CN100563036C - A kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency - Google Patents
A kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency Download PDFInfo
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- CN100563036C CN100563036C CNB2007101186328A CN200710118632A CN100563036C CN 100563036 C CN100563036 C CN 100563036C CN B2007101186328 A CNB2007101186328 A CN B2007101186328A CN 200710118632 A CN200710118632 A CN 200710118632A CN 100563036 C CN100563036 C CN 100563036C
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Abstract
A kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency comprises: deposit layer of silicon dioxide film on Sapphire Substrate; Make the photoresist graphic array by lithography; Make mask with the photoresist graphic array, etch silicon dioxide film with graphic structure; With silicon dioxide film with graphic structure as mask, the etching Sapphire Substrate, with pattern etching on Sapphire Substrate; Sapphire Substrate is cleaned up; Forming cross section is leg-of-mutton pyramid structure; Growing low temperature nucleating layer on the graphical sapphire substrate; On the low temperature nucleating layer, continue the GaN layer that the elevated temperature growing n-type mixes, grow low-dislocation-density and surface and have V-arrangement hole array structure; The multiple quantum well layer that continued growth LED structural material is required and the p section bar bed of material, and make final surface still have V-arrangement hole array structure.
Description
Technical field
The invention belongs to technical field of semiconductors, be meant a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency especially.This method can improve the interior quantum luminous efficiency and the light extraction efficiency of GaN base LED material effectively.
Background technology
Light-emitting diode (LED) is a kind of junction type electroluminescence semiconductor device that can convert the electrical signal to light signal.Advantages such as the basic LED of gallium nitride (GaN) is just efficient with it once occurring as solid state light emitter, long-life, environmental protection, be described as the revolution second time on human illumination history behind Edison's invention electric light, become the focus that semiconductor and lighting field research and development and industry are in the world paid close attention to.But GaN base LED enters the general illumination field at present, also faces many difficult problems on technology and cost, needs further to improve interior quantum luminous efficiency and the light extraction efficiency of LED.
Sapphire Substrate is that nitride carries out one of heteroepitaxial growth substrate the most commonly used at present.Because Sapphire Substrate and nitride epitaxial interlayer exist very macrolattice constant mismatch and thermal expansion coefficient difference, therefore there are very big residual stress and many crystal defects in the nitride epitaxial layer, influence the crystal mass of material, limited the further raising of device photoelectric performance.Simultaneously, have the difference of bigger refractive index between GaN and air, the angle of emergence of light is very little, and the overwhelming majority is got back to the LED device inside again by total reflection, and this has not only reduced the extraction efficiency of light but also has increased the heat radiation difficulty, has influenced the stability of LED device.Adopt the graphic sapphire substrate technology can alleviate in the heteroepitaxial growth Sapphire Substrate and nitride epitaxial layer because the stress that lattice mismatch causes, make it to obtain effective relaxation, reduce the dislocation density in the nitride material greatly, improve the internal quantum efficiency of device.Simultaneously, in order to improve the light extraction efficiency of GaN base LED, people have also carried out many-sided research, as adopting the coarse surface method, adopting photon crystal structure etc.In order more effectively to improve the luminous efficiency of LED, the Sapphire Substrate pattern technology that development cost is low, be easy to realize and the device architecture of highlight extract efficiency are imperative.
Summary of the invention
The objective of the invention is to, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency is provided, this method can reduce the dislocation density in the GaN base LED material effectively, avoid the generation of crackle, improve the crystal mass and the uniformity of epitaxial material, and then can improve the interior quantum luminous efficiency of LED, owing to adopted its surperficial V-arrangement hole array structure of processing method of specific substrate can strengthen the light extraction efficiency of GaN base LED effectively.This graphic sapphire substrate technology has also that technology is simple, cost is low and can avoid advantages such as lens lesion.
The invention provides a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency, it is characterized in that, comprise the steps:
Step 1: deposit layer of silicon dioxide film on Sapphire Substrate;
Step 2: utilize photoetching technique to prepare the photoresist graphic array, its graphic element is circular;
Step 3: make mask with the photoresist graphic array, utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches the silicon dioxide film with graphic structure;
Step 4: as mask, utilize the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with silicon dioxide film with graphic structure, with pattern etching on Sapphire Substrate;
Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film, and Sapphire Substrate is cleaned up;
Step 6: continue with sulfuric acid and phosphoric acid mixed liquor wet etching Sapphire Substrate, forming cross section is leg-of-mutton pyramid structure;
Step 7: utilize organic chemical vapor deposition method growing low temperature nucleating layer on the graphical sapphire substrate;
Step 8: continue the GaN layer that the elevated temperature growing n-type mixes on the low temperature nucleating layer, the control growing condition grows low-dislocation-density and surface and has V-arrangement hole array structure;
Step 9: the required multiple quantum well layer and the p section bar bed of material of continued growth LED structural material on n type GaN layer with V-arrangement hole array structure, and make final surface still have V-arrangement hole array structure.
The thickness of wherein said silicon dioxide film is 20 nanometers-2 micron.
The photoresist graphic array of wherein said circle, the size of graphic element and spacing are 0.5 micron-10 microns.
Wherein said sulfuric acid and phosphoric acid mixeding liquid volume ratio are 1: 3-3: 1.
The temperature of wherein said wet etching is between 320 ℃-520 ℃, and the time of etching is 30 seconds-30 minutes.
The wherein said time with sulfuric acid and phosphoric acid mixed liquor wet etching Sapphire Substrate is that 30s is to 5min.
The growth temperature of wherein said growing low temperature nucleating layer is 400 ℃ to 600 ℃.
The thickness of wherein said low temperature nucleating layer is that 10 nanometers are to 100 nanometers;
Wherein said multiple quantum well layer with V-arrangement hole structure is In
xGa
1-xN/GaN, In
xGa
1-xN/In
yGa
1-yN, Al
xIn
1-xGaN/GaN, Al
xIn
1-xGaN/Al
yGa
1-yN, GaN/Al
xGa
1-xN or Al
xGa
1-xN/Al
yGa
1-yOne or more combination among the N.
A kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency provided by the invention, this method can reduce the dislocation density in the GaN base LED material effectively, avoid the generation of crackle, improve the crystal mass and the uniformity of epitaxial material, and then can improve the interior quantum luminous efficiency of LED, owing to adopted its surperficial V-arrangement hole array structure of processing method of specific substrate can strengthen the light extraction efficiency of GaN base LED effectively.This graphic sapphire substrate technology has also that technology is simple, cost is low and can avoid advantages such as lens lesion.
Description of drawings
In order to further specify content of the present invention, below in conjunction with the example of implementing the present invention is done a detailed description, wherein:
Fig. 1 is the structural section schematic diagram behind the Sapphire Substrate litho pattern; Wherein 1 is Sapphire Substrate, and 2 is silicon dioxide film, and 3 is the photoresist graphic array;
Fig. 2 is to be mask with photoresist graphic array 3, utilizes hydrofluoric acid+ammonium fluoride+H
2Schematic cross-section behind the O mixed liquor etching silicon dioxide film 2; Wherein 1 is Sapphire Substrate, and 2 is the figure silicon dioxide film after the etching, the 3rd, and the photoresist graphic array;
Fig. 3 utilizes the silicon dioxide film 2 of graphic structure to be mask, adopts sulfuric acid and phosphoric acid to mix (volume ratio 3: 1) wet etching Sapphire Substrate 1, with the generalized section of pattern etching after the Sapphire Substrate; Wherein 1 is patterned Sapphire Substrate, the 2nd, and silicon dioxide film;
Fig. 4 is that the diluted hydrofluoric acid wet etching removes remaining silicon dioxide film 1, and the generalized section after Sapphire Substrate 1 cleaned up; Wherein 1 is the patterned sapphire substrate;
Fig. 5 is the Sapphire Substrate 1 that continues with the mixed liquor wet etching graphic structure of sulfuric acid and phosphoric acid, and forming cross section is leg-of-mutton pyramid structure.Wherein 1 is patterned Sapphire Substrate;
Fig. 6 is a growing low temperature nucleating layer 4 on sapphire graphical substrate 1, and the low-dislocation-density of high growth temperature and surface have the n type GaN layer 5 of V-arrangement hole array structure; Wherein 1 is patterned Sapphire Substrate, and 4 is the low temperature nucleating layer, and 5 for having the n type GaN layer of V-arrangement hole array structure;
Fig. 7 is the multiple quantum well layer 6 and the p type GaN layer 7 of continued growth on the n type GaN layer 5 with V-arrangement hole array structure, and the surface also has V-arrangement hole array structure.Wherein 1 is the patterned sapphire substrate, and 4 is the low temperature nucleating layer, and 5 is n type GaN layer, and 6 is multiple quantum well layer, and 7 are surperficial p type GaN layer with V-arrangement hole structure.
Embodiment
See also Fig. 1-shown in Figure 7, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency of the present invention comprises the steps:
Step 1: deposit layer of silicon dioxide film 2 (consulting Fig. 1) on Sapphire Substrate 1, the thickness of this silicon dioxide film 2 are 20 nanometers-2 micron;
Step 2: utilize photoetching technique to prepare photoresist graphic array 3, its graphic element is circular, the photoresist graphic array 3 that this is circular, and the size of graphic element and spacing are 0.5 micron-10 microns;
Step 3: make mask with photoresist graphic array 3, utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches the silicon dioxide film 2 (consulting Fig. 2) with graphic structure;
Step 4: with silicon dioxide film 2 with graphic structure as mask, utilize the mixed liquor wet etching Sapphire Substrate 1 (consulting Fig. 3) of sulfuric acid and phosphoric acid, with pattern etching on Sapphire Substrate 1, this sulfuric acid and phosphoric acid mixeding liquid volume ratio are 1: 3-3: 1, the temperature of this wet etching is between 320 ℃-520 ℃, and the time of etching is 30 seconds-30 minutes;
Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film 2, and Sapphire Substrate 1 is cleaned up (consulting Fig. 4);
Step 6: continue with sulfuric acid and phosphoric acid mixed liquor wet etching Sapphire Substrate 1, the time be 30s to 5min, forming cross section is leg-of-mutton pyramid structure (consulting Fig. 5);
Step 7: utilize organic chemical vapor deposition method growing low temperature nucleating layer 4 on graphical sapphire substrate 1, growth temperature is 400 ℃ to 600 ℃, and thickness is that 10 nanometers are to 100 nanometers (consulting Fig. 6);
Step 8: continue the GaN layer 5 that the elevated temperature growing n-type mixes on low temperature nucleating layer 4, the control growing condition grows low-dislocation-density and surface and has V-arrangement hole array structure;
Step 9: the required multiple quantum well layer 6 and the p section bar bed of material 7 (consulting Fig. 7) of continued growth LED structural material on n type GaN layer 5 with V-arrangement hole array structure, and make final surface still have V-arrangement hole array structure.
Wherein said multiple quantum well layer 6 with V-arrangement hole structure is In
xGa
1-xN/GaN, In
xGa
1-xN/In
yGa
1-yN, Al
xIn
1-xGaN/GaN, Al
xIn
1-xGaN/Al
yGa
1-yN, GaN/Al
xGa
1-xN or Al
xGa
1-xN/Al
yGa
1-yOne or more combination among the N.
Further set forth technical characterstic of the present invention and obvious improvement below by specific embodiment.
Present embodiment is a kind of manufacture method of utilizing the graphical sapphire substrate to improve GaN base LED luminous efficiency.
The silicon dioxide film 2 of 0.3 micron of using plasma chemical gas-phase deposition enhanced (PECVD) deposition techniques on 2 inches c surface sapphire substrate 1 at first, utilize the photoresist graphic array 3 of conventional photoetching technique fabrication cycle then, graphic element is circular, diameter and spacing are 3 microns, and the structural profile after the photoetching as shown in Figure 1;
Then make mask, utilize hydrofluoric acid+ammonium fluoride+H with photoresist graphic array 3
2The O mixed liquor etches into litho pattern array 3 on the silicon dioxide film 2, and structural profile as shown in Figure 2;
Utilize diluted hydrofluoric acid that silicon dioxide film 2 wet etchings of remnants are removed, structural profile as shown in Figure 4;
Continue the Sapphire Substrate 1 with mixed liquor (volume ratio 3: 1) wet etching graphic structure under 400 degree of sulfuric acid and phosphoric acid, make it the graphic array that the surface forms pyramid shape, structural profile as shown in Figure 5;
Utilize MOCVD equipment (P125 of VEECO company type business PC) growing low temperature GaN nucleating layer 4 on patterned Sapphire Substrate 1, and then high growth temperature low-dislocation-density and surperficial n type GaN layer 5 with V-arrangement hole array structure, structural profile is as shown in Figure 6;
Continued growth In0.2Ga0.8N/GaN Multiple Quantum Well 6 and p type GaN layer 7 on the n type GaN layer 5 with V-arrangement hole array structure, final surface also have V-arrangement hole array structure, and structural profile as shown in Figure 7;
The graphic element of the c surface sapphire substrate 1 after the etching is a mesa structure, and table surface height is 1.3 microns.Because the anisotropy of wet etching, cross section is a triangle, and the side is nearly equilateral triangle structure, by { 1 1-2 0}, { 211 0} and { 1-2 1 0} crystal face formation.
The foregoing description has been described the method for utilizing the graphic sapphire substrate to improve GaN base LED luminous efficiency.Because substrate etching technology does not relate to dry etching processes such as RIE or ICP, therefore the graphical sapphire substrate 1 of preparation can avoid the dry etching damage.Simultaneously, the V-arrangement hole array that GaN base LED device architecture surface forms can improve the light extraction efficiency of LED effectively, thereby can further improve the luminous efficiency of GaN base LED.
Claims (6)
1, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency is characterized in that, comprises the steps:
Step 1: deposit layer of silicon dioxide film on Sapphire Substrate;
Step 2: utilize photoetching technique to prepare the photoresist graphic array, its graphic element is circular;
Step 3: make mask with the photoresist graphic array, utilize hydrofluoric acid+ammonium fluoride+H
2The O mixed liquor etches the silicon dioxide film with graphic structure;
Step 4: as mask, utilize the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with silicon dioxide film with graphic structure, with pattern etching on Sapphire Substrate;
Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film, and Sapphire Substrate is cleaned up;
Step 6: continue with sulfuric acid and phosphoric acid mixed liquor wet etching Sapphire Substrate, forming cross section is leg-of-mutton pyramid structure;
Step 7: utilize organic chemical vapor deposition method growing low temperature nucleating layer on the graphical sapphire substrate;
Step 8: continue the GaN layer that the elevated temperature growing n-type mixes on the low temperature nucleating layer, the control growing condition grows low-dislocation-density and surface and has V-arrangement hole array structure;
Step 9: the required multiple quantum well layer and the p section bar bed of material of continued growth LED structural material on n type GaN layer with V-arrangement hole array structure, and make final surface still have V-arrangement hole array structure.
2, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency according to claim 1 is characterized in that the thickness of wherein said silicon dioxide film is 0.3 micron.
3, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency according to claim 1 is characterized in that, the photoresist graphic array of wherein said circle, and the size of graphic element and spacing are 3 microns.
4, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency according to claim 1 is characterized in that wherein said sulfuric acid and phosphoric acid mixeding liquid volume ratio are 3: 1.
5, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency according to claim 1 is characterized in that the temperature of wherein said wet etching is at 400 ℃, and the time of etching is 10 minutes.
6, a kind of method of utilizing patterned substrate to improve GaN base LED luminous efficiency according to claim 1 is characterized in that, wherein said multiple quantum well layer with V-arrangement hole structure is In
xGa
1-xN/GaN.
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| TWI475726B (en) * | 2012-05-09 | 2015-03-01 | Phostek Inc | Light-emitting diode and a method of manufacturing the same |
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| JP2001257166A (en) * | 2000-03-13 | 2001-09-21 | Nippon Telegr & Teleph Corp <Ntt> | Nitride semiconductor substrate and its manufacturing method |
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| TWI475726B (en) * | 2012-05-09 | 2015-03-01 | Phostek Inc | Light-emitting diode and a method of manufacturing the same |
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