in the art can imagine the numerous embodiments the present invention's reflective NEAGaN nano-wire array photocathode and preparation method.Therefore, following embodiment and accompanying drawing are only the exemplary illustrations to technical scheme of the present invention, and should not be considered as of the present invention all or the restriction be considered as technical solution of the present invention or restriction.
Reflective NEAGaN nano-wire array photocathode of the present invention is the superficial growth p-type GaN nano wire 5 at Si or SiC substrate 1, and to growth nano-wire array carry out Cs/O activate obtain, it comprises substrate layer, is positioned at the nano-wire array emission layer on substrate layer surface; Nano-wire array emission layer is made up of some p-type GaN nano wire 5, and p-type GaN nano wire surface is all adsorbed with Cs/O active coating 10; Described substrate layer is Si or SiC.The diameter of p-type GaN nano wire is 10 ~ 100nm, and length is 1 ~ 100 μm, and p-type doping content is 1 × 1019cm-3, and doped chemical is Zn.
In the method for substrate surface growth p-type GaN nano wire be:
Step 101, be first the sulfuric acid of 1:1 and hydrogen peroxide cleaning Si or SiC substrate by volume ratio, then clean substrate with the hydrofluoric acid corrosion that mass percent is 5%;
Step 102, use electron beam evaporation methods evaporated metal Al on substrate form Al layer, and described Al layer thickness is 100 ~ 1000nm;
Step 103, step 2 is evaporated the oxalic acid solution having the substrate of metal A l to be placed in 0.5mol/L carry out electrochemical corrosion, thus form porous alumina membrane at substrate surface;
Step 104, top layer after step 3 electrochemical corrosion had the substrate of pellumina put into mass percent be 4% phosphoric acid and mass percent be 2% chromic acid mixture soak, to remove on aluminum oxide film bottom hole with the aluminium oxide of substrate contact and change the size in hole, with the mesh structural porous anodic aluminum oxide film of formation rule size;
Step 105, use electron beam evaporation methods are in the mesh structural porous anodic aluminum oxide film surface evaporation layer of metal Ni again that step 4 is formed, and the thickness of W metal is 5 ~ 100nm;
Step 106, the substrate that step 5 is formed put into mass percent be 5% NaOH aqueous slkali soak, remove the anodic aluminum oxide film of substrate surface, thus on substrate, obtain W metal nano particle dot matrix;
Step 107, substrate step 6 obtained are put into quartz boat and are placed in the center heating location of CVD reacting furnace;
Step 108, be gallium source by GaCl3, ZnCl2 is doped chemical Zn source, quartz boat is put into as reaction source after the mixing of the ratio of mole ratio 1000:1, reaction source is positioned at the position near CVD reacting furnace air inlet distance substrate about 10cm, substrate is positioned at the center heating location of reacting furnace, then vacuumizes CVD reacting furnace and passes into argon purge boiler tube;
Step 109, the furnace temperature of each warm area of control CVD reacting furnace, first add hot CVD reacting furnace central substrate position temperature to 850 DEG C, and then heat reaction source position temperature to 600 DEG C, ammonia and argon gas is passed into CVD reacting furnace after the temperature of above-mentioned two warm areas rises to design temperature, the flow of argon gas is 200ml/min, the flow of ammonia be 30ml/min, the insulation of CVD reacting furnace carries out deposition reaction to 550 DEG C, sedimentation time is 100 ~ 120min, room temperature is cooled to the furnace after deposition, the GaN nano wire array that obtained top has the P type of Ni catalyst granules to adulterate.
Using the method that the p-type GaN nano wire array of above-mentioned growth on substrate is made into reflective NEAGaN nano-wire array photocathode further as nano-wire array emission layer be:
Step 201, be the Ni particle at the hydrochloric acid of 4%, the mixed acid solution removing p-type GaN nano wire top of phosphoric acid and hydrofluoric acid with mass percent;
Step 11, with the grease on chemical cleaning reagent etching away p-type GaN nano wire surface and impurity, the sulfuric acid of chemical cleaning reagent to be volume ratio be 2:2:1, hydrogen peroxide and deionized water mixed liquor; Then sent in high-temperature vacuum system by p-type GaN nano wire array and carry out adding thermal purification, heating-up temperature is 850 DEG C, makes p-type GaN nano wire array obtain the surface of Atomically clean;
Step 12, use ultravacuum activation technology are in p-type GaN nano wire array surface absorption Cs/O active coating, and now emission layer surface reaches negative electron affinity, final obtained reflective NEAGaN nano-wire array photocathode.
Reflection type GaN nano-wire array photocathode of the present invention solves the problem conflicting to material emission layer thickness requirement of photonic absorption and electron transport in thin-film material, thus can while reduction material emissivity, reduce photoelectronic transport distance, control the abundant absorb photons of diameter of nano wire, achieve the imagination improving GaN photocathode quantum efficiency; The present invention uses anodic oxidation aluminium formwork legal system to be used as CVD growth for nanoscale Ni catalyst granules, and have preparation method simple, favorable repeatability, cost is low, and the advantage such as catalyst particle size is controlled, marshalling; The present invention is when using CVD method to prepare p-type GaN nano wire, and compared with MOCVD method, the reaction source of use is GaCl3, ZnCl2, ammonia and argon gas, has the cheap and advantage that growth course is controlled of raw material; The present invention uses CVD method to prepare P type GaN nano wire array, compared with existing dry etching technology, there is GaN nano wire blemish less, the advantage that size is more small, and length and diameter, than larger, can promote the quantum efficiency of nanowire photodiode negative electrode preferably; The present invention uses GaN nano wire material activation to become reflective negative electron affinity GaN nano wire photocathode, activate successfully and can adsorb one deck Cs/O active coating around nano wire, produce negative electron affinity, thus it is high to form a centre in nano wire, the band structure that surrounding is low, the photoelectron that this band structure is very beneficial for exciting in nano wire transports toward surface and is transmitted in vacuum.
Embodiment
Method at substrate surface absorption proper alignment nanoscale Ni catalyst granules:
First, be the sulfuric acid of 1:1 and hydrogen peroxide cleaning Si or SiC substrate 1 by volume ratio, then be hydrofluoric acid corrosion cleaning cleaning Si or the SiC substrate of 5% with mass percent, the method of electron beam evaporation plating evaporated metal Al layer on substrate layer is utilized to form Al film 2 at clean substrate surface, as shown in (a) in Fig. 2, the thickness of Al film 2 is 100 ~ 1000nm; Carrying out electrochemical corrosion by evaporating the oxalic acid solution having the substrate of Al film 2 to be placed in 0.5mol/L, forming porous alumina membrane at substrate surface; Top layer after electrochemical corrosion is had the substrate of pellumina put into mass percent be 4% phosphoric acid and mass percent be 2% chromic acid mixture soak, to remove bottom aperture with the aluminium oxide of substrate contact and change the size in hole, with the mesh structural porous anodic aluminum oxide film 3 of formation rule size, as shown in (b) in Fig. 2; Utilize the method evaporation layer of metal Ni layer 4 again of electron beam evaporation plating on mesh structural porous anodic aluminum oxide film 3 surface formed, as shown in (c) in Fig. 2, the thickness belonging to Ni layer 4 is 5 ~ 100nm; Then the backing material of formation is put into mass concentration be 5% NaOH aqueous slkali soak, remove the anodised aluminium of substrate surface, substrate obtain W metal nano particle dot matrix, as shown in (d) in Fig. 2.
The method of further growth p-type GaN nano wire array is:
Composition graphs 3, has the substrate of proper alignment nanometer Ni catalyst particles to put into quartz boat on the surface obtained and is placed in the center heating location of CVD reacting furnace, take GaCl3 as gallium source, ZnCl2 is doped chemical Zn source, quartz boat is put into as reaction source 8 after the mixing of the ratio of mole ratio 1000:1, the quartz boat being placed with reaction source is positioned near the position of air outlet apart from substrate 10 ~ 15cm, substrate is positioned at the center heating location of reacting furnace, vacuumizes and pass into argon gas 7 to clean boiler tube, control the furnace temperature of each warm area, first heating reaction furnace central substrate position rises to 850 DEG C, heat reaction source position again and rise to 600 DEG C, ammonia 6 and argon gas 7 is passed into after the temperature of above-mentioned two warm areas rises to design temperature, the flow of argon gas is 200ml/min, the flow of ammonia be 30ml/min, insulation carries out deposition reaction to 550 DEG C, sedimentation time is 100 ~ 120min, stop after deposition passing into carrier gas, substrate cools to room temperature with the furnace, the GaN nano wire array that obtained described top has the P type of Ni catalyst granules to adulterate on substrate, as shown in (e) in Fig. 2, with the Ni particle that mass percent is the hydrochloric acid of 3%, the mixed acid solution removing nano wire top of phosphoric acid and hydrofluoric acid, obtain the P type GaN nano wire array of proper alignment, as shown in (f) in Fig. 2.
The method of further preparation reflective NEAGaN nano-wire array photocathode is:
Remove grease and the impurity of nanowire surface through chemical corrosion, the reagent volume of chemical cleaning is than sulfuric acid, hydrogen peroxide and the deionized water for 2:2:1.Send in high-temperature vacuum system again and carry out adding thermal purification, heating-up temperature is 850 DEG C, makes the GaN nano wire emission layer of p-type obtain atomically clean surfaces; P-type GaN nano wire emission layer adsorption Cs/O active coating 10 is made again by ultravacuum activation technology, the process that Cs, O activate is that Cs continues, and O source is interrupted, emission layer surface reaches negative electron affinity, final obtained reflective NEAGaN nano-wire array photocathode as shown in Figure 1.Its nano wire 5 diameter of reflective NEAGaN nano-wire array photocathode is 10 ~ 100nm, and length is 1 ~ 100 μm, and p-type doping content is 1 × 1019cm-3, and doped chemical is Zn.
Claims (10)
1. a reflective NEAGaN nano-wire array photocathode, the nano-wire array emission layer on the substrate layer surface that it is characterized in that, comprise substrate layer, is positioned at; Nano-wire array emission layer is made up of some p-type GaN nano wire, and p-type GaN nano wire surface is all adsorbed with Cs/O active coating.
2. reflective NEAGaN nano-wire array photocathode as claimed in claim 1, it is characterized in that, described substrate layer is Si or SiC.
3. reflective NEAGaN nano-wire array photocathode as claimed in claim 1, it is characterized in that, the diameter of described p-type GaN nano wire is 10 ~ 100nm, and length is 1 ~ 100 μm, and p-type doping content is 1 × 1019cm-3, and doped chemical is Zn.
4., in a method for substrate surface growth p-type GaN nano wire, it is characterized in that, step is as follows:
Step 101, on substrate evaporated metal Al formed metal Al layer, the described substrate with metal Al layer is placed in oxalic acid solution and carries out electrochemical corrosion, thus substrate surface formed porous alumina membrane;
Step 102, the mixed liquor that described surface has the substrate of mesh structural porous aluminum oxide film to put into phosphoric acid and chromic acid to be soaked, to remove on aluminum oxide film bottom hole with the aluminium oxide of substrate contact, the mesh structural porous anodic aluminum oxide film of formation rule size;
Step 103, at described mesh structural porous anodic aluminum oxide film surface evaporation layer of metal Ni, then substrate is put into NaOH aqueous slkali and soak, remove the anodic aluminum oxide film of substrate surface, thus on substrate, form W metal nano particle dot matrix;
Step 104, substrate and reaction source are put into the quartz boat partition heating of CVD reacting furnace, after the temperature of substrate and reaction source region all reaches design temperature, ammonia and argon gas is passed into CVD reacting furnace, then the insulation of CVD reacting furnace carries out deposition reaction to 550 DEG C, and the p-type GaN nano wire array of Ni catalyst granules is arranged at obtained top.
5., as claimed in claim 4 in the method for substrate surface growth p-type GaN nano wire, it is characterized in that, described substrate layer is Si or SiC; On substrate before evaporated metal Al, being first sulfuric acid and the hydrogen peroxide cleaning substrate of 1:1 by volume ratio, is then the hydrofluoric acid corrosion cleaning substrate of 5% with mass percent; Use electron beam evaporation methods evaporated metal Al on substrate to form Al layer in step 1, described Al layer thickness is 100 ~ 1000nm; Step 1 mesoxalic acid solution concentration is 0.5mol/L.
6. as claimed in claim 4 in the method for substrate surface growth p-type GaN nano wire, it is characterized in that, in step 102, in described phosphoric acid and chromic acid mixture, phosphoric acid quality percentage is 4%, and chromic acid mass percent is 2%.
7., as claimed in claim 4 in the method for substrate surface growth p-type GaN nano wire, it is characterized in that, use electron beam evaporation methods evaporation metal Ni layer in step 103, the thickness of W metal layer is 5 ~ 100nm; Described substrate put into mass percent be 5% NaOH aqueous slkali soak.
8. as claimed in claim 4 in the method for substrate surface growth p-type GaN nano wire, it is characterized in that, in step 104, GaCl3 is gallium source, ZnCl2 is doped chemical Zn source, as reaction source after the mixing of the ratio of mole ratio 1000:1, reaction source is positioned near CVD reacting furnace air inlet and the position of distance substrate about 10cm, and substrate is positioned at the center heating location of CVD reacting furnace; First vacuumize CVD reacting furnace before heating and pass into argon purge boiler tube; Substrate position heating-up temperature to 850 DEG C, reaction source position heating-up temperature to 600 DEG C; Described argon flow amount is 200ml/min, ammonia flow be 30ml/min; The deposition reaction time is 100 ~ 120min.
9. the method using method described in claim 4 to prepare reflective NEAGaN nano-wire array photocathode, it is characterized in that, be the Ni catalyst granules of the hydrochloric acid of 4%, the mixed acid solution removing p-type GaN nano wire array top of phosphoric acid and hydrofluoric acid with mass percent; Send in high-temperature vacuum system after cleaning and carry out adding thermal purification, make p-type GaN nano wire array obtain the surface of Atomically clean; Then in p-type GaN nano wire array surface absorption Cs/O active coating.
10. prepare the method for reflective NEAGaN nano-wire array photocathode as claimed in claim 9, it is characterized in that, with grease and the impurity on chemical cleaning reagent etching away p-type GaN nano wire surface, the sulfuric acid of chemical cleaning reagent to be volume ratio be 2:2:1, hydrogen peroxide and deionized water mixed liquor; Hot temperature degree in high-temperature vacuum system is 850 DEG C; Use ultravacuum activation technology in p-type GaN nano wire array surface absorption Cs/O active coating.
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