CN102856442B - Method for improving uniformity of epitaxial layer of sapphire substrate - Google Patents
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- 239000000758 substrate Substances 0.000 title claims abstract description 103
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 98
- 239000010980 sapphire Substances 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000001259 photo etching Methods 0.000 claims abstract description 7
- 229920002120 photoresistant polymer Polymers 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000001039 wet etching Methods 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 7
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000001312 dry etching Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 4
- 238000007796 conventional method Methods 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract 1
- 229910002601 GaN Inorganic materials 0.000 description 40
- 230000035882 stress Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
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- 238000004140 cleaning Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
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- 238000000407 epitaxy Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
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- Led Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a method for improving uniformity of an epitaxial layer of a sapphire substrate. The method includes: performing laser scribing to the front or back of the sapphire substrate to obtain a square pattern of 0.1mil*0.1mil to 100mil*100mil, performing photoetching to obtain a round pattern 2 micrometers to 3 micrometers in diameter in a square area so as to produce the sapphire patterned substrate, and growing GaN-LED by MOCVD (metal organic chemical vapor deposition). By the method, stress generated in GaN growth is reduced, and growth uniformity is improved. In addition, after the GaN-LED is grown by the method, a produced die can be broken directly, one-step scribing and breaking process is omitted, process time is saved, and efficiency is improved. Groove faces cut by laser help improve light emergence of the die.
Description
Technical field
The present invention relates to a kind of method improving growing GaN epitaxial loayer uniformity on sapphire pattern substrate, belong to photoelectron technical field.
Background technology
For GaN base light-emitting diode (GaN-LED), the warpage issues of backing material and the uniformity of grown epitaxial layer are the objects that numerous people pay close attention to; Conventional backing material has sapphire, Si, SiC at present.Usually, on a sapphire substrate, Sapphire Substrate has many advantages to the epitaxial loayer primary growth of GaN base materials and devices: first, and the production technology of Sapphire Substrate is ripe, device quality is better; Secondly, sapphire stability is fine, is applicable in high growth temperature environment; 3rd, sapphire mechanical strength is high, is easy to process and cleaning.Therefore, mostly all GaN base LED is prepared using sapphire as substrate.But use sapphire also to there are some problems as substrate, due to lattice mismatch and thermal stress mismatch, the warpage of substrate own is obvious, and after growing GaN, epitaxial loayer easily splits, and affects the making of chip, causes difficulty to follow-up device fabrication.
For lattice mismatch and the thermal stress mismatch problems of Sapphire Substrate, many employings sapphire pattern substrate technology (PSS) at present, PSS can solve owing to there is larger lattice mismatch and coefficient of thermal expansion mismatch between sapphire and GaN on the one hand, for a face, Sapphire Substrate lattice constant 3.18, thermal coefficient of expansion 7.5 × 10
-6k
-1, GaN lattice constant 0.47, thermal coefficient of expansion 5.59 × 10
-6k
-1; The simultaneously PSS miniature figure structural change growth course of GaN, can suppress defect to extend to epitaxial surface, reduce the defect concentration of extension.On the other hand, there is gap in the refractive index of extension GaN and Sapphire Substrate and the refractive index of air, the refractive index 2.4 of GaN material is higher than the refractive index 1.0 of Sapphire Substrate refractive index 1.7 and air, the light sent from GaN active area arrives Sapphire Substrate, when the angle of incidence is larger than a critical angle, namely there is total reflection, propagate through GaN material, to the interface of GaN and air, GaN refractive index is also greater than the refractive index of air, when the angle of incidence is larger than a critical angle, total reflection phenomenon can be there is equally, the light that such multiple total reflection causes GaN active area to send is absorbed by material through repeatedly reflecting between sapphire and air, reduce the extraction efficiency of light, PSS graphic structure changes the round that active area sends light, reduce incidence angle, reduce the chance of total reflection, increase bright dipping chance, more light is reflected through PSS structure function, improve light extraction efficiency.Although PSS technology improves light extraction efficiency, but do not reduce the stress produced in growth course, the uniformity of grown epitaxial layer also fails therefore to increase.
Chinese patent document CN1294649 discloses a kind of method of wet etching sapphire pattern substrate, comprise: steam coating silicon dioxide mask layer on sapphire C face, is carved into bar shaped by photoetching technique, then this substrate of corrosive liquid wet etching, finally remove mask, obtain sapphire pattern substrate.Adopt the substrate growth epitaxial loayer directly forming figure, during growing GaN base, threading dislocation direction by vertically transferring level to, thus reduces GaN base epitaxial loayer dislocation density, improves epitaxial loayer crystal mass.But the method can not discharge stress in advance, produce larger stress, make it warpage in GaN growth process, after growth, the uniformity of epitaxial wafer is also poor.In addition, use wet etching to obtain the mask pattern of silicon dioxide, because third dimension (size) is very little, the method for wet etching is difficult to the size controlling figure, and the cost of dry etching is very high, is unfavorable for mass production.
Summary of the invention
The present invention is directed to prior art Problems existing, a kind of method improving sapphire flat substrate or graph substrate epitaxial layer of gallium nitride uniformity is provided.
Terminological interpretation:
MOCVD: metal organic vapor phase epitaxy.
GaN-LED:GaN based light-emitting diode.
PSS figure: Patterned sapphire substrate sapphire pattern substrate.
Wet etching: be etachable material is immersed in the technology of carrying out in corrosive liquid corroding.The mixed solution of sulfuric acid and phosphoric acid is commonly used in this area, corrodes at 250-300 DEG C.
Dry etching: use ICP (sense coupling) to etch.
Technical scheme of the present invention is as follows:
Improve a method for epitaxial layer of sapphire substrate uniformity, comprise the following steps:
(1) utilize laser scribing means to carry out laser scribing to Sapphire Substrate, on Sapphire Substrate front or the back side, mark the square-shaped patterns of 0.1mil × 0.1mil ~ 100mil × 100mil with laser, obtained sapphire flat substrate.
(2) in gained sapphire flat substrate, mocvd method growing GaN epitaxial loayer is adopted.For the preparation of LED.
Square-shaped patterns size preferred 10mil × 10mil ~ 30mil × 30mil described in step (1) in said method.
Laser scribing described in step (1) in said method, scratch depth preferably 2 μm ~ 10 μm, width preferably 0.5 μm ~ 5 μm.
Said method is concrete preferred version with the Sapphire Substrate front scribing of embodiment 1.
Improve a method for epitaxial layer of sapphire substrate uniformity, comprise the following steps:
1) utilize laser scribing means to carry out laser scribing to Sapphire Substrate, on Sapphire Substrate front or the back side, mark the square-shaped patterns of 0.1mil × 0.1mil ~ 100mil × 100mil with laser, obtained sapphire flat substrate.
2) in step 1) on sapphire flat substrate front, SiN or SiO of evaporation one deck 100nm ~ 500nm
2mask; As Fig. 2.Mask layer is coated with one deck photoresist, utilize the figure that photolithography plate designs by photoresist, transfer on the square-shaped patterns area mask layer of 0.1mil × 0.1mil ~ 100mil × 100mil, after development, peel off the mask on photoresist, retain the mask on figure, by washed with de-ionized water, the mask pattern of formation rule, as Fig. 3;
3) by step 2) obtained substrate etches, and obtains the sapphire pattern substrate of mask layer; Recycling hydrofluoric acid solution erosion removal mask, rinses, dries, obtain the sapphire pattern substrate that laser scribing is crossed; The sapphire pattern substrate that this laser scribing is crossed adopts mocvd method growing GaN epitaxial loayer, for the preparation of LED.
Sapphire pattern substrate prepared by front laser scribing as shown in Figure 4; Sapphire pattern substrate prepared by backside laser scribing, as shown in Figure 5.
Step 1 in said method) described in laser scribing, scratch depth 2 μm ~ 10 μm, width 0.5 μm ~ 3 μm.
Step 1 in said method) described in square-shaped patterns size preferred 10mil × 10mil ~ 30mil × 30mil.
Step 2 in said method) described in mask pattern be circular, diameter is 2 μm ~ 3 μm.
Step 3 in said method) described in cleaning be first each ultrasonic 10min in acetone, ethanol respectively, then use deionized water rinsing.
Step 2 in said method) described in etching by prior art, wet etching or dry etching.
Said method is concrete preferred version with embodiment 2,4.
With mocvd method growing GaN epitaxial loayer in the sapphire flat substrate crossed at above-mentioned laser scribing or graph substrate, because laser scribing is by Sapphire Substrate Stress Release, reduce the stress produced in growth course, improve the uniformity of GaN epitaxial layer.
Feature of the present invention and excellent results as follows:
1, the present invention is by Sapphire Substrate laser scribing, the sapphire flat substrate of gained can be directly used in mocvd method growing GaN epitaxial loayer, because stress can first discharge by laser scribing, produces tensile stress in GaN growth process, substrate is stretched out, thus reduces substrate warpage degree.
2, first Sapphire Substrate is marked square-shaped patterns with laser by the present invention, then such as circular pattern is prepared by sapphire pattern substrate technology, and then growing GaN epitaxial loayer, because Sapphire Substrate great majority are concave surfaces, downsagging, after laser scribing streaks, stress is first discharged, then growing GaN, in GaN growth process, produce tensile stress, substrate is stretched out, thus reduces angularity.Thus solve sapphire growth GaN lattice mismatch, produce stress comparatively large, the problem that epitaxial loayer easily splits and uniformity is poor.
3, the GaN of method Sapphire Substrate of the present invention growth is for the preparation of LED, can after making tube core direct sliver on former, the step sliver operation in minimizing subsequent technique, save time, laser scribing crosses the inclined-plane of generation, can increase tube core bright dipping.
Accompanying drawing explanation
Fig. 1 is the vertical view of the Sapphire Substrate prepared by laser scribing.In figure, horizontal, vertical straight line is laser scratch.
Fig. 2 is the schematic diagram of making PSS figure in laser scribing square-shaped patterns region.Only with the figure signal in a lattice, it is the PSS figure that front sees in laser scribing region.
Fig. 3 makes figure substrate masks after the laser scribing of front.Fig. 4 is the graph substrate produced after the laser scribing of front.
Fig. 5 makes graph substrate in front according in scribing rear region after backside laser scribing.Front etched features correspond to the region of backside laser paddle-tumble.
Wherein, 1, Sapphire Substrate, 2, photoresist (mask pattern), 3, SiO
2film, 4, sapphire pattern substrate (PSS figure).
Embodiment
Below in conjunction with embodiment, the present invention is done through a step explanation.The laser scribing means used in embodiment is this area conventional equipment, model: AS2112, Newwave company produces.The Sapphire Substrate used in embodiment is brilliant U.S. 2 inch substrates in Taiwan.
Embodiment 1:
Improve the method for sapphire flat substrate epitaxial layer of gallium nitride uniformity, step is as follows:
(1) Sapphire Substrate is loaded in laser scribing means; Fixing Sapphire Substrate, on blue film, is adsorbed on plant bottom case by vacuum mode; By laser (1.3W), Sapphire Substrate front or the back side are drawn the square-shaped patterns of upper 10mil × 10mil, scratch depth 6 μm, front scribing schematic diagram is as Fig. 1;
(2) pass through MOCVD growing GaN epitaxial loayer in obtained sapphire flat substrate front, prepare LED by prior art.
Embodiment 2:
Improve the method for sapphire pattern substrate epitaxial layer of gallium nitride uniformity, step is as follows:
1) Sapphire Substrate is loaded in laser scribing means; Fixing Sapphire Substrate, on blue film, is adsorbed on plant bottom case by vacuum mode; By laser (1.3W), Sapphire Substrate front is drawn the square-shaped patterns of upper 10mil × 10mil, see Fig. 1; Scratch depth 5 μm, width 1 μm;
2) on sapphire front, the thick SiO of last layer 200nm is steamed by the method for evaporation
2mask; Mask layer is coated with last layer photoresist, utilizes photoresist by photoetching circular pattern, diameter 2 μm, transfer on the square-shaped patterns area mask layer of 10mil × 10mil, utilize photoetching to expose version, 20 seconds time for exposure, develop after 60 seconds, developer solution is alkaline solution; Toast 30 minutes, corrosion (or etching) mask layer, remove photoresist according to a conventional method, washed with de-ionized water is complete, and the mask pattern of formation rule, is shown in Fig. 3;
3) by step 2) obtained substrate utilizes existing wet etching technique to etch, namely etch in 250-300 DEG C in the mixed solution of sulfuric acid and phosphoric acid, after having etched, hydrofluoric acid solution is utilized to remove mask, by acetone, ethanol, namely washed with de-ionized water obtains required sapphire pattern substrate, sees Fig. 4;
4) by the above-mentioned sapphire pattern substrate prepared by MOCVD growing GaN, for the preparation of LED.
Embodiment 3:
As described in Example 2, difference is, only draws the square-shaped patterns of 10mil × 10mil at the Sapphire Substrate back side.
Embodiment 4:
Improve the method for sapphire pattern substrate epitaxial layer of gallium nitride uniformity, step is as follows:
1) Sapphire Substrate is loaded in laser scribing means; Fixing Sapphire Substrate, on blue film, is adsorbed on plant bottom case by vacuum mode; By laser (1.3W), sapphire backsides is drawn the square-shaped patterns of upper 20mil × 20mil, scratch depth 7 μm, width 2 μm;
2) on sapphire front, the thick SiN mask of last layer 300nm is steamed by the method for evaporation; Mask layer is coated with last layer photoresist, utilize photoresist to be transferred on the square-shaped patterns area mask layer of 20mil × 20mil by diameter 2.5 μm of circular patterns, utilize photoetching to expose version, 20 seconds time for exposure, develop after 60 seconds, developer solution is alkaline solution; Toast 30 minutes, corrosion (or etching) mask layer, remove photoresist according to a conventional method, washed with de-ionized water is complete, the mask pattern of formation rule;
3) by step 2) obtained substrate utilizes existing dry etching technology to etch, and adopts BCl
3and Cl
2gas etching, after having etched, utilize hydrofluoric acid solution to remove mask, by acetone, ethanol, namely washed with de-ionized water obtains required sapphire pattern substrate, sees Fig. 4;
4) by the above-mentioned sapphire pattern substrate prepared by MOCVD growing GaN, for the preparation of LED.
The sapphire pattern substrate epitaxial layer of gallium nitride of testing example 1-4, method of testing adopts X-Ray swing curve to test the uniformity of 102 half-peak breadths and photoluminescence spectrum test GaN growth, and test data is listed in the table below:
| Sample | X-Ray (102) half-breadth (s) | Uniformity |
| Embodiment 1 is just drawing sapphire flat substrate | 286 | 3.3 |
| Embodiment 2 just draws sapphire pattern substrate | 251 | 3.1 |
| Embodiment 3 is carried on the back and is drawn sapphire pattern substrate | 284 | 3.6 |
| Embodiment 4 is carried on the back and is drawn sapphire pattern substrate | 255 | 3.5 |
| Without the sapphire pattern substrate of laser scribing | 326 | 4.0 |
Illustrate: without the sapphire pattern substrate of laser scribing, substrate graph preparation method is identical with embodiment 2, does not just carry out laser scribing.
Conclusion: known according to above contrast, method of the present invention improves epitaxy of gallium nitride layer growth uniformity and GaN-LED quality.
Claims (2)
1. improve a method for epitaxial layer of sapphire substrate uniformity, step is as follows:
(1) Sapphire Substrate is loaded in laser scribing means; Fixing Sapphire Substrate, on blue film, is adsorbed on plant bottom case by vacuum mode; By 1.3W laser, Sapphire Substrate front is drawn the square-shaped patterns of upper 10mil × 10mil, scratch depth 5 μm, width 1 μm;
(2) on sapphire front, the SiO that evaporation one deck 200nm is thick
2mask; Mask layer is coated with last layer photoresist, utilizes photoresist to be transferred on the square-shaped patterns area mask layer of 10mil × 10mil by 2 μm of circular patterns, utilize photoetching to expose version, 20 seconds time for exposure, develop after 60 seconds, developer solution is alkaline solution; Toast 30 minutes, corrosion or etching mask layer, remove photoresist according to a conventional method, washed with de-ionized water is complete, the mask pattern of formation rule;
(3) utilize existing wet etching technique to etch substrate obtained for step (2), after etch, utilize hydrofluoric acid solution removal mask, by acetone, ethanol, namely washed with de-ionized water obtains required sapphire pattern substrate;
(4) by the above-mentioned sapphire pattern substrate prepared by MOCVD growing GaN, for the preparation of LED.
2. improve a method for epitaxial layer of sapphire substrate uniformity, step is as follows:
(1) Sapphire Substrate is loaded in laser scribing means; Fixing Sapphire Substrate, on blue film, is adsorbed on plant bottom case by vacuum mode; By 1.3W laser, sapphire backsides is drawn the square-shaped patterns of upper 20mil × 20mil, scratch depth 7 μm, width 2 μm;
(2) on sapphire front, the SiN mask that evaporation one deck 300nm is thick; Mask layer is coated with last layer photoresist, utilizes photoresist to be transferred on the square-shaped patterns area mask layer of 20mil × 20mil by 2.5 μm of circular patterns, utilize photoetching to expose version, 20 seconds time for exposure, develop after 60 seconds, developer solution is alkaline solution; Toast 30 minutes, corrosion or etching mask layer, remove photoresist according to a conventional method, washed with de-ionized water is complete, the mask pattern of formation rule;
(3) utilize existing dry etching technology to etch the substrate that step (2) is obtained, adopt BCl
3and Cl
2gas etching, after having etched, utilize hydrofluoric acid solution to remove mask, by acetone, ethanol, namely washed with de-ionized water obtains required sapphire pattern substrate;
(4) by the above-mentioned sapphire pattern substrate prepared by MOCVD growing GaN, for the preparation of LED.
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| CN107507890A (en) * | 2017-08-04 | 2017-12-22 | 东莞市中图半导体科技有限公司 | A kind of preparation method of graphical sapphire substrate |
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| CN108015425A (en) * | 2017-11-22 | 2018-05-11 | 武汉华工激光工程有限责任公司 | A kind of process of laser ablation sapphire surface coating |
| CN109599469A (en) * | 2018-12-18 | 2019-04-09 | 华中科技大学鄂州工业技术研究院 | Moth ocular structure deep-UV light-emitting diode and preparation method |
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| CN101740677A (en) * | 2008-11-20 | 2010-06-16 | 深圳世纪晶源华芯有限公司 | GaN based LED epitaxial wafer of graphical substrate and method for preparing same |
| CN102760794A (en) * | 2011-04-29 | 2012-10-31 | 山东华光光电子有限公司 | Preparation method of low-stress gallium nitride epitaxial layer |
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| CN101740677A (en) * | 2008-11-20 | 2010-06-16 | 深圳世纪晶源华芯有限公司 | GaN based LED epitaxial wafer of graphical substrate and method for preparing same |
| CN101582479A (en) * | 2009-06-10 | 2009-11-18 | 上海蓝光科技有限公司 | Light emitting diode chip structure and manufacturing method thereof |
| CN102760794A (en) * | 2011-04-29 | 2012-10-31 | 山东华光光电子有限公司 | Preparation method of low-stress gallium nitride epitaxial layer |
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| CN107507890A (en) * | 2017-08-04 | 2017-12-22 | 东莞市中图半导体科技有限公司 | A kind of preparation method of graphical sapphire substrate |
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