CN109256305A - Transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation - Google Patents
Transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation Download PDFInfo
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Abstract
The present invention relates to a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation includes the following steps: 1) to prepare material；2) high-temperature baking, nucleating layer growth, the growth of high-quality GaN peeling layer are successively carried out；3) the high aluminium component AlGaN photoemissive layer of growth p-type Mg doping；4) in AlGaN surface bond quartz window material；5) GaN layer is thoroughly decomposed using laser induced breakdown technology, peeling liner bottom；6) surface AlGaN carries out Cs or Cs/O layers of activation.Advantage: 1) replacing AlN as ultraviolet light photo cathode buffer layer, reduce buffer growth difficulty, improve the crystal quality of p-type AlGaN emission layer using GaN, is conducive to prepare more highly sensitive photocathode；2) buffer layer laser induced breakdown technology, sufficiently decomposition GaN layer are used, realizes substrate desquamation, can absorption to avoid substrate and buffer layer to ultraviolet incident ray, ensure that efficient detection of the photoemissive layer to ultraviolet light；3) substrate of laser lift-off may be reused, economy.
Description
Technical field
The present invention is a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation, belongs to ultraviolet spy
Survey field of material technology.
Background technique
Ultraviolet detection technology is that the another dual-use photoelectricity to grow up after infrared and Laser Detection Technique is visited
Survey technology.Due to the strong absorption and scattering process of the gas molecules such as ozone in atmosphere, solar radiation (ultraviolet source)
Light wave between medium wavelength 220-280nm is almost completely absorbed, thus the ultraviolet radioactive of this spectral coverage near sea level almost
Zero is decayed to, referred to as " day-old chick ".What ultraviolet detection mainly utilized is exactly the ultraviolet band of day-old chick, because in low latitude and ground
The 280nm that face is detected UV signal below is construed as from artificial emission source, for example, burning hydrocarbon,
All contain a large amount of ultraviolet signals in rocket and jet engine wake flame, guided missile plumage flame.Therefore, ultraviolet detection technology no matter
Military or civil field suffers from wide application value.
Ultraviolet vacuum detection device based on photocathode, vacuum device have fast response time, low noise, high gain etc. excellent
Point.As the core component of ultraviolet vacuum detection device, the quantum efficiency of photocathode is the most important of decision device overall performance
Factor.GaN base ultraviolet light photo cathode quantum efficiency based on negative electron affinity (NEA) (NEA) photoemission can be higher than 70%, more by
To favor.III group nitride material of GaN base is the novel semiconductor material for developing microelectronic component, opto-electronic device, AlGaN material
Material is with the variation of aluminium component, and forbidden bandwidth can be from 3.4 to 6.2eV consecutive variations, and corresponding wavelength changes from 365nm
200 nm cover day-old chick wave band, be develop deep ultraviolet detector ideal material, it can be achieved that high selectivity day it is blind ultraviolet
Detection.The ultraviolet light photo cathode technique research reported both at home and abroad at present mainly using p-type GaN material as photoelectric cathode materials,
Since GaN forbidden bandwidth is 3.4eV, the ultraviolet light that the ultraviolet detector based on GaN photocathode is 200-365nm to wavelength
Absorption will be generated, can not achieve truly full-time blind detection (200-280nm).Therefore must be greater than using Al component
0.4 p-type AlGaN photoelectric cathode materials are just able to achieve full-time blind ultraviolet detection.However, due to the AlN monocrystalline of large scale homogeneity
Substrate is not easy to prepare, at present more epitaxial growths that nitride is just carried out using foreign substrate (such as sapphire, silicon, silicon carbide),
But the direct epitaxial growth high Al contents AlGaN material in foreign substrate usually has very high defect concentration, epitaxial layer table
Face rises and falls greatly, causes device performance poor.Therefore, before growing high Al contents AlGaN layer, it usually needs carry out GaN or AlN
The growth of buffer layer, to improve the crystal quality of AlGaN layer.Transmission-type AlGaN solar blind UV cathode electroactive material, ultraviolet light from
Substrate back is incident, it is desirable that substrate and buffer layer have stronger transmitance to 200-280nm ultraviolet light, and Si, SiC, GaN are equal
Can strong absorption wave band ultraviolet light, therefore ultraviolet permeability is generally used based on AlGaN solar blind UV cathode electroactive material
Higher Sapphire Substrate and AlN buffer layer.But epitaxial growth AlN film is extremely difficult in Sapphire Substrate.Mainly have two
The reason of aspect: (1) Al-N bond energy is very strong, and Al atom is restricted in the diffusion of growing surface, and lateral growth rate is very
It is low, it is hardly formed two-dimensional layer growth；(2) source the Al TMAl and NH in MOCVD growth3Between have a strong pre-reaction, it is pre- anti-
A large amount of reactants can should be not only consumed, and the solid bond object formed may be deposited on sample surfaces and be unable to sufficiently divide
Solution, leads to the incorporation of impurity in epitaxial layer, or even will cause the polycrystalline growth of epitaxial layer.It is moved to improve the surface of Al atom
Shifting ability can generally improve the growth temperature (1200-1500 DEG C) in MOCVD, therefore higher to equipment power supply heating requirements.By
In the difficulty of AlN growth, the AlN grown on a sapphire substrate dislocation density (> 10 still with higher9cm-2)
[J.Cryst.Growth414(2015)76；J. Appl. Phys. 87(2000)996].And Grown on Sapphire Substrates GaN
Buffer layer is then relatively easy to, and growth temperature lower (950-1050 DEG C), growth rate are fast, and the dislocation density of epitaxial layer is also lower
(the 2-3 order of magnitude lower than AlN buffer layer) [J. Alloys Compd. 633 (2015) 494-498;Appl. Phys.
Lett. 88 (2006) 241917], but GaN buffer layer is high to deep ultraviolet light absorptivity, is to restrict it in AlGaN ultraviolet light photo yin
The key of pole application.The p-type AlGaN material of high defect concentration forms a large amount of electron capture center inside photocathode, leads
It causes carrier diffusion length reduction, interface recombination increase and electron surface escape probability to reduce, causes photocathode amount
Sub- efficiency reduces, the final photoelectric sensitivity for influencing detector.Therefore, using which kind of buffering in the preparation process of photocathode
Layer process should can reduce the defect concentration of AlGaN emission layer, while guarantee the relatively high transmittance of deep ultraviolet light, be to prepare height
The key of sensitivity AlGaN ultraviolet light photo cathode.
Laser lift-off technique (Laser lift off) is by (such as sapphire, SiC lining on laser projection to transparent substrate
Bottom) decomposition that causes GaN material, a technology [Phys. stat. for being separated from each other substrate and epitaxial material
sol. (c) 6 (2003) 1627].In this technique, the wavelength of laser will select properly, and the energy of laser photon is big
In the forbidden bandwidth of GaN, that is, requires the wavelength of laser to be less than 364nm, could be absorbed strongly by GaN.
Summary of the invention
Proposed by the present invention is a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation, mesh
Be laser lift-off technique is applied in transmission-type AlGaN ultraviolet light photo cathode preparation process, propose a kind of based on substrate
The transmission-type AlGaN ultraviolet light photo cathode preparation method of removing, to overcome the defect of AlGaN emission layer present in the prior art
The problems such as density is excessively high, deep ultraviolet light transmitance is lower, avoids the absorption of substrate and GaN material to ultraviolet light, obtain compared with
High conversion quantum efficiency prepares high performance AlGaN photocathode.
A kind of technical solution of the invention: transmission-type AlGaN ultraviolet light photo cathode preparation side based on substrate desquamation
Method includes the following steps:
1) prepare material: taking the substrate of a growing nitride；
2) grow GaN peeling layer: substrate is transferred to MOCVD system, substrate is successively carried out high-temperature baking, nucleating layer growth,
The growth of high-quality GaN peeling layer；
3) p-AlGaN emission layer is grown: on high-quality GaN buffer layer, the high aluminium component AlGaN photoelectricity of growth p-type Mg doping
Emission layer；
4) quartz window front is bonded: the epitaxial material of step 3 is transferred out of MOCVD system, clean the surface, on the surface AlGaN
Bonding quartz window material；
5) substrate desquamation: the material of step 4 is transferred in laser lift-off equipment, using laser induced breakdown technology that GaN layer is thorough
It decomposes, peeling liner bottom；
6) Cs or Cs/O layers of activation: quartz window is the back side, and AlGaN is front surface, is banged using chemical cleaning and high-power electron beam
The adsorbate for hitting removal cathode material surface, AlGaN photoelectric cathode materials is transferred in ultra-high vacuum system, in AlGaN table
Face carries out Cs or Cs/O layers of activation.
Beneficial effects of the present invention:
(1) it replaces AlN as ultraviolet light photo cathode buffer layer using GaN, reduces buffer growth difficulty, greatly improve
The crystal quality of p-type AlGaN emission layer is conducive to prepare more highly sensitive photocathode；
(2) buffer layer laser induced breakdown technology, sufficiently decomposition GaN layer are used, realizes substrate desquamation, it can be to avoid substrate and buffer layer
Absorption to ultraviolet incident ray ensure that efficient detection of the photoemissive layer to ultraviolet light；
(3) substrate of laser lift-off may be reused, economy.
(4) advantage that GaN buffer layer epitaxy technique is simple, crystal quality is high is played, buffer layer laser induced breakdown technology is answered
In the preparation for using AlGaN ultraviolet light photo cathode, there is important novelty.
Detailed description of the invention
Attached drawing 1 is the transmission-type AlGaN ultraviolet light photo cathode preparation method flow chart based on substrate desquamation.
Attached drawing 2 is AlGaN ultraviolet light photo-cathode material structure figure before substrate desquamation.
Attached drawing 3 is AlGaN ultraviolet light photo-cathode material structure figure after substrate desquamation.
Wherein, S1-S6 is step 1-6, and 10 be substrate, 20 be GaN buffer layer, 30 is p-AlGaN emission layer, 40 be quartzy
Window, 50 be C, Cs/O active coating.
Specific embodiment
A kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation, includes the following steps:
1) prepare material: taking the substrate of a growing nitride；
2) grow GaN peeling layer: substrate is transferred to MOCVD system, substrate is successively carried out high-temperature baking, nucleating layer growth,
The growth of high-quality GaN peeling layer；
3) p-AlGaN emission layer is grown: on high-quality GaN buffer layer, the high aluminium component AlGaN photoelectricity of growth p-type Mg doping
Emission layer；
4) quartz window front is bonded: the epitaxial material of step 3 is transferred out of MOCVD system, clean the surface, on the surface AlGaN
Bonding quartz window material；
5) substrate desquamation: the material of step 4 is transferred in laser lift-off equipment, using laser induced breakdown technology that GaN layer is thorough
It decomposes, peeling liner bottom；
6) Cs or Cs/O layers of activation: quartz window is the back side, and AlGaN is front surface, is banged using chemical cleaning and high-power electron beam
The adsorbate for hitting removal cathode material surface, AlGaN photoelectric cathode materials is transferred in ultra-high vacuum system, in AlGaN table
Face carries out Cs or Cs/O layers of activation.
Substrate described in step 1) is one of sapphire, silicon carbide, silicon, gallium nitride single crystal.
GaN peeling layer described in step 2 with a thickness of 0.5 μm -5 μm.
P-AlGaN photoemissive layer described in step 3) is with a thickness of 50-200nm, Al component >=0.4, Mg doping concentration model
Enclose is 1018cm-3-1019cm-3。
Quartz window material thickness described in step 4) is 2mm-5mm.
The laser wavelength range that laser lift-off technique described in step 5) uses is 300nm-360nm.
Further explanation of the technical solution of the present invention with reference to the accompanying drawing
As shown in Fig. 1, a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation, including walk as follows
It is rapid:
1) prepare material: taking the substrate of a growing nitride；
2) grow GaN peeling layer: substrate is transferred to MOCVD system, substrate is successively carried out high-temperature baking, nucleating layer growth,
The growth of high-quality GaN peeling layer；
3) p-AlGaN emission layer is grown: on high-quality GaN buffer layer, the high aluminium component AlGaN photoelectricity of growth p-type Mg doping
Emission layer；
4) quartz window front is bonded: the epitaxial material of step 3 is transferred out of MOCVD system, clean the surface, on the surface AlGaN
Bonding quartz window material；As shown in Fig. 2.
5) substrate desquamation: the material of step 4 is transferred in laser lift-off equipment, using laser induced breakdown technology by GaN layer
It thoroughly decomposes, peeling liner bottom；As shown in Fig. 3.
6) Cs or Cs/O layers of activation: quartz window is the back side, and AlGaN is front surface, utilizes chemical cleaning and high energy electron
The adsorbate on beam bombardment removal cathode material surface, AlGaN photoelectric cathode materials are transferred in ultra-high vacuum system,
The surface AlGaN carries out Cs or Cs/O layers of activation.
Embodiment 1
A twin polishing Sapphire Substrate 10 is taken, substrate is transferred to MOCVD system, in 1100 DEG C of atmosphere of hydrogen of substrate high temperature
Baking 5 minutes, is cooled to 600 DEG C of progress 20nmGaN nucleating layer growths；It further heats up slow to 1050 DEG C of progress high-quality GaNs
The growth of layer 20 is rushed, growth thickness is 2 μm；
Secondly on high-quality GaN buffer layer, growth temperature is improved to 1080 DEG C, the high aluminium component AlGaN that growth p-type Mg is adulterated
Photoemissive layer 30, thickness 100nm, Al component 0.4, Mg doping concentration 1 × 1019cm-3；
Then, it is cooled to room temperature, epitaxial material is transferred out of MOCVD system, acetone, ethyl alcohol, deionized water ultrasound is respectively adopted
Clean the surface is dirty, the bonding quartz window material 40 on AlGaN emission layer, and quartz window material thickness is 2mm；
Then, material is transferred in laser lift-off equipment, using the laser of wavelength 325nm, focuses and decompose GaN layer 20,10
GaN is thoroughly decomposed after minute, peeling liner bottom 10；
Finally, the photoelectric cathode materials to peeling liner bottom carry out chemical cleaning, AlGaN photoelectric cathode materials are transferred to vacuum degree
Better than 10-8In the ultra-high vacuum system of Pa magnitude, using high-power electron beam bombard the surface AlGaN, remove adsorption carbon,
The impurity such as hydrogen, oxygen obtain the surface of atom level cleaning, carry out Cs or Cs/O layer 50 on the surface AlGaN and activate, with a thickness of one
Monoatomic layer, the final transmission-type AlGaN ultraviolet light photo cathode for obtaining high-quantum efficiency.
Embodiment 2
Firstly, taking a silicon substrate 10, substrate is transferred to MOCVD system, to 5 points of baking in 1100 DEG C of atmosphere of hydrogen of substrate high temperature
Clock is cooled to 600 DEG C of progress 20nmAlN nucleating layer growths；It further heats up raw to 1050 DEG C of progress high-quality GaN buffer layers 20
Long, growth thickness is 5 μm；
Secondly on high-quality GaN buffer layer, growth temperature is improved to 1080 DEG C, the high aluminium component AlGaN that growth p-type Mg is adulterated
Photoemissive layer 30, thickness 70nm, Al component 0.5, Mg doping concentration are 5 × 1019cm-3；
Then, it is cooled to room temperature, epitaxial material is transferred out of MOCVD system, acetone, ethyl alcohol, deionized water ultrasound is respectively adopted
Clean the surface is dirty, the bonding quartz window material 40 on AlGaN emission layer, and quartz window material thickness is 4mm；
Then, material is transferred in laser lift-off equipment, using the laser of wavelength 325nm, focuses and decompose GaN layer 20,20
GaN is thoroughly decomposed after minute, peeling liner bottom 10；
Finally, the photoelectric cathode materials to peeling liner bottom carry out chemical cleaning, AlGaN photoelectric cathode materials are transferred to vacuum degree
Better than 10-8In the ultra-high vacuum system of Pa magnitude, using high-power electron beam bombard the surface AlGaN, remove adsorption carbon,
The impurity such as hydrogen, oxygen obtain the surface of atom level cleaning, carry out Cs or Cs/O layer 50 on the surface AlGaN and activate, with a thickness of one
Monoatomic layer, the final transmission-type AlGaN ultraviolet light photo cathode for obtaining high-quantum efficiency.
Embodiment 3
Firstly, taking a silicon carbide substrates 10, substrate is transferred to MOCVD system, to drying in 1100 DEG C of atmosphere of hydrogen of substrate high temperature
It is 5 minutes roasting, it is cooled to 900 DEG C of progress 60nm AlN nucleating layer growths；It further heats up to 1050 DEG C of progress high-quality GaN bufferings
Layer 20 is grown, and growth thickness is 1.5 μm；
Secondly on high-quality GaN buffer layer, growth temperature is improved to 1080 DEG C, the high aluminium component AlGaN that growth p-type Mg is adulterated
Photoemissive layer 30, thickness 150nm, Al component 0.4, Mg doping concentration are 5 × 1018cm-3；
Then, it is cooled to room temperature, epitaxial material is transferred out of MOCVD system, acetone, ethyl alcohol, deionized water ultrasound is respectively adopted
Clean the surface is dirty, the bonding quartz window material 40 on AlGaN emission layer, and quartz window material thickness is 5mm；
Then, material is transferred in laser lift-off equipment, using the laser of wavelength 355nm, focuses and decompose GaN layer 20,10
GaN is thoroughly decomposed after minute, peeling liner bottom 10；
Finally, the photoelectric cathode materials to peeling liner bottom carry out chemical cleaning, AlGaN photoelectric cathode materials are transferred to vacuum degree
Better than 10-8In the ultra-high vacuum system of Pa magnitude, using high-power electron beam bombard the surface AlGaN, remove adsorption carbon,
The impurity such as hydrogen, oxygen obtain the surface of atom level cleaning, carry out Cs or Cs/O layer 50 on the surface AlGaN and activate, with a thickness of one
Monoatomic layer, the final transmission-type AlGaN ultraviolet light photo cathode for obtaining high-quantum efficiency.
Embodiment 4
Firstly, taking a gallium nitride monocrystal substrate 10, substrate is transferred to MOCVD system, to 1000 DEG C of ammonia atmosphere of substrate high temperature
Middle baking 5 minutes is cooled to 900 DEG C of progress 20nm GaN nucleating layer growths；It further heats up to 1050 DEG C of progress high-quality GaNs
Buffer layer 20 is grown, and growth thickness is 0.5 μm；
Secondly on high-quality GaN buffer layer, growth temperature is improved to 1080 DEG C, the high aluminium component AlGaN that growth p-type Mg is adulterated
Photoemissive layer 30, thickness 200nm, Al component 0.4, Mg doping concentration are 1 × 1018cm-3；
Then, it is cooled to room temperature, epitaxial material is transferred out of MOCVD system, acetone, ethyl alcohol, deionized water ultrasound is respectively adopted
Clean the surface is dirty, the bonding quartz window material 40 on AlGaN emission layer, and quartz window material thickness is 5mm；
Then, material is transferred in laser lift-off equipment, using the laser of wavelength 355nm, focuses and decompose GaN layer 20,10
GaN is thoroughly decomposed after minute, peeling liner bottom 10；
Finally, the photoelectric cathode materials to peeling liner bottom carry out chemical cleaning, AlGaN photoelectric cathode materials are transferred to vacuum degree
Better than 10-8In the ultra-high vacuum system of Pa magnitude, using high-power electron beam bombard the surface AlGaN, remove adsorption carbon,
The impurity such as hydrogen, oxygen obtain the surface of atom level cleaning, carry out Cs or Cs/O layer 50 on the surface AlGaN and activate, with a thickness of one
Monoatomic layer, the final transmission-type AlGaN ultraviolet light photo cathode for obtaining high-quantum efficiency.
Claims (6)
1. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation, which is characterized in that including walking as follows
It is rapid:
1) prepare material: taking the substrate of a growing nitride；
2) grow GaN peeling layer: substrate is transferred to MOCVD system, substrate is successively carried out high-temperature baking, nucleating layer growth,
The growth of high-quality GaN peeling layer；
3) p-AlGaN emission layer is grown: on high-quality GaN buffer layer, the high aluminium component AlGaN photoelectricity of growth p-type Mg doping
Emission layer；
4) quartz window front is bonded: the epitaxial material of step 3 is transferred out of MOCVD system, clean the surface, on the surface AlGaN
Bonding quartz window material；
5) substrate desquamation: the material of step 4 is transferred in laser lift-off equipment, using laser induced breakdown technology that GaN layer is thorough
It decomposes, peeling liner bottom；
6) Cs or Cs/O layers of activation: quartz window is the back side, and AlGaN is front surface, is banged using chemical cleaning and high-power electron beam
The adsorbate for hitting removal cathode material surface, AlGaN photoelectric cathode materials is transferred in ultra-high vacuum system, in AlGaN table
Face carries out Cs or Cs/O layers of activation.
2. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation according to claim 1,
It is characterized in that substrate described in step 1) is one of sapphire, silicon carbide, silicon, gallium nitride single crystal.
3. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation according to claim 1,
Be characterized in that GaN peeling layer described in step 2 with a thickness of 0.5 μm -5 μm.
4. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation according to claim 1,
It is characterized in that p-AlGaN photoemissive layer described in step 3) with a thickness of 50-200nm, Al component >=0.4, Mg doping concentration model
Enclose is 1018cm-3-1019cm-3。
5. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation according to claim 1,
It is characterized in that quartz window material thickness described in step 4) is 2mm-5mm.
6. a kind of transmission-type AlGaN ultraviolet light photo cathode preparation method based on substrate desquamation according to claim 1,
It is characterized in that the laser wavelength range that laser lift-off technique described in step 5) uses for 300nm-360nm.
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| CN111933747A (en) * | 2020-07-22 | 2020-11-13 | 中国电子科技集团公司第十三研究所 | Surface array back-incident solar blind ultraviolet detector and preparation method thereof |
| CN111933741A (en) * | 2020-07-22 | 2020-11-13 | 中国电子科技集团公司第十三研究所 | Back incidence ultraviolet detector based on silicon substrate and preparation method thereof |
| CN111933748A (en) * | 2020-07-22 | 2020-11-13 | 中国电子科技集团公司第十三研究所 | Back-incident solar blind ultraviolet detector and manufacturing method thereof |
| CN113921665A (en) * | 2021-12-14 | 2022-01-11 | 山西中科潞安紫外光电科技有限公司 | Deep ultraviolet LED epitaxial wafer with vertical structure and growth method thereof |
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| CN111933747A (en) * | 2020-07-22 | 2020-11-13 | 中国电子科技集团公司第十三研究所 | Surface array back-incident solar blind ultraviolet detector and preparation method thereof |
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| CN113921665A (en) * | 2021-12-14 | 2022-01-11 | 山西中科潞安紫外光电科技有限公司 | Deep ultraviolet LED epitaxial wafer with vertical structure and growth method thereof |
| CN114220889A (en) * | 2021-12-14 | 2022-03-22 | 山西中科潞安紫外光电科技有限公司 | Deep ultraviolet LED epitaxial wafer with vertical structure and growth method thereof |
| CN113921665B (en) * | 2021-12-14 | 2022-04-12 | 山西中科潞安紫外光电科技有限公司 | Deep ultraviolet LED epitaxial wafer with vertical structure and growth method thereof |
| CN114220889B (en) * | 2021-12-14 | 2024-04-30 | 山西中科潞安紫外光电科技有限公司 | Deep ultraviolet LED epitaxial wafer with vertical structure and growth method thereof |
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