CN101315968A - Production method of GaN multi-layer quantum point photoelectric material - Google Patents
Production method of GaN multi-layer quantum point photoelectric material Download PDFInfo
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- CN101315968A CN101315968A CNA2008101502724A CN200810150272A CN101315968A CN 101315968 A CN101315968 A CN 101315968A CN A2008101502724 A CNA2008101502724 A CN A2008101502724A CN 200810150272 A CN200810150272 A CN 200810150272A CN 101315968 A CN101315968 A CN 101315968A
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Abstract
The invention discloses a preparation method for a GaN multi-layer quantum dot photoelectric material; the process of the manufacture method comprises the following steps: an MOCVD equipment is firstly used to lead a low temperature damping layer and an n-ALGaN-based substrate layer (2) of a high-temperature Ga polar surface to grow on an underlay; subsequently, the n-AlGaN-based substrate layer (2) is corroded by a melting KOH process; an inverted hexangular pyramid shape corrosion hole (3) is formed at the exposal position of the staggered surface of the n-AlGaN; subsequently, a GaN thin layer (4) grows on the corroded n-AlGaN-based substrate layer; furthermore, an AlGaN thin layer (5) grows on the GaN thin layer; the bottom of the inverted hexangular pyramid shape corrosion hole (3) forms a GaN quantum pot (6); subsequently, according to the given layer number of the GaN thin layer (4), the GaN quantum pot is formed at the bottom of the inverted hexangular pyramid shape corrosion hole of all GaN thin layers; finally, a p-AlGaN layer grows on the uppermost GaN thin layer. The preparation method of the invention has the advantages of simple technology, easy controlling dimension of the quantum pot and uniformility, thus being applicable to manufacturing the photoelectron devices with high brightness, high efficiency, high stability and continuous and adjustable wavelength in batch.
Description
Technical field
The invention belongs to microelectronics technology, relate to the making of semi-conducting material, the particularly making of GaN quantum dot light electric material can be used for batch making high brightness high efficiency high stability and the continuously adjustable opto-electronic device of wavelength.
Background technology
Semiconductor-quantum-point has totally different optical property in bulk material, and the layer structure of quantum dot is that the fusion of nano material and traditional microelectronics and photoelectron technology brought may.And be considered to be in the material that application prospect is arranged in blue light and the UV wavelength range most for a long time as the GaN of third generation semi-conducting material representative.Utilize GaN base indigo plant/green luminescence device tranmitting frequency that GaN low-dimensional quantum point material structure makes with change in size change, line of departure width, luminous quantum efficiency is higher relatively and the photostability of superelevation, is subjected to people's extensive concern in recent years.
Make the GaN quantum dot and can adopt following several method: 1. microfabrication method.Promptly containing on the quantum well of two-dimensional electron gas the method for etching again.2. artificial substrate selective growth method.Promptly on the patterned substrate of manually making, grow, perhaps selective growth quantum dot on the surface after mask, the etching.3. direct growth method.I.e. direct growth quantum dot on various natural surfaces is as low-angle face, super step surface and high-index surface; Perhaps utilize the self-organization grown quantum point of heterogeneous interface stress.4. surfactant or surface oxidation agent method.
Wherein, preceding two kinds of methods are easy to control the growth position and the uniformity of quantum dot, but since the damage that brings of etching process and because of the figure true resolution not high, make the quantum dot lateral dimension bigger than longitudinal size, and introduce defective easily, reduce electronics-hole-recombination efficient and luminous intensity is reduced.In addition, microfabrication and graph substrate will be introduced multiple working procedure, be unfavorable for developing to the industrialization direction of practicality.Though then two kinds of methods can prepare the zero defect quantum dot, be difficult to realize size and inhomogeneity control to quantum dot.
The content of invention
The deficiency that is to overcome above-mentioned prior art of the present invention provides a kind of manufacture method of GaN multi-layer quantum point photoelectric material, with the size and the uniformity of simple technology controlling and process GaN quantum dot, to improve the performance of GaN base nanostructure opto-electronic device.
Technical scheme of the present invention is:
That utilizes the etch natural selection forms the shape of falling hexagonal pyramid etch pit at extension n-AlGaN substrate surface, in GaN/AlGaN superlattice structure growth course next, and the formation quantum dot that gas surface transport mechanism makes self-organizing bottom hexagonal vertebra shape hole.Its concrete operations step is as follows:
A, with the MOCVD equipment n-AlGaN basalis of low temperature growth buffer layer and high temperature Ga polar surface successively on substrate;
B, the n-AlGaN basalis is corroded with fusion KOH method, the place of appearing on the surface of this n-AlGaN dislocation forms the shape of falling hexagonal pyramid etch pit;
C, on the n-AlGaN basalis after the corrosion growing GaN thin layer, make the GaN thickness thickness outside its hole in the shape of falling the hexagonal pyramid etch pit (3);
D, the AlGaN thin layer of growing on the GaN thin layer make the bottom of the shape of falling hexagonal vertebra etch pit form the GaN quantum dot;
E, the number of plies of pressing the GaN thin layer of setting repeat above-mentioned steps C and D, form the GaN quantum dot in the shape of falling the hexagonal vertebra etch pit bottom of all GaN thin layers;
F, the p-AlGaN layer of on the GaN of the superiors thin layer, growing.
The uniformity of the quantum dot in the technique scheme is controlled by substrate AlGaN layer crystal particle size, and crystallite dimension increases end temperature resilient coating annealing pressure by low temperature buffer growth conditions control in the two step method, can reduce crystallite dimension, improves the quantum dot uniformity.
The density of the quantum dot in the technique scheme is controlled by substrate n-AlGaN laminar surface dislocation density.By changing high temperature AlGaN growth conditions, change this layer cross growth speed.Growth temperature is high more or the V/III ratio is more little, and dislocation transverse curvature degree is big more, and the surface level dislocation density is more little, thereby quantum dot density is more little.
The width of the quantum dot in the technique scheme is controlled by the etch pit width.Increase etching time or increase corrosion temperature, increase etch pit hexagon diameter, thereby increase the quantum dot width.Therefore,, regulate the quantum dot width, obtain any width quantum dot, thereby obtain the quantum dot of different glow frequencies, realize luminous continuously by change to etching condition.
Quantum dot thickness in the technique scheme is by the THICKNESS CONTROL of GaN thin layer.By changing the GaN layer growth time, regulate this layer thickness, to regulate the quantum dot thickness, obtain any thickness quantum dot.Thereby obtain the quantum dot of different glow frequencies, realize luminous continuously.
N-AlGaN thickness of thin layer in the technique scheme changes according to the change of GaN thickness of thin layer, and the two is proportional, and this thickness adjusted realizes by changing this layer growth time.
The GaN/AlGaN superlattice number of plies in the technique scheme is adjustable.Increase the number of plies of cycling deposition, can increase the quantum dot number of plies, thereby improve the luminous intensity of this material structure.
The advantage that the present invention compared with prior art has:
1, the uniformity of quantum dot is controlled by substrate AlGaN layer crystal particle size among the GaN multi-layer quantum point preparation method provided by the invention, and crystallite dimension is controlled by the low temperature buffer growth conditions.The density of quantum dot is controlled by substrate AlGaN laminar surface dislocation density, and surface dislocation density is controlled by the heat zone growth conditions.This method has made full use of the growth characteristic control quantum dot density and the uniformity of crystal self, with respect to direct growth method and surfactant or surface oxidation agent method, is easy to control, and is reliable and stable.
2, among the GaN multi-layer quantum point preparation method provided by the invention owing to adopt the quantum dot that obtains different glow frequencies by control to etching condition and growth time, not only control procedure is easy, and can realize continuously luminous.
3, quantum dot size and uniformity are subjected to irrelevant controlling factors respectively among the GaN multi-layer quantum point preparation method provided by the invention, thereby solved the size of quantum dot in the GaN quantum dot manufacture process and the problem that uniformity can't satisfy simultaneously, nanometer technology organically is dissolved in the traditional microelectronics and photoelectron technology.
4, rely on the surperficial gas phase transport of simple natural etching method and crystal growth to form quantum dot among the GaN multi-layer quantum point preparation method provided by the invention, microfabrication method and manually substrate selective growth method relatively, when guaranteeing the quantum point mass, operation is simple, easy to operate, thereby be applicable to large-scale industrialization production.
The description of the drawings
Fig. 1 is a process chart of the present invention;
Fig. 2 is the schematic diagram of Quantum Dots Growth process of the present invention;
Fig. 3 is the schematic cross-section that the single quantum dot of the present invention forms;
Fig. 4 is the schematic top plan view of the single quantum dot of the present invention;
Fig. 5 is the schematic perspective view of the single quantum dot of the present invention;
Fig. 6 is the schematic cross-section of multi-layer quantum point of the present invention.
Embodiment
With reference to Fig. 1, manufacturing process of the present invention is as follows:
Step 1, the n-AlGaN basalis 2 of low temperature growth buffer layer 1 and high temperature Ga polar surface successively on substrate, as shown in Figure 1a.
In MOCVD equipment with traditional two step method growth low temperature buffer layer 1 earlier, the n-AlGaN basalis 2 of regrowth high temperature Ga polar surface, wherein the temperature of resilient coating is 450 ± 20 ℃, and GaN quantum dot uniformity that basalis temperature, V/III and annealing pressure produce subsequent step and density are by very big relation.The present invention adopts the uniformity by the crystallite dimension control GaN quantum dot that reduces n-AlGaN basalis 2, promptly realizes that by the annealing pressure that increases low temperature buffer layer this annealing pressure is 250～400torr.The present invention adopts the density by the density control GaN quantum dot of n-AlGaN basalis surface dislocation, promptly change the n-AlGaN basalis temperature of growth high temperature Ga polar surface and V/III than and realize the density control of GaN quantum dot.For reaching 5 * 10
9Cm
-2Above high quantum dot density, it is adjustable that the temperature of growth n-AlGaN basalis is located at 800 ℃～900 ℃ scopes, and it is adjustable that the V/III ratio is located at 3000～6000 scopes; For reaching 5 * 10
8Cm
-2Following low quantum dot density, it is adjustable that the n-AlGaN basalis temperature of will growing is located at 1000 ℃～1100 ℃ scopes, and it is adjustable that the V/III ratio is located at 1000～2000 scopes.
Corrode this n-AlGaN layer with fusion KOH, because crystalline anisotropy and Ga surface chemistry stability make dislocation appear on the AlGaN surface and locates optionally to be corroded the shape of falling hexagonal pyramid etch pit 3.The width may command subsequent step of adjusting this shape of falling hexagonal pyramid etch pit 2 forms the width of GaN quantum dot, promptly by the etching time or the corrosion temperature that change this step, realizes the change to etch pit hexagon diameter.For example, change to 10nm for the quantum dot width by 2nm, under fixing corrosion temperature, etching time increases to 10min by 1min; Or under fixing etching time, corrosion temperature increases to 300 ℃ by 210 ℃.
Growing GaN thin layer 4 on the n-AlGaN basalis after the corrosion, when cross growth speed was very fast, reactant was shifted to bottom, the shape of falling hexagonal pyramid hole in a large number, incorporates lattice there into, thus the GaN thickness of conical pit bottom is outside the hole, as shown in Figure 2.For realizing big GaN cross growth speed, can select high relatively growth temperature and relative low V/III than condition, the growth temperature of reference is 800 ℃～900 ℃, the V/III ratio is 3000～6000.The controllable thickness system subsequent step that changes this GaN thin layer forms the thickness of GaN quantum dot, promptly by the THICKNESS CONTROL of the GaN layer growth time realization in this step of change to the GaN quantum dot, for thickness is the GaN thin layer of 1～5nm, and the time of its growth is 30s～150s.
Growth AlGaN thin layer 5 on GaN thin layer 4 because AlGaN atomic surface mobility is less than the Ga atom, therefore in the shape of falling the hexagonal pyramid hole with the hole outside the AlGaN layer thickness more consistent.Thereby the formation GaN quantum dot between the bottom two layers AlGaN of the shape of falling hexagonal vertebra hole of self-organizing.This GaN quantum dot shape is hexagon, as shown in Figure 4.The three-dimensional shape of the GaN quantum dot bottom this etch pit as shown in Figure 5.For realizing low AlGaN cross growth speed, can select high relatively growth temperature and relative low V/III than condition, the growth temperature of reference is 1000 ℃～1100 ℃, the V/III ratio is 1000～2000.The thickness of the thickness of this AlGaN thin layer 5 and GaN thin layer 4 is proportional, and the thickness of AlGaN thin layer 5 realizes by the time that changes this layer growth, is the AlGaN thin layer of 1～5nm for thickness, and its growth time is 30s～150s.
Since the AlGaN thin layer in fall hexagonal vertebra hole with cheat outside thickness about equally, the shape in hole can not occur bigger variation because of the increase of the number of plies.Therefore the multilayer GaN/AlGaN superlattice structure of growing continuously can obtain the GaN quantum dot of sandwich construction, promptly press the number of plies of the GaN thin layer of setting 4, repeat above-mentioned steps 3 and step 4, then form the GaN quantum dot, as shown in Figure 6 in the shape of falling the hexagonal vertebra etch pit bottom of all GaN thin layers.The number of plies that the brightness of these GaN quantum dots improves by increasing the GaN thin layer realizes.For example, when the brightness that adjust the GaN quantum dot was 60lumen/watt, its number of plies was at least 5 layers.
The step 6. p-AlGaN layer 8 of growing on the GaN of the superiors thin layer 7 is shown in Fig. 1 g.
Growth p-AlGaN layer 8 on the GaN of the superiors thin layer 7 is filled and led up the shape of falling hexagonal vertebra hole, forms even curface, finishes the making of whole GaN multi-layer quantum point photoelectric material.
The present invention provides following examples according to above-mentioned steps, but is not limited to these embodiment.
Embodiment 1
(1) with the MOCVD equipment n-AlGaN basalis of growing low temperature AlN resilient coating and high temperature Ga polar surface successively on Sapphire Substrate, temperature buffer layer is 450 ℃, and annealing pressure is 400torr, and the growth temperature of heat zone is 1000 ℃, and the V/III ratio is 1160;
(2) corrode this AlGaN layer with fusion KOH, corrosion temperature is 280 ℃, and etching time is 4min.Clean corrosion surface, be reentered in the MOCVD equipment;
(3) grow thick is the GaN thin layer of 2nm on the n-AlGaN basalis after the corrosion, and growth time is about 60s;
(4) grow thick is the AlGaN thin layer of 2.5nm on the GaN thin layer, and growth time is about 75s.
(5) repeat above-mentioned steps (3) and step (4) totally 5 times.
(6) growth p-AlGaN layer and cap layer, the shape of falling hexagonal vertebra hole is filled and led up, and forms smooth quantum dot optoelectronic material surface.
(1) with the MOCVD equipment n-AlGaN basalis of growing low temperature AlN resilient coating and high temperature Ga polar surface successively on silicon carbide substrates, temperature buffer layer is 460 ℃, and annealing pressure is 350torr, and the growth temperature of heat zone is 1100 ℃, and the V/III ratio is 1000;
(2) corrode this AlGaN layer with fusion KOH, corrosion temperature is 210 ℃, and etching time is 8min.Clean corrosion surface, be reentered in the MOCVD equipment;
(3) grow thick is the GaN thin layer of 3nm on the n-AlGaN basalis after the corrosion, and growth time is about 90s;
(4) grow thick is the AlGaN thin layer of 4nm on the GaN thin layer, and growth time is 116s;
(5) repeat above-mentioned steps (3) and (4) totally 3 times;
(6) growth p-AlGaN layer and cap layer, the shape of falling hexagonal vertebra hole is filled and led up, and forms smooth quantum dot optoelectronic material surface.
(1) with the MOCVD equipment n-AlGaN basalis of growing low temperature AlN resilient coating and high temperature Ga polar surface successively on silicon substrate, temperature buffer layer is 440 ℃, and annealing pressure is 300torr, and the growth temperature of heat zone is 900 ℃, and the V/III ratio is 3000;
(2) corrode this AlGaN layer with fusion KOH, corrosion temperature is 230 ℃, and etching time is 3min.Clean corrosion surface, be reentered in the MOCVD equipment;
(3) grow thick is the GaN thin layer of 1nm on the n-AlGaN basalis after the corrosion, and growth time is 30s;
(4) grow thick is the AlGaN thin layer of 1.5nm on the GaN thin layer, and growth time is 40s.
(5) repeat above-mentioned steps (3) and (4) totally 6 times.
(6) growth p-AlGaN layer and cap layer, the shape of falling hexagonal vertebra hole is filled and led up, and forms smooth quantum dot optoelectronic material surface.
It is several that substrate of the present invention is not limited to that the foregoing description provides, and can select dielectric substrate or Semiconductor substrate arbitrarily.The number of plies of GaN thin layer 4 of the present invention is that the brightness requirement of the photoelectric material of multi-layer quantum point is set according to active layer.The density of quantum dot of the present invention can be selected arbitrarily, be not limited to provide in the foregoing description 5 * 10
9Cm
-2Above high quantum dot density and 5 * 10
8Cm
-2Following low quantum dot density.
Claims (8)
1. the manufacture method of a GaN multi-layer quantum point photoelectric material comprises following process:
A, with the MOCVD equipment n-AlGaN basalis (2) of low temperature growth buffer layer (1) and high temperature Ga polar surface successively on substrate;
B, n-AlGaN basalis (2) is corroded with fusion KOH technology, the place of appearing on the surface of this n-AlGaN dislocation forms the shape of falling hexagonal pyramid etch pit (3);
C, on the n-AlGaN basalis after the corrosion growing GaN thin layer (4), make the GaN thickness thickness outside its hole in the shape of falling the hexagonal pyramid etch pit (3);
D, the AlGaN thin layer (5) of growing on GaN thin layer (4) make the bottom of the shape of falling hexagonal vertebra etch pit (3) form GaN quantum dot (6);
E, the number of plies of pressing the GaN thin layer of setting (4) repeat above-mentioned steps C and D, form the GaN quantum dot in the shape of falling the hexagonal vertebra etch pit bottom of all GaN thin layers;
F, the p-AlGaN layer (8) of on the GaN of the superiors thin layer (7), growing.
2. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 1, the uniformity that it is characterized in that the GaN quantum dot is by reducing the crystallite dimension control of n-AlGaN basalis (2), realize by the annealing pressure that increases the low temperature buffer layer in the steps A that promptly this annealing pressure is adjustable in 250～400torr scope.
3. by the described GaN multi-layer quantum point photoelectric material of claim 1 manufacture method, the density that it is characterized in that the GaN quantum dot is by the density control of n-AlGaN basalis surface dislocation, promptly change the n-AlGaN basalis temperature of growth high temperature Ga polar surface in the steps A and V/III than and realize.
4. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 1, it is characterized in that of the width control of the width of GaN quantum dot by the shape of falling hexagonal pyramid etch pit (3), promptly, realize change to etch pit hexagon diameter by the etching time or the corrosion temperature that change step B.
5. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 1, it is characterized in that the THICKNESS CONTROL of the thickness of GaN quantum dot by the GaN thin layer, promptly realize by changing the GaN layer growth time among the step C, for thickness is the GaN thin layer of 1～5nm, and the time of its growth is 30s～150s.
6. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 1, it is characterized in that the brightness of GaN quantum dot improves by increasing the number of plies realization of quantum dot in the step e, when brightness was 60lumen/watt, its number of plies was at least 5 layers.
7. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 1, the thickness that it is characterized in that the thickness of AlGaN thin layer (5) and GaN thin layer (4) is proportional, the thickness of this AlGaN thin layer (5) was realized by the time that changes this layer growth, for thickness is the AlGaN thin layer of 1～5nm, and its growth time is 30s～150s.
8. by the manufacture method of the described GaN multi-layer quantum point photoelectric material of claim 4, the etching time that it is characterized in that changing step B is to carry out under the fixing condition of corrosion temperature, and the corrosion temperature that changes step B is to carry out under the fixing condition of etching time; Change to 10nm for the quantum dot width by 2nm, under fixing corrosion temperature, its etching time increases to 10min by 1min; Or under fixing etching time, corrosion temperature increases to 300 ℃ by 210 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2494498C2 (en) * | 2011-02-24 | 2013-09-27 | Юрий Георгиевич Шретер | Semiconductor light-emitting device |
| CN105355741A (en) * | 2015-11-02 | 2016-02-24 | 厦门市三安光电科技有限公司 | LED epitaxial structure and making method thereof |
| CN106601784A (en) * | 2015-10-15 | 2017-04-26 | 比亚迪股份有限公司 | Substrate and substrate formation method |
| CN110098292A (en) * | 2019-03-06 | 2019-08-06 | 西安电子科技大学 | Bluish-green light emitting diode with quantum dots and preparation method based on nano graph |
| CN112397618A (en) * | 2020-11-27 | 2021-02-23 | 安徽中医药大学 | Epitaxial structure of light emitting diode and preparation method thereof |
-
2008
- 2008-07-04 CN CN200810150272A patent/CN100585895C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2494498C2 (en) * | 2011-02-24 | 2013-09-27 | Юрий Георгиевич Шретер | Semiconductor light-emitting device |
| CN106601784A (en) * | 2015-10-15 | 2017-04-26 | 比亚迪股份有限公司 | Substrate and substrate formation method |
| CN105355741A (en) * | 2015-11-02 | 2016-02-24 | 厦门市三安光电科技有限公司 | LED epitaxial structure and making method thereof |
| CN110098292A (en) * | 2019-03-06 | 2019-08-06 | 西安电子科技大学 | Bluish-green light emitting diode with quantum dots and preparation method based on nano graph |
| CN110098292B (en) * | 2019-03-06 | 2022-04-29 | 西安电子科技大学 | Blue-green quantum dot light-emitting diode based on nano-pattern and preparation method thereof |
| CN112397618A (en) * | 2020-11-27 | 2021-02-23 | 安徽中医药大学 | Epitaxial structure of light emitting diode and preparation method thereof |
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