CN104319234A - Method for growing high-crystal quality AlN epitaxial layer - Google Patents
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Abstract
The invention relates to the technical field of epitaxial layer growth and in particular relates to a method for growing a high-crystal quality AlN epitaxial layer based on a large-inclination angle sapphire substrate. The method employs the large-inclination angle sapphire substrate and comprises the steps of roasting the substrate, depositing an AlN nucleating layer at a low temperature, heating for annealing, performing high-temperature epitaxial growth of AlN and reducing the dislocation density by use of macro steps caused by the step bunching effect, and controlling the AlN surface appearance, increasing the growth speed and correcting the surface appearance and promoting the weakening and disappearing of the macro steps so as to obtain flat AlN surface. The method is used for growing the high-crystal quality AlN epitaxial layer low in dislocation density and flat in surface. The method is simple and feasible, and does not cause any pollution on an MOCAD system.
Description
Technical field
The present invention relates to outer layer growth technical field, particularly relate to a kind of method based on high inclination-angle Grown on Sapphire Substrates high-crystal quality ALN epitaxial loayer.
Background technology
In recent years, in medical treatment, sterilization, printing, under the promotion of the aspect application great demands such as data storage, detection and secure communication, deep ultraviolet (DUV) luminescent device being core with high Al contents AlGaN (Al component is greater than 0.4, is called for short high Al-AlGaN) and sensitive detection parts day by day cause the attention of people.And high-performance DUV luminescent device and detector will be developed, AlN substrate and high-crystal quality AlN template are one of key foundation realizing above-mentioned device, and therefore the preparation method of the two seems very important.Because current business-like AlN single crystalline substrate is expensive, be difficult to acquisition, thus selecting in the Sapphire Substrate that UV transmittance is very high, adopt metal-organic chemical vapor deposition equipment (MOCVD) to prepare high-crystal quality AlN template just becomes international main flow route.But, there is larger lattice mismatch in above-mentioned preparation process, cause producing in AlN and a large amount of run through dislocation TD (10
9-10
10cm
-2), have a strong impact on the performance of AlGaN base photoelectric device, thus develop low-dislocation-density AlN method for preparing template very important.
(0001) surface sapphire substrate adopts the technical process of MOCVD growing AIN template be generally divided into following double teacher:
(1) stage is toasted: under hydrogen environment, under high temperature (as 1100 DEG C), toast substrate about 10 minutes;
(2) the substrate pre-treatment stage: cooling (as 950 DEG C), Alization substrate;
(3) nucleation stage: be adjusted to stratum nucleare growth temperature (as 940 DEG C), and with trimethyl aluminium and ammonia for source growing AIN nucleating layer;
(4) temperature rise period: temperature is raised (as 1100-1300 DEG C);
(5) the epitaxial growth stage: pass into trimethyl aluminium and ammonia growing AIN epitaxial loayer, thickness is 1-3 micron.
Due to the restriction of substrate technology and the Wuli-Shili-Renli system approach of AlN itself, add MOCVD growth temperature not high enough (being generally no more than 1200 DEG C) commercial at present.The growth behavior of AlN cannot be cut out completely, make effectively to realize in the preparation be difficult at AlN in high-crystal quality GaN epitaxy growth effective " two-step method " middle " multiaspect control model " (as shown in Figure 1) reducing dislocation.The image force of multiple aufwuchsplate to dislocation cannot be utilized to be used for realizing running through the bending effect (bending) of dislocation, and then to realize dislocation and bury in oblivion, react, the physical process no longer upwards extended.In addition, due to biaxial stress suffered in AlN growth course on (0001) surface sapphire, in the main dislocation movement by slip system of wurtzite structure nitride, { 0001}<11-20>, { 1-100}<11-20>, { 1-100}<0001>, { 11-20}<0001>, { effective shear stress factor of 11-20}<1-100> is zero.So realize dislocation movement by slip by stress engineering, create dislocation meet so that bury in oblivion, the approach that reacts also very poor efficiency.Based on above-mentioned restriction, the AlN epitaxial growth framework that effectively can reduce and run through dislocation (comprising screw dislocation and edge dislocation) must be developed.
Therefore, for above deficiency, the invention provides a kind of method growing the high-crystal quality AlN epitaxial loayer of low-dislocation-density and surfacing.
Summary of the invention
(1) technical problem that will solve
The technical problem to be solved in the present invention is that high-crystal quality AlN epitaxial loayer dislocation density prepared by conventional method MOCVD is large, the problem of surface irregularity.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of growing method of high-crystal quality AlN epitaxial loayer, adopt high inclination-angle Sapphire Substrate, comprising the following steps:
S1: baking substrate;
S2: low temperature depositing AlN nucleating layer;
S3: heat up annealing;
S4:AlN high temperature epitaxy grows, and grand step that effect causes reduces dislocation density to utilize step to gather;
S5:AlN surface topography controls, and improves speed of growth correction surface topography, promotes weakening and disappearing of described grand step, to obtain the AlN surface of surfacing.
Preferably, between described step S1 and described step S2, following step is performed:
S20, nitride deposition.
Preferably, the nitridation process temperature of described step S20 is 900-1000 DEG C, and chamber pressure is 50-100mbar, and nitridation time is 5-20s.
Preferably, described step S4 epitaxial growth temperature is 1000-1200 DEG C, and the molar flow ratio of ammonia and metal organic source is less than 400, and growth pressure is 50-100mbar.
Preferably, the inclination angle of described high inclination-angle Sapphire Substrate is 1 °-4 °.
Preferably, before described step S1, perform step S0 realize described nitridation time and described inclination angle matches; The AlN nucleating layer thickness realizing being formed in described nitridation time and step S2 matches.
Preferably, described thickness is 7-15nm.
Preferably, the speed of growth of the AlN in described step S4 is 0.5-0.7 μm/h, and the speed of growth of the AlN in described step S5 is for being not less than 1 μm/h.
Preferably, the method by improving metal organic source flow in described step S5 improves the described speed of growth.
Preferably, described growing method is metal-organic chemical vapor deposition equipment method.
(3) beneficial effect
Technique scheme tool of the present invention has the following advantages: the growing method of this high-crystal quality AlN epitaxial loayer adopts high inclination-angle Sapphire Substrate, comprises baking substrate; Low temperature depositing AlN nucleating layer; Heat up annealing; AlN high temperature epitaxy grows, and the grand step effect utilizing step coalescence to cause reduces edge dislocation density; AlN surface topography controls, and changes speed of growth correction surface topography, promotes weakening and disappearing of grand step effect, to obtain the AlN surface of surfacing.High inclination-angle sapphire does substrate and produces very little atomic steps width, makes lower growth temperature just can realize the two dimensional mode of AlN; The coalescence effect of atomic steps in high inclination-angle Sapphire Substrate is utilized to cause grand step, and then the image force effect to dislocation caused, realize the minimizing bending effect of dislocation being realized to dislocation, utilize X-ray diffraction ω scan A lN epitaxial loayer (002) face swing curve halfwidth can lower than 100arscec, (102) face halfwidth lower than 500arscec, and then can have very low spiral shell type and edge dislocation density; By the adjustment to the AlN speed of growth, realize the grand step eliminated because atomic steps coalescence causes, realize very smooth AlN surface.Therefore, low, the surfacing of AlN epitaxial loayer dislocation density of the growing method growth of high-crystal quality AlN epitaxial loayer provided by the invention.The inventive method is simple, and can not cause any pollution to MOCVD system.
Accompanying drawing explanation
Fig. 1 is the multiaspect control model schematic diagram that existing GaN MOCVD growth " two-step method " runs through dislocation minimizing;
Fig. 2 is " multiaspect control model " schematic diagram that the epitaxial loayer of AlN in high inclination-angle Sapphire Substrate is prepared Dislocations and reduced;
Fig. 3 (a), Fig. 3 (b) are (0001) surface sapphire substrate schematic diagrames;
Fig. 4 is the step block diagram of high-crystal quality AlN outer layer growth method provided by the invention.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Figure 4 shows that the step block diagram of the high-crystal quality AlN outer layer growth method that the present embodiment provides.The invention provides a kind of growing method of high-crystal quality AlN epitaxial loayer, adopt high inclination-angle Sapphire Substrate, comprise the following steps:
S1: baking substrate;
S2: low temperature depositing AlN nucleating layer;
S3: heat up annealing;
S4:AlN high temperature epitaxy grows, and grand step that effect causes reduces dislocation density to utilize step to gather;
S5:AlN surface topography controls, and improves speed of growth correction surface topography, promotes weakening and disappearing of described grand step, to obtain the AlN surface of surfacing.
The AlN epitaxial loayer dislocation density of the growing method growth of high-crystal quality AlN epitaxial loayer provided by the invention is low, surfacing.The inventive method is simple, and can not cause any pollution to MOCVD system.
Step S20 is performed: nitride deposition between step S1 and step S2.For improving the efficiency reducing dislocation further, introducing nitriding process process, to expect the compacting generation of screw dislocation and the adjustment of stress, widening the window of growth technique further.
The nitridation process temperature of step S20 is 900-1000 DEG C, and chamber pressure is 50-100mbar, and nitridation time is 5-20s.
Step S4 epitaxial growth temperature is 1000-1200 DEG C, and the molar flow ratio (V/III mol ratio) of ammonia and metal organic source is less than 400, and growth pressure is 50-100mbar.
The inclination angle of high inclination-angle Sapphire Substrate is C off M (or A) 1 °-4 °.Wherein, in order to high-quality epitaxial growth, the actual substrate used, when cutting, all has certain angle of inclination relative to (0001) positive crystal face.The mode tilted has two kinds, and as shown in Fig. 3 (b), one is be that axle rotates certain inclination angle with a-Axis, and two is be that axle rotates certain inclination angle with m-Axis.What the Sapphire Substrate in (0001) face of such as C off M 2 ° referred to is exactly with a-Axis is that axle rotates 2 ° of substrates carrying out cutting and polishing and prepare; What (0001) face of C off A 2 ° referred to is then be that axle rotates 2 ° of substrates carrying out cutting and polishing and prepare with m-Axis.Wherein, shown in Fig. 3 (a), X is reference edge.
Before step S1, perform step S0 realize nitridation time and inclination angle matches; The AlN nucleating layer thickness realizing being formed in nitridation time and step S2 matches.Further, can be obtained by experiment repeatedly, the matched data between optimized nitridation time and inclination angle and nucleating layer thickness, and then can make that the high-crystal quality AlN epitaxial loayer dislocation density of generation is lower, surface is more smooth.It is also like this in like manner matching with nucleating layer thickness, and wherein, the criterion of judgement is: whether dislocation density reduces.Further, the thickness of the AlN nucleating layer formed in step S2 is 7-15nm.
The speed of growth of the AlN in step S4 is 0.5-0.7 μm/h, and the speed of growth of the AlN in step S5 is for being not less than 1 μm/h.
Method by improving metal organic source flow in step S5 improves the described speed of growth.
Further, growing method is metal-organic chemical vapor deposition equipment method.
The present invention is on the nitride-based semiconductor heteroepitaxial growth process basis of routine, realizes preparing low-dislocation-density AlN epitaxial thin film material.Its core concept is by adopting high inclination-angle (miscut angle) (0001) surface sapphire substrate method, produce the crystal face of other orientation except (0001) face, do one's utmost to create " multiaspect control model ", realize burying in oblivion and reacting of dislocation.Meanwhile, by choosing, there is different angle Sapphire Substrate, effectively can cut out the atomic steps width of substrate surface, add the degree of freedom that MOCVD Material growth mode parameter controls.And the rigors effectively reduced AlN growth temperature, realize stability and the reliability of two dimensional mode (layer by layer or step-flow pattern), ensure the smooth of surface.
Preparation method of the present invention comprises several stages such as substrate bake, underlayer nitriding, low temperature depositing AlN nucleating layer, intensification, the growth of AlN high temperature epitaxy.In order to grow high-crystal quality AlN epitaxial loayer, technical essential of the present invention has 3 points.One is the introducing of underlayer nitriding treatment process, and this step, by changing its micro-structural to the modification of sapphire substrate surface, is conducive to realizing extremely low screw dislocation density.Two is adopt high inclination-angle (selecting C off M (or A) 1 °-4 °) Sapphire Substrate, change the atomic steps width that substrate surface effectively can be cut out in substrate inclination angle, such as when inclination angle changes to 4 ° from 2 °, step width can be reduced to 18.6nm from 37.2nm, much smaller than the step width 372.2nm of now widely used conventional sapphire substrate C off M 0.2 °, the very little atomic steps width that high inclination-angle causes, makes lower growth temperature just can realize the two dimensional mode of AlN; The more important thing is, grand step (macro step) face that the coalescence effect (bunching) of atomic steps on high inclination-angle substrate produces can be utilized, and then the image force effect causing dislocation, realize the bending effect (bending) to dislocation, create dislocation meet and then merge, form dislocation loop and bury in oblivion behavior and then dislocation minimizing, the particularly reduction (as shown in Figure 2) of edge dislocation density.Three is after the physical process completing the minimizing of AlN Dislocations above, by the adjustment to the AlN speed of growth, realizes eliminating the grand step caused because atomic steps gathers, and realizes very smooth AlN surface.Based on above main points, in the present invention, preferred technical scheme is first optimized the coupling of substrate inclination angle and nitridation time, and the coupling of both realizations realizes the AlN of low-dislocation-density; Then on this basis, by changing the speed of growth of AlN, realizing the control of effects on surface pattern, eliminating grand step, realizing monatomic steps pattern.On the Process ba-sis optimized, the high growth temperature of AlN can reduce greatly to the requirement of temperature, lower temperature just can prepare the AlN epitaxial film with better crystal mass, far below the high temperature of more than 1400 DEG C that the AlN epitaxial growth of bibliographical information in the world needs, the restriction that general commercial MOCVD growth temperature is lower can be removed greatly, there is very large using value.
In the methods of the invention, in the substrate bake stage, baking temperature is 1080-1150 DEG C; Underlayer nitriding phase temperature is 900-1000 DEG C; At low temperature AI N nucleation stage, temperature is 900-1000 DEG C, chamber pressure 50-100mbar, and thickness is 7-15nm; Intensification annealing stage, rises to high temperature epitaxy temperature 1000-1200 DEG C from nucleating layer temperature, and the time is 100-250s, and stablizes 20-50s; AlN high temperature epitaxy growth phase, epitaxial growth temperature is that 1000-1200 DEG C, V/III mol ratio is less than 400 (according to MOCVD configuration adjustment, adopting as far as possible little V/III mol ratio), growth pressure 50-100mbar; Other condition adopts conventional AlN growth conditions; The last surface topography adjusting stage, when keeping other condition of high temperature epitaxy growth constant, by improving the flow of metal organic source, increasing the AlN speed of growth, reduce and eliminate grand step, realize the AlN surface of atomically flating.The method key point is: (1) underlayer nitriding stage, the time of nitrogenize needs and AlN nucleating layer thickness matching, significantly can reduce X-ray diffraction ω in AlN and scan (002) face swing curve halfwidth, otherwise then cause the rising of this value of a half width; (2) AlN high temperature epitaxy growth phase, speeds control is to 0.5-0.7 micro-m/h, and the effect causing grand step to realize dislocation minimizing reduces by the too fast speed of growth; (3) the last surface topography adjusting stage, improved the speed of growth of AlN by the method improving metal organic source flow, realize the AlN surface of atomically flating.
Embodiment one
1) with metal-organic chemical vapor deposition equipment (MOCVD) equipment (3 × 2 " Thomas Swan CCS MOCVD); substrate adopts the Sapphire Substrate in (0001) face of C off M 2 °; pass into H2; chamber pressure is 120mbar; toast 600s at 1100 DEG C, cleaning substrate.
2) cool to 950 DEG C, pass into ammonia nitrogenize 7s, H2 is as carrier gas, and chamber pressure is 100mbar.And trimethyl aluminium is passed in reative cell.
3) 950 DEG C of growing low temperature AlN, growth thickness is 10nm.
4) keep chamber pressure to be 100mbar, stop logical trimethyl aluminium, continue to pass into ammonia, with 200 second time, temperature is risen to 1100 DEG C, stablize 20s.
5) pass into ammonia and trimethyl aluminium, keep chamber pressure 80mbar, the condition that temperature is 1100 DEG C, V/III mol ratio is 375, high temperature epitaxy growing AIN, and thickness is 1 μm.
6) in maintenance 5) on the constant basis of other condition, improve the flow of trimethyl aluminium flow to 30umol/min, continuation epitaxial growth AlN, thickness is 500nm.
In the AlN epitaxial loayer that embodiment one obtains, X-ray diffraction ω is utilized to scan (002) face swing curve halfwidth lower than 100arscec, (102) face halfwidth is lower than 500arscec, and then has lower spiral shell type and edge dislocation density.
Wherein, halfwidth refers to the difference of surface sweeping angle corresponding to the X ray ω-rocking scans peak of curve intensity half place of particular crystal plane, and this value is less, and crystal mass is better.Two conventional crystal faces be (002) and (102) face, (002) face value of a half width correspondence screw dislocation density, and dislocation density be proportional to this half width values square; (102) the corresponding edge dislocation density of the value of a half width in face, dislocation density be also proportional to this half width values square.
Embodiment two
1) with metal-organic chemical vapor deposition equipment (MOCVD) equipment (3 × 2 " Aixtron CCS FP-MOCVD); substrate adopts the Sapphire Substrate in (0001) face of C off M 4 °; pass into H2; chamber pressure is 120mbar; toast 600s at 1100 DEG C, cleaning substrate.
2) cool to 930 DEG C, pass into ammonia nitrogenize 10s, H2 is as carrier gas, and chamber pressure is 90mbar.And trimethyl aluminium is passed in reative cell.
3) 930 DEG C of growing low temperature AlN, growth thickness is 10nm.
4) keep chamber pressure to be 100mbar, stop logical trimethyl aluminium, continue to pass into ammonia, with 100 second time, temperature is risen to 1000 DEG C, stablize 20s.
5) pass into ammonia and trimethyl aluminium, keep chamber pressure 60mbar, the condition that temperature is 1000 DEG C, V/III mol ratio is 200, high temperature epitaxy growing AIN, and thickness is 0.8 μm.
6) in maintenance 5) on the constant basis of other condition, improve trimethyl aluminium flow, continue epitaxial growth AlN, speed is 1.0 μm/h, and thickness is 300nm.
In the AlN epitaxial loayer that embodiment two obtains, X-ray diffraction ω is utilized to scan (002) face swing curve halfwidth lower than 100arscec, (102) face halfwidth is lower than 500arscec, and then has lower spiral shell type and edge dislocation density.
In sum, the invention provides a kind of method growing the high-crystal quality AlN epitaxial loayer of low-dislocation-density and surfacing.The inventive method is simple, and can not cause any pollution to MOCVD system.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
1. a growing method for high-crystal quality AlN epitaxial loayer, is characterized in that, adopts high inclination-angle Sapphire Substrate, comprises the following steps:
S1: baking substrate;
S2: low temperature depositing AlN nucleating layer;
S3: heat up annealing;
S4:AlN high temperature epitaxy grows, and grand step that effect causes reduces dislocation density to utilize step to gather;
S5:AlN surface topography controls, and improves speed of growth correction surface topography, promotes weakening and disappearing of described grand step, to obtain the AlN surface of surfacing.
2. growing method according to claim 1, is characterized in that, between described step S1 and described step S2, perform following step:
S20, nitride deposition.
3. growing method according to claim 2, is characterized in that, the nitridation process temperature of described step S20 is 900-1000 DEG C, and chamber pressure is 50-100mbar, and nitridation time is 5-20s.
4. growing method according to claim 1, is characterized in that, described step S4 epitaxial growth temperature is 1000-1200 DEG C, and the molar flow ratio of ammonia and metal organic source is less than 400, and growth pressure is 50-100mbar.
5. growing method according to claim 1, is characterized in that, the inclination angle of described high inclination-angle Sapphire Substrate is 1 °-4 °.
6. growing method according to claim 5, is characterized in that, performs step S0 and realized described nitridation time and described inclination angle matches before described step S1; The AlN nucleating layer thickness realizing being formed in described nitridation time and step S2 matches.
7. growing method according to claim 6, is characterized in that, described thickness is 7-15nm.
8. growing method according to claim 1, is characterized in that, the speed of growth of the AlN in described step S4 is 0.5-0.7 μm/h, and the speed of growth of the AlN in described step S5 is for being not less than 1 μm/h.
9. growing method according to claim 1, is characterized in that, the method by improving metal organic source flow in described step S5 improves the described speed of growth.
10. the growing method according to any one of claim 1-9, is characterized in that, described growing method is metal-organic chemical vapor deposition equipment method.
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| 冯超: "蓝宝石衬底上高质量ALN材料生长研究", 《中国优秀硕士学位论文全文数据库信息科技辑》 * |
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