CN101771115A - Method for treating nitrogen surface after laser lift-off of gallium nitride-based material - Google Patents
Method for treating nitrogen surface after laser lift-off of gallium nitride-based material Download PDFInfo
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- CN101771115A CN101771115A CN200910076039A CN200910076039A CN101771115A CN 101771115 A CN101771115 A CN 101771115A CN 200910076039 A CN200910076039 A CN 200910076039A CN 200910076039 A CN200910076039 A CN 200910076039A CN 101771115 A CN101771115 A CN 101771115A
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Abstract
The invention provides a method for treating a nitrogen surface after laser lift-off of gallium nitride-based material, comprising the following steps of removing metal gallium by soaking in hydrochloric acid solution; ICP (Inductively Coupled Plasma) pretreatment in reaction atmosphere of nitrogen gas or inert gas; ICP treatment in reaction atmosphere of chlorine gas, silicon tetrachloride and argon gas; and ICP post-treatment in reaction atmosphere of oxygen gas and trifluoromethane. The method is used for treating an N surface of a GaN LBD with a film flip structure, a vertical injection structure or a self-supporting vertical structure after laser lift-off, overcomes the defects of a wet etching method and a chemical mechanical polishing method, is suitable for mass production without side effects, and solves the problem of reduction of light extraction efficiency of an untreated surface.
Description
Technical field
The present invention relates to the processing method of gallium nitride in the field of photoelectric technology (GaN) sill (comprising the GaN light-emitting diode) nitrogen surface after laser lift-off.
Background technology
Laser lift-off is the key technology of making film inverted structure (Thin-Film Flip-Chip) and vertical injecting structure (Vertical InjectionStructure) and self-supporting (Free Standing) vertical stratification GaN light-emitting diode (LED).The suitable laser of condition such as one beam energy simultaneously shine the GaN sill that is grown on the sapphire from sapphire, because the crystalline quality of the nucleating layer GaN of grow first on sapphire is relatively poor, just can resolve into Ga and N under the irradiation of laser
2Thereby, GaN and sapphire are separated, this is a laser lift-off technique.W.S.Wong at first utilized laser lift-off successfully to prepare with film GaN (W.S.Wong, T.Sands, the and N.W.Cheung of adhering with epoxy resin on silicon chip in 1997, Appl.Phys.Lett.72,599. (1998) .), and prepared successful film GaN LED (W.S.Wong in 1999, M.Kneissl, D.P.Bour, P.Mei, L.T.Romano, N.M.Johnson, N.W.Cheung, and T.Sands, Appl.Phys.Lett.75,1360. (1999)).In the ensuing several years, laser lift-off prepares the film inverted structure and has been in control swift and violent development with vertical injecting structure and self-supporting vertical stratification GaN light-emitting diodes.Present most GaN is grown on (0001) surface sapphire, be (0001) crystal orientation, reason owing to lattice mismatch between six side's symmetry of GaN and GaN and the sapphire, GaN presents spontaneous polarization and piezoelectric polarization, therefore most GaN sills all are certain polarity, on (0001) surface sapphire, the Grown GaN surface be Ga polarity as the present modal MOCVD of utilization equipment, corresponding with it, therefore be N polarity with the contacted GaN face of sapphire, the surface of removing the GaN behind the sapphire through laser lift-off will be N polarity.Because the crystal structure of nucleating layer is second-rate, there is remaining gallium on the surface after process laser emission is peeled off, and very coarse, and a lot of holes is arranged, and can seriously reduce light extraction efficiency.Usually the processing method of Ga face GaN has dry etching (ICP), wet etching (KOH solution), chemico-mechanical polishing (CMP).Because the different (E.S.Hellman of N face and Ga face GaN polarity, MRS Internet J.Nitride Semicond.Res.3,11 (1998) .), and N face GaN surface is distinctive coarse because of sustaining damage behind the laser lift-off, the characteristic of porous, feasible dry etching (the S.Tripathy that depends on polarity and surface appearance strongly, A.Ramam, S.J.Chua, J.S.Pan, and Alfred Huan, J.Vac.Sci.Technol.A, 19,2522. (2001)), the N face GaN after to laser lift-off is no longer suitable for the treatment conditions commonly used of wet etching (E.S.Hellman, MRS Intemet J.NitrideSemicond.Res.3,11 (1998) .).Further, the GaN film of laser lift-off normally utilizes intermediate metal to electroplate at copper substrate or key with on Si sheet substrate, and wet etching causes coming off of film easily, and because a large amount of K
+Ion easily remains in the GaN sidewall, causes the electric leakage of LED tube core, reduces the LED quality; GaN film behind the laser lift-off has only several micron thickness, and therefore the polishing uniformity in the restive 2 inches faces of chemico-mechanical polishing is not suitable for large-scale industrialization production.
Therefore, invent a kind of be suitable for large-scale production and also do not have side effects the method handled of N face, making the film inverted structure for laser lift-off is vital with vertical injecting structure and self-supporting vertical stratification GaN light-emitting diode (LED).
Summary of the invention
The objective of the invention is to overcome the deficiency of wet etching and cmp method, a kind of dry process method that is applicable to the N face GaN behind the laser lift-off is provided, solved the problem that untreatment surface reduces light extraction efficiency.
Technical scheme of the present invention is:
The processing method of N face behind a kind of GaN sill laser lift-off, its step comprises:
1) removes gallium with the GaN sill behind the hydrochloric acid solution immersion laser lift-off;
2) ICP (Inductively Coupled Plasma, inductively coupled plasma) preliminary treatment, the surface of the laser lift-off that removal sustains damage: the GaN sill after adopting the ICP plasma to laser lift-off carries out preliminary treatment, wherein, reaction atmosphere is nitrogen or inert gas or their mist; The density of plasma is 10
10Cm
-3-10
11 Cm
-35 minutes to 30 minutes processing time.
3) ICP handles, removing the non-of N face mixes layer and generate the coarse surface that helps improving light extraction efficiency: the GaN sill after adopting the ICP plasma to laser lift-off is handled, wherein, reaction atmosphere is the mist of chlorine, silicon tetrachloride and argon gas, mixed proportion is volume ratio 1: 0.5: 0.05 to 1: 0.05: 0.5, and the density of plasma is 10
12Cm
-3-10
13Cm
-31 minute to 30 minutes processing time.
4) ICP reprocessing, repair of Surface Damage and passivation: the GaN sill after adopting the ICP plasma to laser lift-off carries out reprocessing, and wherein, reaction atmosphere is the mist of oxygen and fluoroform, and mixed proportion is volume ratio 1: 0.25 to 1: 4; The density of plasma is 10
11Cm
-3-10
12 Cm
-35 minutes to 30 minutes processing time.
Above-mentioned steps 1) hydrochloric acid solution in is the mixed solution of 1: 1～1: 10 concentrated hydrochloric acid of volume ratio and water normally, soak time 30 seconds to 5 minutes.
Further, in above-mentioned steps 2) in, the ICP preliminary treatment can be adopted source power 200-300W, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-60sccm.Reaction atmosphere generally is nitrogen or argon gas, or the mist of nitrogen and argon gas, and nitrogen, argon gas mixed volume were than preferred 1: 1.Preferred 20min-30min of processing time.
In above-mentioned steps 3) in, ICP handles can adopt source power 100-500W, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-40sccm.Chlorine, silicon tetrachloride, argon gas mixed volume ratio are preferably 1: 0.1: 0.2 to 1: 0.2: 0.1.Preferred 10min-20min of processing time.
In above-mentioned steps 4) in, the ICP reprocessing can be adopted source power 100-500W, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-80sccm.Oxygen, tetrafluoromethane mixed volume ratio are preferably 1: 0.5 to 1: 2.Preferred 5min-10min of processing time.
Compared with prior art, the invention has the beneficial effects as follows:
1) utilize high density that the ICP preliminary treatment produces, with the GaN hypoergia but inert gas plasmas such as the nitrogen of high bombardment property, argon, helium, remove the gallium nitride of the resilient coating of the laser damage after being peeled off, avoid occurring the nitrogen face light-shielding structure of porous; The N plasma can be repaired the N disappearance that causes owing to laser irradiation simultaneously.
2) utilize ICP to handle the high density that produces, the argon plasma of high response chlorine plasma and hypoergia, the N face of the low carrier concentration of removal is non-mixes a layer gallium nitride, and utilizes the composition of silicon tetrachloride to remove the residual oxygen of reative cell.
3) high density of utilizing the ICP reprocessing to produce, and with oxygen, the fluoro plasma of the reproducibility of GaN hypoergia, the affected layer that produces in ICP handles is repaired.
Description of drawings
Fig. 1 is that laser lift-off vertically injects (Vertical Injection Structure) GaN light-emitting diode structure schematic diagram.
Fig. 2 is laser lift-off film upside-down mounting (Thin-Film Flip-Chip) GaN light-emitting diode structure schematic diagram.
Fig. 3 is laser lift-off self-supporting (Free Standing) vertical stratification GaN light-emitting diode structure schematic diagram.
Embodiment
Below in conjunction with accompanying drawing, by embodiment the present invention is described in further detail, should be understood that following examples only are illustrative, the present invention is not subjected to the restriction of these embodiment.
The N face of GaN based vertical structure LED behind embodiment 1, the laser lift-off is handled
As shown in Figure 1, the structure of the vertical injection luminescent diode behind the laser lift-off is from bottom to top: electro-coppering or bonding silicon chip substrate 1, bonding metal layer 21, P face speculum 3, P type electrode 4, P type GaN 5, quantum well 6, N type GaN7, the non-layer GaN 8 that mix, resilient coating GaN 9.
Following concrete processing is carried out on GaN surface behind the above-mentioned laser lift-off:
1) utilizes GaN based vertical structure LED30 second after 1: 1 mixed solution of concentrated hydrochloric acid and water volume ratio soaks laser lift-off, remove that to peel off the Ga that the rear surface produces residual.
2) affected layer that N face GaN surface forms is removed in ICP preliminary treatment.According to the laser threshold difference, the thickness of affected layer is about 50～100nm.Reaction atmosphere is nitrogen or argon gas or helium or other inert gases, or the mist of their mist such as nitrogen and argon gas, the source power of adjusting ICP is between 200-300W, substrate bias power is 150-200W, chamber pressure is 5-10mTorr, gas flow is 30-40sccm, makes plasma density 10
10-11Cm
-3In the scope.The processing time of ICP is between the 15min-30min.
3) ICP handles, and removes the non-layer of mixing of N face.Reaction atmosphere is that chlorine, argon gas and silicon tetrachloride volume ratio are 26: 4: 5 mist, the source power of adjusting ICP is between 300-400W, and substrate bias power is 100-150W, and chamber pressure is 2-5mTorr, gas flow is 20-40sccm, makes plasma density 10
12-13Cm
-3In the scope.The processing time of ICP is between the 5min-30min.
4) ICP reprocessing, repair of Surface Damage and passivation.Reaction atmosphere is that oxygen and fluoroform volume ratio are 1: 1 mist, and the source power of adjusting ICP is between 100-200W, and substrate bias power is 50-100W, and chamber pressure is 10-20mTorr, and gas flow is 40-80sccm, makes plasma density 10
11-12Cm
-3In the scope.The processing time of ICP is between the 5min-20min.
By a large amount of experiment relatively, use the 20mA forward operating voltage reduction 0.4-0.5 down of this method vertical injection luminescent diode of handling of laser lift-off and the vertical injection luminescent diode of laser lift-off that uses usual method to handle to lie prostrate.
The N face of the GaN base film flip LED behind embodiment 2, the laser lift-off is handled
As shown in Figure 2, another embodiment of the present invention: film upside-down mounting (Thin-Film Flip-Chip) LED.Be successively from top to bottom: key and Si substrate 1, flip chip bonding metal level 22, P face speculum 3, P type electrode 4, P type GaN 5, quantum well 6, N type GaN 7, the non-layer GaN 8 that mix, resilient coating GaN 9, N type electrode 10.
Following processing is done on GaN surface to the film flip LED behind the above-mentioned laser lift-off:
1) utilizes 1: 1 mixed solution of concentrated hydrochloric acid and water volume ratio to soak GaN base film flip LED 30 seconds behind the laser lift-off, remove that to peel off the Ga that the rear surface produces residual.
2) affected layer that N face GaN surface forms is removed in ICP preliminary treatment.According to the laser threshold difference, the thickness of affected layer is about 50～100nm.Reaction atmosphere is nitrogen or argon gas or other inert gases, or the mist of their mist such as nitrogen and argon gas, the source power of adjusting ICP is between 250-350W, substrate bias power is 150-200W, chamber pressure is 2-20mTorr, gas flow is 10-30sccm, makes plasma density 10
10-11Cm
-3In the scope.The processing time of ICP is between the 15min-30min.
3) ICP handles, and generates the coarse surface that helps improving light extraction efficiency.Reaction atmosphere is that chlorine, argon gas and silicon tetrachloride volume ratio are 22: 8: 5 mist, the source power of adjusting ICP is between 350-450W, and substrate bias power is 100-150W, and chamber pressure is 2-5mTorr, gas flow is 20-40sccm, makes plasma density 10
12-13Cm
-3In the scope.The processing time of ICP is between the 5min-20min.
4) ICP reprocessing.Reaction atmosphere is that oxygen and fluoroform volume ratio are 2: 1 mist, and the source power of adjusting ICP is between 200-300W, and substrate bias power is 50-100W, and chamber pressure is 15-20mTorr, and gas flow is 40-80sccm, makes plasma density 10
11-12Cm
-3In the scope.The processing time of ICP is between the 5-30min.
By a large amount of experiment relatively, use the 20mA light extraction efficiency raising 30% down of this method film inverted light-emitting diode (LED) of handling and the film inverted light-emitting diode (LED) that uses usual method to handle.
The N face of GaN base self-supporting vertical stratification LED behind embodiment 3, the laser lift-off is handled
As shown in Figure 3, another embodiment of the present invention: self-supporting (Free-standing) vertical stratification LED.Be successively from top to bottom: P face routing electrode 23, P face speculum 3, P type electrode 4, P type GaN 5, quantum well 6, N type GaN 7, the non-layer GaN 8 that mix, resilient coating GaN 9.
Self-supporting vertical stratification vertical stratification LED behind the above-mentioned laser lift-off is done following processing:
1) utilizes 1: 1 mixed solution of concentrated hydrochloric acid and water volume ratio to soak GaN base self-supporting vertical stratification LED 30 seconds behind the laser lift-off, remove that to peel off the Ga that the rear surface produces residual.
2) affected layer that N face GaN surface forms is removed in ICP preliminary treatment.According to the laser threshold difference, the thickness of affected layer is about 50～100nm.Reaction atmosphere is nitrogen or argon gas or other inert gases, or the mist of their mist such as nitrogen and argon gas, the source power of adjusting ICP is between 300-400W, substrate bias power is 150-200W, chamber pressure is 10-20mTorr, gas flow is 20-30sccm, makes plasma density 10
10-11Cm
-3In the scope.The processing time of ICP is between the 15min-30min.
3) ICP handles, and removes the non-layer of mixing of N face.Reaction atmosphere is that chlorine, silicon tetrachloride and argon gas volume ratio are 28: 2: 5 mist, the source power of adjusting ICP is between 400-500W, and substrate bias power is 100-150W, and chamber pressure is 2-5mTorr, gas flow is 20-30sccm, makes plasma density 10
12-13Cm
-3In the scope.The processing time of ICP is between the 10min-20min.
4) ICP reprocessing, repair of Surface Damage and passivation reason.Reaction atmosphere is that oxygen and fluoroform volume ratio are 1: 2 mist, and the source power of adjusting ICP is between 200-300W, and substrate bias power is 50-100W, and chamber pressure is 5-10mTorr, and gas flow is 40-80sccm, makes plasma density 10
11-12Cm
-3In the scope.The processing time of ICP is between the 5min-30min.
By a large amount of experiment relatively, use 0.3 volt-0.5 volt of the 20mA forward operating voltage reduction down of this method self-supporting light emitting diode with vertical structure of handling and the self-supporting light emitting diode with vertical structure that uses usual method to handle.
Claims (9)
1. the processing method of N face behind the GaN sill laser lift-off may further comprise the steps:
1) removes gallium with the GaN sill behind the hydrochloric acid solution immersion laser lift-off;
2) ICP preliminary treatment: reaction atmosphere is nitrogen or inert gas or their mist, and the density of plasma is 10
10Cm
-3-10
11Cm
-3, 5～30 minutes processing times;
3) ICP handles: reaction atmosphere is that chlorine, silicon tetrachloride and argon gas volume ratio are 1: 0.5: 0.05 to 1: 0.05: 0.5 mist, and the density of plasma is 10
12Cm
-3-10
13Cm
-3, 1～30 minute processing time;
4) ICP reprocessing: reaction atmosphere is that oxygen and fluoroform volume ratio are 1: 0.25 to 1: 4 mist, and the density of plasma is 10
11Cm
-3-10
12Cm
-3, 5～30 minutes processing times.
2. processing method as claimed in claim 1 is characterized in that: the hydrochloric acid solution in the described step 1) is volume ratio 1: 1～1: 10 the concentrated hydrochloric acid and the mixed solution of water, and soak time is 30 seconds to 5 minutes.
3. processing method as claimed in claim 1 is characterized in that: described step 2) the pretreated source power 200-300W of ICP, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-60sccm.
4. processing method as claimed in claim 1 is characterized in that: described step 2) the pretreated reaction atmosphere of ICP is that nitrogen, argon gas volume ratio are 1: 1 mist, processing time 20min-30min.
5. processing method as claimed in claim 1 is characterized in that: the source power 100-500W that described step 3) ICP handles, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-40sccm.
6. processing method as claimed in claim 1 is characterized in that: the reaction atmosphere that described step 3) ICP handles is that chlorine, silicon tetrachloride and argon gas volume ratio are 1: 0.1: 0.2 to 1: 0.2: 0.1 mist, processing time 10min-20min.
7. processing method as claimed in claim 1 is characterized in that: the source power 100-500W of described step 3) ICP reprocessing, substrate bias power 50-200W, chamber pressure 2-20mTorr, gas flow 10-80sccm.
8. processing method as claimed in claim 1 is characterized in that:: the reaction atmosphere of described step 3) ICP reprocessing is that oxygen and tetrafluoromethane volume ratio are 1: 0.5 to 1: 2 mist, processing time 5min-10min.
9. as the described processing method of arbitrary claim in the claim 1～8, it is characterized in that: described GaN sill is film inverted structure GaN light-emitting diode, vertical injecting structure GaN light-emitting diode or self-supporting vertical stratification GaN light-emitting diode.
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