CN101488475A - Implementing method for self-stripping thick film gallium nitride from substrate sapphire - Google Patents
Implementing method for self-stripping thick film gallium nitride from substrate sapphire Download PDFInfo
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Abstract
本发明涉及一种厚膜氮化镓与衬底蓝宝石自剥离的实现方法，其特征在于采用了带有钝化层超大纳米孔径GaN作为厚膜的模板。在生长厚膜GaN之前，在(0001)面蓝宝石衬底上，沉积一层GaN薄膜，然后在其上蒸发一层金属Al，再采用电化学的方法生成多孔状阳极氧化铝(AAO)，然后将其刻蚀成多孔状，接着往多孔GaN孔中沉积一层介质SiO2或SiNx薄层，这样就在GaN模板上得到了带有钝化层超大纳米孔径的结构，经过清洗后，最后把这个多孔衬底置于HVPE反应腔内生长GaN厚膜。本发明提供的方法避免了光刻制作掩膜的复杂工艺，而且将孔隙尺寸缩小到纳米量级，金属Al和SiO2层均可采用电子束蒸发、溅射等方法来制备。
The invention relates to a method for realizing the self-stripping of thick-film gallium nitride and substrate sapphire, which is characterized in that GaN with a passivation layer with super large nanometer aperture is used as a thick-film template. Before growing thick-film GaN, a GaN thin film is deposited on the (0001) plane sapphire substrate, and then a layer of metal Al is evaporated on it, and then porous anodized aluminum oxide (AAO) is formed by electrochemical methods, and then It is etched into a porous shape, and then a thin layer of dielectric SiO 2 or SiN x is deposited in the porous GaN hole, so that a structure with a passivation layer with a large nanopore diameter is obtained on the GaN template. After cleaning, the final Put this porous substrate in the HVPE reaction chamber to grow GaN thick film. The method provided by the invention avoids the complex process of making a mask by photolithography, and reduces the pore size to the nanometer level, and the metal Al and SiO2 layers can be prepared by electron beam evaporation, sputtering and other methods.
Description
Technical field
The present invention relates to thick film gallium nitride (GaN) and Sapphire Substrate from the method for peeling off.Be intended to solve thick film GaN and be difficult to substrate sapphire separate, easily split broken problem, improve the epitaxial growth GaN quality of materials simultaneously, belong to the preparing technical field of GaN material.
Background technology
The GaN material has good characteristics such as high-luminous-efficiency, high heat conductance, high temperature resistant, radioresistance, acid and alkali-resistance, high strength and high rigidity, be taken as in the world one of state-of-the-art semi-conducting material in recent years and get most of the attention, the efficient indigo plant of making, green, purple, white light-emitting diode and laser have obtained using widely.Yet GaN generally is deposited on the Sapphire Substrate at present, using sapphire, to make extension GaN material also be at present mature technique, yet because GaN material and the sapphire lattice mismatch of foreign substrate (16%) and thermal expansion mismatch coefficient (9～25%) are all very big, in the GaN of extension material, there are very big stress and higher dislocation density inevitably, thus the performance and the life-span of greatly having reduced the GaN device.Therefore the needs to GaN self-supporting substrate become very urgent.And HVPE (hydride gas-phase epitaxy) growth rate height, equipment is simple, preparation cost is low, is acknowledged as the most promising growing GaN self-supporting substrate approach in recent years, has therefore attracted domestic and international researcher's extensive interest.Though adopt this method successfully to prepare thick film GaN substrate [R.J.Molnar et al.J.Cryst.Growth, V178,147,1997], but still be faced with two hang-ups: high dislocation density and stress split broken greatly and easily.People have attempted some new methods, comprising horizontal extension outgrowth (ELOG) technology, growth interruption technology etc., but the GaN dislocation density skewness that conventional ELOG method grows out, have limited the utilance of GaN material; Compression in the thick film GaN epitaxial loayer is still quite big in addition, all is easy to cracked when growth course or employing laser lift-off.Nearest 2 years, external seminar adopted porous GaN film as substrate, utilizes metal oxide vapour phase epitaxy (MOCVD) epitaxial growth high quality GaN epitaxial loayer [Y.D.Wasng et al.Appl.Phys.Lett., 85,816 (2004) .].It is the thick film GaN material HVPE epitaxial growth of substrate that the inventor has also carried out with the nanoporous GaN on the sapphire, attempts to realize the selective epitaxy growth of microcell air bridges mode, improves the quality of thick film GaN, reduces the stress in the material simultaneously.But because the growth rate of HVPE is very fast, be difficult to as MOCVD still can be complete after growth retain cavity among the nanometer GaN, the restriction of this method is that peeling off still of thick film GaN and Sapphire Substrate need be taked independent stripping technology.For this reason, how when improving the epitaxial material quality, can realize that again it is a problem of needing solution badly that Sapphire Substrate is peeled off easily.The present invention proposes a kind of GaN template that has passivation layer super large nano aperture structure for this reason.This method design is ingenious, simple, effect is remarkable.
Summary of the invention
The object of the present invention is to provide a kind of thick film GaN and substrate sapphire from the implementation method of peeling off.
The invention is characterized in the GaN that adopts the super large nano aperture vesicular texture have passivation layer template as the thick film growth, then this template is placed in the reaction chamber of hydride gas phase epitaxial growth equipment, through microcell transversal epitaxial growth process, connect into complete GaN film, when thick film reaches in certain thickness or the cool down, under action of compressive stress, thick film GaN and Sapphire Substrate take place from peeling off.
Have passivation layer super large nano aperture cellular GaN template with the little substrate of sapphire;
Having passivation layer super large nano aperture cellular GaN template is to utilize electrochemical method corroding metal Al to generate the AAO layer, after the ICP etching, then at the long-pending one deck SiO of inner hole deposition
2Or the SiNx layer forms.
The described preparation process that has the GaN template of passivation layer super large nano aperture vesicular texture is:
(1) with the sapphire be substrate, the GaN epitaxial loayer of 0.1～50 micron of the one deck of growing thereon earlier is as template;
(2) on the template of GaN epitaxial loayer, electron beam or sputtering technology evaporation one deck 50nm～1 μ m metal Al thin layer;
(3) template is adopted electrochemical method Al is oxidized to the porous anodic aluminium oxide (AAO) that is evenly distributed;
(4) template is put into phosphoric acid or phosphoric acid and soaked that part of aluminium oxide that contacts with the GaN of lower floor with removal aperture bottom and the size that changes the hole with the mixed solution of chromic acid;
(5) utilize AAO as mask,, form cellular GaN by ICP or RIE etching;
(6) in porous GaN hole, deposit one deck SiO again
2Or SiNx; Wherein, coupled plasma is induced in the ICP representative, and RIE represents reactive ion etching;
(7) remove AAO with hydrochloric acid solution, on the GaN template, obtained having passivation layer super large nano-pore and distributed.
Described on Sapphire Substrate, growth is to adopt in HVPE, metal organic chemical vapor deposition or the molecular beam epitaxial method any one as the GaN epitaxial loayer of template; The thickness of GaN epitaxial loayer is about 50nm-1 μ m;
It is the electrochemical method that adopts that described metal A l film changes uniform porous anodic aluminium oxide into, specifically is to place oxalic acid (0.3-0.5mol/L) or sulfuric acid (15wt%) solution to carry out electrochemical corrosion template;
The described mixed solution that template is put into phosphoric acid or phosphoric acid and chromic acid specifically is that the mixed solution that template is put into phosphoric acid (5wt%) or phosphoric acid (6wt%) and chromic acid (1.8wt%) is soaked 50～100min, regular ultra-large aperture (60～200nm) mesh structural porous anodic aluminum oxide films (AAO) have just been formed, then carry out ICP etching or RIE (reactive ion) etching formation cellular GaN as mask, in porous GaN hole, deposit one deck medium SiO again with AAO
2Or SiN
xLayer is removed residual A AO layer with acid solution then, promptly can be made into the GaN template that has passivation layer super large nano aperture structure.Then this template is placed the reaction chamber of the HVPE equipment thick film GaN (seeing embodiment for details) of growing, growth after annealing gas is N
2, H
2Perhaps both mists.Because the selectivity of vapor phase epitaxial growth, during growth, GaN is on the GaN table top of selecting to be grown between the hole, and can be from SiO in the super large nano-pore
2Begin growth, connect into complete GaN film through the transversal epitaxial growth process, therefore, the space at the interface of thick film GaN and template can intactly be retained, realized the growth pattern of microcell air bridges, and the compression in the thick film GaN layer obtains at the hole edge discharging, while is along with the increase of thick film GaN thickness, inner compression can be increasing, in reaching certain one-tenth-value thickness 1/10 or cool down, under the effect of compression, thick film GaN and substrate sapphire will promptly take place from peeling off phenomenon from spontaneous separating on the sapphire of bottom in thick film GaN.In addition, in the microcell transversal epitaxial growth process of thick film GaN material, the dislocation that results from the GaN template will be subjected to SiO
2The inhibition of mask greatly reduces the dislocation density of epitaxial loayer GaN thus, thereby has improved the quality of GaN film.This method is simple, and effect is obvious, for having the requirement of passivation layer super large nano aperture GaN template construct not high yet, be suitable for scientific experiment and adopt when producing in batches.
As mentioned above, provided by the invention is to adopt to have passivation layer super large nano aperture GaN as template from stripping means, transversal epitaxial growth process growth thick film GaN material, and its advantage is summarized as follows:
1. in the super large nano-pore, inject SiO
2Or SiN
xThin layer forms and has passivation layer super large nano aperture structure, thereby has made the epitaxially grown template of thick film GaN, has realized peeling off certainly, has saved other independent stripping processes.The GaN material can not be at passivation layer SiO
2Nucleation on the surface, GaN can only select to be grown on the GaN table top between the nano-pore, and can not begin growth in the super large nano-pore; Connect into complete GaN film through the transversal epitaxial growth process then, promptly, preserved space at the interface in good condition, allow the compression in the epitaxial loayer fully be discharged, overcome thick film and very easily split broken problem at this by realizing microcell air bridges growth pattern; When thick film reaches in certain thickness or the cool down, thick film GaN and Sapphire Substrate will take place from peeling off phenomenon, the negative effect of having avoided other independent stripping processes to bring;
2. in the super large nano-pore, inject SiO
2Thereby thin layer formation has passivation layer super large nano aperture structure and has made the epitaxially grown template of thick film GaN, has improved quality of materials.Because realized the microcell horizontal extension outgrowth of material growth, thereby significantly reduced dislocation density, improved crystal mass;
3. the size and the distribution at interval of being evenly distributed of the super large nano-pore of Xing Chenging, and aperture also can be regulated with the need;
Since as the size that has passivation layer super large nano-pore of mask and spaced apart evenly, so dislocation distributes comparatively evenly in HVPE Grown GaN epitaxial loayer, improved the utilization ratio of the thick film GaN after growing;
5. super large nano aperture GaN template of the present invention is to be deposited on on the Sapphire Substrate, on the Grown GaN epitaxial loayer, can adopt HVPE, gas phase epitaxy of metal organic compound (MOCVD) or molecular beam epitaxy (MBE) method as the GaN outer layer growth method of template.
Description of drawings
Fig. 1 is the structural representation before peeling off provided by the invention, 1. sapphires among the figure; 2.MOCVD-GaN; 3.SiO
2Or SiN
X4. space 5.HVPE-GaN.
Embodiment
Below by the introduction of specific embodiment, further set forth substantive distinguishing features of the present invention and obvious improvement.
Thick film gallium nitride of the present invention and substrate sapphire comprise following a few step from the method for peeling off:
A. at first, make the GaN that has passivation layer super large nano aperture structure as the thick film GaN growth templates, making step is:
1. on the Sapphire Substrate of (001) face, adopt HVPE, MOCVD or molecular beam epitaxial method about 3 microns GaN films of growing, with this film as the HVPE template; 2. template adopts the method for electron beam evaporation to deposit the metal Al thin layer that 300nm is thick in 200 ℃ temperature then; 3. again the template that has the Al layer is put into oxalic acid solution (0.3mol/L), at room temperature adopt 40 volts voltage to carry out the about 15min of anodic oxidation, then metal A l is etched electrochemically into the porous anodic alumina film AAO of regular distribution; 4. and then template place 30 ℃ of phosphoric acid solutions (5wt%) to soak 52min, purpose is to enlarge aperture (80nm) and remove that part of aluminium oxide that the aperture bottom contacts with the GaN of lower floor; 5. then this template is placed the etching 9min of ICP system, in the GaN hole, deposit the thick SiO of 5nm again
26. at last in 20% hydrochloric acid solution, soak 60min, remove residual A AO layer, can form and have SiO
2Passivation layer super large nano aperture structure distribution;
B. the GaN of the super large nano aperture structure that has passivation layer that steps A is made puts into the hvpe reactor chamber as template, at N
2Be warming up to 800 ℃ in the atmosphere, begin logical NH
3The GaN layer of protection template begins logical HCl and grows in the time of 1050 ℃; When epitaxial loayer reaches in certain thickness or the cool down, under the effect of compression, thick film GaN will be separated with the Sapphire Substrate of bottom is spontaneous, overcome thick film GaN and easily split broken problem, avoid the complicated technology and the negative effect thereof of laser lift-off simultaneously.In addition, characterize by sample test, the result shows: adopt this method growth to reduce dislocation density in the GaN epitaxial loayer greatly, significantly improved the crystalline quality of crystal, discharged epitaxial loayer stress greatly.
Claims (9)
1, a kind of thick film GaN and substrate sapphire are from the implementation method of peeling off, the GaN film of super large nano aperture vesicular texture that it is characterized in that adopting passivation layer is as the template of thick film growth, then this template is placed in the reaction chamber of hydride gas phase epitaxial growth equipment, through microcell transversal epitaxial growth process, connect into complete GaN film, when thick film reaches in certain thickness or the cool down, thick film GaN and Sapphire Substrate take place from glass under action of compressive stress;
The preparation process of the GaN film of the super large nano aperture vesicular texture of described passivation layer as the thick film growth templates is:
(a) with the sapphire be substrate, grow one deck GaN epitaxial loayer thereon as template earlier;
(b) on the template of GaN epitaxial loayer, deposition layer of metal Al thin layer;
(c) template is adopted electrochemical method Al is oxidized to the porous anodic aluminium oxide that is evenly distributed;
(d) template is put into phosphoric acid or phosphoric acid and soaked that part of aluminium oxide that contacts with the GaN of lower floor with removal aperture bottom and the size that changes the aperture with the mixed solution of chromic acid;
(e) utilize porous anodic aluminium oxide as mask,, form cellular GaN by ICP or RIE method etching;
(f) in porous GaN hole, deposit one deck SiO again
2Or SiNx is as the passivation layer medium;
(g) remove porous anodic aluminium oxide with hydrochloric acid solution, on the GaN template, obtained having passivation layer super large nano-pore and distributed.
2, the implementation method of peeling off certainly by described thick film GaN of claim 1 and substrate sapphire, it is characterized in that step a is described on Sapphire Substrate, growth is adopted in hydride gas phase epitaxial growth, metal organic chemical vapor deposition or the molecular beam epitaxial method any one as the GaN epitaxial loayer of template.
3, by claim 1 or 2 described thick film GaNs and substrate sapphire from the implementation method of peeling off, it is characterized in that described in the step a the GaN epitaxy layer thickness as template be the 0.1-50 micron.
4, by the described thick film GaN of claim 1 and substrate sapphire from the implementation method of peeling off, it is characterized in that step b described on the GaN epitaxial loayer metal A l thin film deposition adopt electron beam evaporation or sputtering method preparation; The little 50nm-1 μ of Al film m.
5, the implementation method of peeling off certainly by described thick film GaN of claim 1 and substrate sapphire is characterized in that it is the electrochemical method that adopts that the described metal A l film oxidation of step c is distributed as uniform porous anodic aluminium oxide; Described electrochemical method is that template is placed concentration is that the oxalic acid solution of 0.3-0.5mol/L or mass percentage concentration are 15% sulfuric acid.
6, the implementation method of peeling off certainly by described thick film GaN of claim 1 and substrate sapphire, it is characterized in that the described phosphoric acid solution mass percentage concentration of steps d is 5%, described mixed solution be mass percentage concentration be 6% and mass percentage concentration be that 1.8% chromic acid is formed, soak time is 50-100min.
7, the implementation method of peeling off certainly by described thick film GaN of claim 1 and substrate sapphire is characterized in that described super large nano aperture is 60-200nm.
8, by the described thick film GaN of claim 1 and substrate sapphire from the implementation method of peeling off, the GaN film of super large nano aperture vesicular texture that it is characterized in that adopting passivation layer is as template, places that the growth thick film GaN is at N in the reaction chamber
2Be warming up to 800 ℃ under the atmosphere, begin logical NH
3The GaN layer of protection template begins logical HCl growth, the growth after annealing in the time of 1050 °.
9, by the described thick film GaN of claim 8 and substrate sapphire from the implementation method of peeling off, the gas of the after annealing that it is characterized in that growing is N
2, H
2Or both mists.
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| CN112301422B (en) * | 2019-08-01 | 2024-12-17 | 北京飓芯科技有限公司 | Substrate stripping method based on laminated mask substrate |
| CN115148579A (en) * | 2022-06-24 | 2022-10-04 | 东莞市中镓半导体科技有限公司 | Preparation method of single crystal substrate |
| CN115513137A (en) * | 2022-08-18 | 2022-12-23 | 福建中晶科技有限公司 | Method for stripping sapphire and gallium nitride substrate |
| CN118263338A (en) * | 2024-05-28 | 2024-06-28 | 金阳(泉州)新能源科技有限公司 | Combined passivation back contact cell with passivation barrier layer and manufacturing and application thereof |
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