CN101702419A - Surface roughening method of p-GaN layer or ITO layer in GaN-based LED chip structure - Google Patents
Surface roughening method of p-GaN layer or ITO layer in GaN-based LED chip structure Download PDFInfo
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Abstract
The invention discloses a surface roughening method of a p-GaN layer or an ITO layer in a GaN-based LED chip structure. The method comprises the following steps: (1) growing a low-temperature GaN buffer layer, an undoped GaN layer, an n-GaN layer, a multiple quantum well layer, a stack-up structure of the p-GaN layer and an extended layer evaporating ITO current on a semiconductor substrate in sequence; and (2) preparing monolayer nickel nano particles as a mask, and preparing a roughening structure on the p-GaN layer or the ITO layer. The method of the invention has simple steps, low cost, good roughening effect; by carrying out surface roughening on the p-GaN layer or the ITO layer of the GaN-based LED by the method of the invention, the total reflection of the photon in the chip can be inhibited and the light outgoing efficiency of the devices can be improved.
Description
Technical field
The present invention relates to the photoelectric device field, be specifically related to the method for coarsening surface of p-GaN layer in a kind of GaN based LED chip structure or ITO layer.
Background technology
In recent years, light-emitting diode (LED) becomes one of the most valued light source technology undoubtedly.LED has the little characteristic of volume on the one hand; LED possesses the electricity-saving characteristic of low current, low voltage drive on the other hand.Estimate that in theory the luminous efficiency of semiconductor LED illuminating lamp can meet or exceed 10 times of incandescent lamp, 2 times of fluorescent lamp.Simultaneously it also to have sound construction, shock resistance and shock resistance strong; Extra long life can reach 100000 hours; No infrared ray and ultraviolet radiation; No mercury helps numerous advantages such as environmental protection.Wherein, as in one of main application of optoelectronic areas, the GaN sill has obtained more and more people's concern, utilizes the GaN base semiconductor material can produce super brightness indigo plant, green, white light emitting diode.Because the brightness of GaN based light-emitting diode has obtained very big raising, make the GaN based light-emitting diode all obtain application in a lot of fields, for example traffic lights, mobile phone are backlight, automobile tail light, short haul connection, photoelectricity computer are interconnected etc.May then will cause the revolution of Lighting Industry in the near future as the GaN base white light LEDs of energy-saving and environmental protection ligthing paraphernalia especially, boundless application prospect is arranged, in a single day semiconductor lighting becomes a reality, and its meaning is not second to Edison's invention incandescent lamp.Based on the important function of GaN base LED, the luminous efficiency that how to improve GaN base LED has become the focus of concern.Suddenly wait to develop reliable method improves luminous power to the researcher, thereby increases substantially the class of LED product, increases economic efficiency.Under the standard operation electric current of 20mA, the luminous power of typical GaN base blue led chip is about 4mW at present, and many manufacturers start with from the raising external quantum efficiency and improve luminous power, can make luminous power more than 4.5mW.Early stage LED assembly development concentrates on and promotes its internal quantum, development along with growth technology and multi-quantum pit structure, the internal quantum efficiency of superhigh brightness LED has had very large improvement, the LED internal quantum efficiency of blue light GaN base can reach more than 70% at present, ultraviolet GaN base LED can reach 80%, and further the space of improving is less.
The photoelectric conversion efficiency of semi-conducting material itself far exceeds other illuminating source, the external quantum efficiency that improves GaN base LED is significant to the development and application that promotes LED, under the situation in view of the almost approaching theoretical limit of the raising of present its internal quantum, the light that promotes the LED assembly takes out efficient will become important problem.This requires to design new chip structure to a great extent and improves chip light-emitting efficiency, and then reach the purpose that promotes luminous efficiency (or external quantum efficiency), the high-power chip technology also just is absorbed in how to be lifted out the luminous efficiency that optical efficiency promotes chip, and the major technique approach that adopts both at home and abroad mainly contains at present: growth distribution bragg reflection layer (DBR) structure, flip chip technology, surface coarsening technology and photonic crystal technology.Wherein the surface coarsening technology is generally had an optimistic view of as the simple relatively technology of a kind of manufacture craft, and it does not need to make the strict physical dimension as photonic crystal, and manufacture method is also more.Usually common GaN base LED chip manufacture craft is the stacked structure of n-GaN layer, multiple quantum well layer and p-GaN layer of growing successively on Sapphire Substrate, then deposits the ITO current-diffusion layer, produces metal electrode then.Because the refractive index of GaN material and ito thin film is about 2.5 and 2.1, than big many of the refractive index of surrounding air, total reflection phenomenon will take place in the photon that produces at active layer through p-GaN and ITO interface and ITO and air interface the time like this, causes most of light to be folded back and can not appear device surface.By surface coarsening, can destroy the total reflection behavior of photon, increase the probability that photon is escaped from device surface, thereby improve luminous efficiency.
In the method for coarsening surface that has proposed at present, though all raising in various degree LED brightness, yet specification requirement height, process that these methods also expose wayward, shortcoming such as forward bias rising can appear.Therefore, be necessary to work out that a kind of manufacture craft is simple relatively, cost is low, be convenient to the method for coarsening surface that industrialization is produced.
Summary of the invention
The objective of the invention is to the deficiency according to existing surface coarsening technology, provide a kind of manufacture craft simple relatively, cost is low, the method for coarsening surface that alligatoring is effective.
The present invention is achieved by the following technical programs:
The method for coarsening surface of p-GaN layer or ITO layer is characterized in that comprising the steps: in a kind of GaN based LED chip structure
(1) growing low temperature GaN resilient coating, the GaN layer that undopes, n-GaN layer, multiple quantum well layer, p-GaN layer and evaporation ITO current extending successively on Semiconductor substrate;
(2) preparation individual layer nickel nano particle is made the alligatoring structure as mask at p-GaN layer or ITO laminar surface.
Wherein, the preferred sapphire of material, silicon or the SiC of the Semiconductor substrate in the described step (1).
The preparation method of individual layer nickel nano particle mask is as follows described in the step (2):
1. dispose the nickel nano particle dispersion liquid: with the diameter of 1～20wt% is that the nano-nickel powder of 50nm～200nm is dissolved in absolute ethyl alcohol, adds dispersant, and mixed liquor is carried out ultrasonic dispersion treatment 8～30min;
2. the spin coating of nickel nano particle dispersion liquid: above-mentioned nanometer nickel particles dispersion liquid is spin-coated on p-GaN layer or the ITO laminar surface, forms individual layer nickel nano particle film;
3. the oven dry of individual layer nickel nano particle film: have the epitaxial wafer sample of individual layer nickel nano particle to dry spin coating, form the required individual layer nickel nano particle mask layer of ICP etching.
Wherein, preferred oleic acid of described dispersant or citric acid.
The preferred self-assembled monolayer nickel nano particle of described individual layer nickel nano particle mask mask.
In order to make the suspendability of nickel nano particle in dispersant better, described nickel nano particle is preferred non-oxide nickel nano particle before the configuration dispersion liquid, so need carry out following processing: with watery hydrochloric acid with react after nano-nickel powder mixes by mass ratio at 5: 1, leave standstill 20min behind the sonic oscillation 30min, outwell supernatant liquor, and cyclic washing to pH value is 6～7.
When roughening treatment is carried out on the p-GaN surface, in the ICP etching process, preferably use Cl
2/ BCl
3/ Ar is as etching gas, and etching condition is preferably: BCl
3Flow be 2～15sccm, the flow of Ar is 5～30sccm, Cl
2Flow be 110～35sccm, ICP power is 500～750W, RF power is 100～300W, etch period is 10s～1min, forms concavo-convex pattern at the p-GaN laminar surface after the etching; Sample after the etching is put into ethanolic solution, and ultrasonic cleaning is removed the nickel nano particle mask and rinse well.
When the ITO current extending is carried out roughening treatment, in the ICP etching process, preferably use Cl
2/ BCl
3/ Ar or Cl
2/ Ar is as etching gas, and etching condition is preferably: BCl
3Flow be 5～10sccm, the flow of Ar is 2～15sccm, Cl
2Flow be 25～60sccm, ICP power is 200～500W, RF power is 100～350W, etch period is 1～4min, forms concavo-convex pattern at ITO current expansion laminar surface after the etching; Sample after the etching is put into ethanolic solution, and ultrasonic cleaning is removed the nickel nano particle mask and rinse well.
In the above-mentioned ICP etching process, can control the degree of roughness of p-GaN layer or ITO current extending by the time of ICP etching processing, during particularly to the alligatoring of p-GaN layer, in order to bring into play the photoelectric characteristic of device, etching depth is no more than the 1/2 preferable of p-GaN layer thickness.
In the surface coarsening process of p-GaN layer or ITO layer, growing epitaxial is the common technology in this area on Semiconductor substrate in the GaN based LED chip structure.
Compared with prior art, the present invention has following beneficial effect:
The method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure of the present invention, by alligatoring with p-GaN layer or ITO layer, destroyed the reflex that photon takes place through p-GaN and ITO interface and ITO and air interface the time, increase photon and escaped from the probability of device surface, improved luminous efficiency.The inventive method process is easy to control, and manufacture craft is simple relatively, and cost is low, and process is controlled easily, is convenient to industrialization production.
Description of drawings
Fig. 1 is the structural representation of conventional GaN base LED, and wherein, 1 is the P electrode, and 2 is the ITO layer, and 3 is the p-GaN layer, and 4 is quantum well, and 5 is the N electrode, and 6 is the n-GaN layer, and 7 are the GaN layer that undopes, and 8 is low temperature GaN resilient coating, and 9 is Sapphire Substrate;
Fig. 2 is the structural representation by the GaN base LED that ITO current extending surface coarsening is improved light emission rate, wherein, 1 is the P electrode, and 2 is surface coarsening ITO layer, and 3 is the p-GaN layer, 4 is quantum well, 5 is the N electrode, and 6 is the n-GaN layer, and 7 are the GaN layer that undopes, 8 is low temperature GaN resilient coating, and 9 is Sapphire Substrate;
Fig. 3 is the structural representation that improves the GaN base LED of light emission rate by the alligatoring of p-GaN laminar surface, and wherein, 1 is the P electrode, and 2 is the ITO layer, 3 is surface coarsening p-GaN layer, and 4 is quantum well, and 5 is the N electrode, and 6 is the n-GaN layer, 7 are the GaN layer that undopes, and 8 is low temperature GaN resilient coating, and 9 is Sapphire Substrate;
Fig. 4 is by alligatoring simultaneously improves the structural representation of the GaN base LED of light emission rate to p-GaN layer and ITO current extending, wherein, 1 is the P electrode, and 2 is surface coarsening ITO layer, and 3 is surface coarsening p-GaN layer, 4 is quantum well, 5 is the N electrode, and 6 is the n-GaN layer, and 7 are the GaN layer that undopes, 8 is low temperature GaN resilient coating, and 9 is Sapphire Substrate;
Fig. 5 is the GaN base LED and the common GaN base LED current-voltage correlation correlation curve of ITO current-diffusion layer surface coarsening;
Fig. 6 is the GaN base LED and the common GaN base LED luminous intensity correlation curve of ITO current extending surface coarsening.
Embodiment
Further explain the present invention below in conjunction with embodiment, but embodiment does not do any qualification to the present invention.
The method that improves the LED light emission rate by alligatoring ITO current expansion laminar surface mainly may further comprise the steps:
(1) adopt that metal-organic chemical vapor deposition equipment method (MOCVD) grows low temperature GaN resilient coating successively on Semiconductor substrate, the stacked structure of the GaN layer that undopes, n-GaN layer, multiple quantum well layer, p-GaN layer and evaporation ITO layer.Wherein the material of Semiconductor substrate is a sapphire;
(2) epitaxial wafer that grows is carried out MESA photoetching and ICP etching, GaN comes out up to the n type;
(3) adopt means of electron beam deposition depositing one deck ito thin film as current extending on the substrate after the MESA photoetching, the thickness of film is 350nm;
(4) take by weighing 3g nanometer nickel particles in 30mL ethanol, add the 0.6g citric acid, ultrasonic dispersion 15min.If nickel nano particle surface oxidation before the dispersion liquid preparation, then the oxide on surface to be removed earlier, concrete operations are watery hydrochloric acid (1: 10) and nano-nickel powder to be put into beaker with mass ratio at 5: 1 react, adopt supersonic wave cleaning machine sonic oscillation 30min, 20min is left standstill in the failure of oscillations then, outwells supernatant liquor, and be 6～7 with deionized water wash to pH value repeatedly, and then carry out dispersion experiment;
(5) the nanometer nickel particles dispersion liquid that the prepares speed with 3800rpm is spin-coated on the ITO surface, the spin coating time is 60s, then substrate 120 ℃ of baking 30min in the baking oven of nitrogen protection is formed the individual layer nickel nano particles;
(6) the ICP photoetching treatment is carried out on the ITO surface that will be covered with individual layer nickel nano particle mask, selects Cl
2/ Ar is as the etching plasma gas, and etching condition is: the flow of Ar is 5sccm, Cl
2Flow be 35sccm, ICP power is 350W, RF power is 150W, etch period is 180s, forms the alligatoring structure on ITO surface after the etching, then the substrate after the ICP etching is put into the ethanolic solution ultrasonic cleaning, the removal nickel nano particle;
(7) metal electrode is made: on the basis that forms ITO current-diffusion layer surface coarsening, the LED technology for preparing electrode by routine forms required electrode (Fig. 2), and wherein electrode material is Cr/Ni/Au (5nm/20nm/1000nm).
(8) Fig. 5 and Fig. 6 represent the current-voltage characteristic curve of prepared GaN base LED and the characteristic curve of luminous intensity-electric current, and the LED luminous strength ratio ITO laminar surface that the result shows the alligatoring of the ITO laminar surface not LED of alligatoring improves more than 30%.
The method that improves GaN base LED light emission rate by alligatoring p-GaN laminar surface mainly may further comprise the steps:
(1) adopt that metal-organic chemical vapor deposition equipment method (MOCVD) grows low temperature GaN resilient coating successively on Semiconductor substrate, the stacked structure of the GaN layer that undopes, n-GaN layer, multiple quantum well layer, p-GaN layer and evaporation ITO layer.Wherein, the p-GaN layer is made of 10nm thick p-GaN layer and the thick magnesium p type GaN layer of mixing of 180nm, and the material of Semiconductor substrate is a silicon;
(2) take by weighing 3g nanometer nickel particles in 30mL ethanol, add 0.6g oleic acid, ultrasonic dispersion 10min.Before the dispersion liquid preparation deoxidation being carried out on the nickel nano particle surface handles, the oxide on surface that is about to nano-nickel powder is removed, concrete operations are watery hydrochloric acid (1: 10) and nano-nickel powder to be put into beaker with mass ratio at 5: 1 react, adopt supersonic wave cleaning machine sonic oscillation 30min, 20min is left standstill in the failure of oscillations then, outwells supernatant liquor, and be 6～7 with deionized water wash to pH value repeatedly, and then carry out the dispersion liquid preparation;
(3) the nanometer nickel particles dispersion liquid that the prepares speed with 4000rpm is spin-coated on the p-GaN laminar surface, the spin coating time is 50s, then substrate 120 ℃ of bakings in the baking oven of nitrogen protection is formed individual layer nickel nano particle mask in 30 minutes;
(4) the p-GaN laminar surface that will be covered with individual layer nickel nano particle mask carries out the ICP etching processing, select Cl2/BCl3/Ar as the etching plasma gas, etching condition is: the flow of Cl2 is 15sccm, and the flow of BCl3 is 5sccm, and the flow of Ar is 10sccm, ICP power is 550W, RF power is 150W, and etch period is 30s, forms the alligatoring structure on the p-GaN surface after the etching, then the substrate after the ICP etching is put into the ethanolic solution ultrasonic cleaning, remove nickel nano particle;
(2) substrate to p-GaN laminar surface alligatoring carries out MESA photoetching and ICP etching, and GaN comes out up to the n type;
(3) adopting means of electron beam deposition is that the ito thin film of 250nm is as current extending at deposition one layer thickness on the substrate after MESA photoetching and the ICP etching;
(7) metal electrode is made: on the basis that forms the alligatoring of p-GaN laminar surface, the LED metal electrode preparation technology by routine forms required electrode, and wherein electrode material is Cr/Ni/Au (5nm/20nm/1000nm).
(8) structural representation of the GaN of p-GaN laminar surface alligatoring base LED as shown in Figure 3.
In sum, the present invention by the surface coarsening to ITO current-diffusion layer or p-GaN layer can improve GaN base LED luminous intensity.Coarsening process adopts the ICP dry etching technology, and with the individual layer nickel nano particle of self assembly as mask.Use this method also can obtain the structure (Fig. 4) of p-GaN layer and the alligatoring simultaneously of ITO current extending simultaneously, the result can make the photon of more multiple active layers generation escape from chip surface, reaches the purpose that improves the LED luminous efficiency.
Claims (9)
1. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure is characterized in that comprising the steps:
(1) growing low temperature GaN resilient coating, the GaN layer that undopes, n-GaN layer, multiple quantum well layer, p-GaN layer and evaporation ITO current extending successively on Semiconductor substrate;
(2) preparation individual layer nickel nano particle is made the alligatoring structure as mask at p-GaN layer or ITO laminar surface.
2. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 1, the material that it is characterized in that Semiconductor substrate described in the step (1) is sapphire, silicon or SiC.
3. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 1 is characterized in that the preparation method of individual layer nickel nano particle mask described in the step (2) is as follows:
(1) configuration nickel nano particle dispersion liquid: with the diameter of 1～20wt% is that the nano-nickel powder of 50nm～200nm is dissolved in absolute ethyl alcohol, adds dispersant, and mixed liquor is carried out ultrasonic dispersion treatment 8～30min;
(2) spin coating of nickel nano particle dispersion liquid: above-mentioned nanometer nickel particles dispersion liquid is spin-coated on p-GaN layer or the ITO laminar surface, forms individual layer nickel nano particle film;
(3) oven dry of individual layer nickel nano particle film: have the epitaxial wafer sample of individual layer nickel nano particle to dry spin coating, form the required individual layer nickel nano particle mask layer of ICP etching.
4. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 3 is characterized in that dispersant is oleic acid or citric acid described in the step (1).
5. according to the method for coarsening surface of p-GaN layer or ITO layer in claim 1 or the 3 described GaN based LED chip structures, it is characterized in that described individual layer nickel nano particle mask is a self-assembled monolayer nickel nano particle mask.
6. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 3, it is characterized in that described nano-nickel powder is non-oxide, need carry out following processing in preparation before the dispersion liquid: with watery hydrochloric acid with react after nano-nickel powder mixes by mass ratio at 5: 1, leave standstill 20min behind the sonic oscillation 30min, outwell supernatant liquor, and cyclic washing to pH value is 6～7.
7. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 1 is characterized in that described step is used Cl in (2) when the p-GaN layer being carried out the surface coarsening processing
2/ BCl
3/ Ar is as etching gas, and etching condition is: BCl
3Flow be 2～15sccm, the flow of Ar is 5～30sccm, Cl
2Flow be 110～35sccm, ICP power is 500～750W, RF power is 100～300W, etch period is 10s～1min, forms concavo-convex pattern at the p-GaN laminar surface after the etching.
8. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 1 is characterized in that described step is used Cl in (2) when the ITO layer being carried out the surface coarsening processing
2/ BCl
3/ Ar or Cl
2/ Ar is as etching gas, and etching condition is: BCl
3Flow be 5～10sccm, the flow of Ar is 2～15sccm, Cl
2Flow be 25～60sccm, ICP power is 200～500W, RF power is 100～350W, etch period is 1～4min, forms concavo-convex pattern at ITO current expansion laminar surface after the etching.
9. the method for coarsening surface of p-GaN layer or ITO layer in the GaN based LED chip structure according to claim 7, when it is characterized in that the p-GaN layer carried out surface coarsening, the degree of depth of described etching is no more than 1/2 of p-GaN layer thickness.
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2009
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