CN1825539A - Method for growing non-crack III family nitride on silicon substrate - Google Patents
Method for growing non-crack III family nitride on silicon substrate Download PDFInfo
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Abstract
The invention is a method for growing crackles family-III nitride on a silicon substrate, using stress compensating buffer layer to grow crackles a family-III nitride film on the silicon substrate, and comprising the steps of: 1) firstly depositing an about 20 nanometer thick aluminized high-temperature aluminum nitride buffer layer on a monocrystalline silicon substrate and then depositing a layer of hexagonal-phase matter (such as low-temperature aluminum nitride, gallium aluminum nitride or boron nitride) whose lattice constant is far less than that of the family-III nitride and thus forming a buffer layer with stress compensating function; and 2) adding in an activating agent to make a stress compensating layer easy to form at low temperature and simultaneously the surface smooth and the crystal quality high; 3) because the lattice constant of the predeposited hexagonal-phase matter is less than that of the family-III nitride, able to introduce pressure stress into the family-III nitride film grown on the predeposited hexagonal-phase matter so as to compensate drawing stress caused by mismatching with the silicon substrate.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly a kind of stress compensation resilient coating prepares the method for the silica-based III group-III nitride of flawless film.
Background technology
With gallium nitride (GaN) is the III group-III nitride semiconductor of representative owing to can be used for blue-ray LED and LD, the high-density optical storage, and high temperature, high-power and high-frequency electron device, fields such as ultraviolet detector, thereby have boundless application prospect.
Yet, be difficult to obtain high-quality gallium nitride (GaN) film owing to there is not homo-substrate.So far Zhi Bei device level gallium nitride (GaN) film obtains on Sapphire Substrate mostly.Because Sapphire Substrate hardness is big, non-conductive, and cost an arm and a leg, be difficult to produce in enormous quantities, force people to go to attempt in inexpensive, heat conduction, conduction, large scale, be easy to cleavage and be easy to growth high-quality gallium nitride (GaN) on the integrated silicon substrate of photoelectricity, to overcome the shortcoming of Sapphire Substrate.
But lattice mismatch reaches 20% between silicon (Si) and the gallium nitride (GaN), and thermal mismatching is more up to 56%, epitaxial growth of gallium nitride on silicon substrate (GaN) is highly susceptible to cracking, and crackle becomes the main problem of puzzlement growth of device level high-quality gallium nitride (GaN) on silicon (Si) base.
The main method that solves crackle in the basic gallium nitride of silicon (Si) (GaN) at present has following several:
1, in the enterprising line mask of silicon substrate or the direct horizontal extension method of etching.The artificial continuous surface with silicon of this method isolates and comes, and gallium nitride (GaN) epitaxial growth is limited in the small window area, can effectively alleviate the stress in the big plane, stops the generation of crackle.Shortcoming is a complex process, and the flawless zone is less.
2, in gallium nitride (GaN), insert low temperature aluminium nitride (AlN) layer.By certain thickness low temperature polycrystalline aluminium nitride (AlN) layer, can partly discharge because the stress that thermal mismatching produces is realized the flawless film.
3, adopt aluminum gallium nitride (AlGaN) layer of gradient gradual change.Utilize the lattice constant of aluminium nitride (AlN) to be slightly less than the lattice constant of gallium nitride (GaN), make in the gallium nitride (GaN) of growth on aluminum gallium nitride (AlGaN) layer compression to occur, the tensile stress that forms in can the partial offset temperature-fall period reduces the generation of crackle.
Above first method complex process, second method can reduce crystal mass, and the effect of the third method is better.
The basic gallium nitride of silicon (Si) (GaN) film growth practice confirms, utilize " stress engineering " principle, adopt gradient gradual change aluminum gallium nitride (AlGaN) layer, in gallium nitride (GaN) film of growth subsequently, introduce compression, compensating hot tensile stress, is to reduce the effective method of crackle.But utilizing the method can only grow thickness so far is 1 micron flawless gallium nitride (GaN) film.This mainly is that the growth for Thin Film temperature is high more because high-quality gallium nitride aluminium (AlGaN) film need be grown at higher temperature (growth temperature that is higher than gallium nitride (GaN)), and then the stress compensation effect is more little; Simultaneously aluminium (Al) content can't be carried De Taigao, if aluminium (Al) content too high (greater than 20%) then aluminum gallium nitride (AlGaN) layer itself also can ftracture.Difference than the aluminum gallium nitride (AlGaN) of low-aluminum-content layer and gallium nitride (GaN) layer crystal lattice constant is little, can't introduce the compression of the hot tensile stress of adequate remedy.
Summary of the invention
The object of the present invention is to provide a kind of stress compensation resilient coating to prepare the method for the silica-based III group-III nitride of flawless film.Refer in particular to a kind of stress compensation resilient coating that on silicon substrate, inserts, with preparation flawless III group-III nitride film, and utilize activating agent to prepare low temperature aluminium nitride (AlN), aluminum gallium nitride (AlGaN) the stress compensation resilient coating of rich aluminium (Al), with a kind of new stress compensation cushioning layer material borazon, reach 1.5 microns flawless III group-III nitride films with preparation thickness.
The invention provides a kind of structure of inserting the stress compensation resilient coating, growing flawless III group-III nitride film on silicon substrate of utilizing.This method technology is simple, can grow at a lower temperature by introducing activating agent that aluminium content can reach 40%, crystal mass is high and flawless aluminum gallium nitride (AlGaN) the stress compensation resilient coating that has an even surface, can effectively eliminate the crackle in silicon based gallium nitride (GaN) film in the large tracts of land, can grow obtains about 1.5 microns of thickness, the flawless III group-III nitride film that device can be used.Process window broad of the present invention simultaneously, to the dependence of appointed condition a little less than, be a kind of method of pervasive elimination silicon based gallium nitride (GaN) crackle.
In order to achieve the above object, technical solution of the present invention provide a kind of on silicon substrate the method for growing flawless III group-III nitride, it is between silicon substrate and III group-III nitride film, insert the stress compensation resilient coating at low temperatures by introducing activating agent, growth obtains the flawless III group-III nitride film that thickness≤1.5 micron, device can be used on the stress compensation resilient coating again.
Described method, it comprises step:
A) temperature is in the time of 1000 ~ 1100 ℃, in surface of silicon earlier behind the thick aluminum layer of deposition 1 ~ 2nm, and regrowth aluminum nitride buffer layer 20 ~ 30nm;
B) be cooled to 900～950 ℃, feed ammonia, trimethyl gallium, trimethyl aluminium or other unstripped gas, feed surfactant simultaneously, the aluminum gallium nitride of growing aluminum nitride or rich aluminium or boron nitride stress compensation resilient coating 50 ~ 500nm, the thickness of stress compensation resilient coating is regulated according to the flow velocity and the temperature of unstripped gas;
C) last, be warmed up to 1000 ~ 1100 ℃, growing flawless III group-III nitride film on the stress compensation resilient coating.
Described method, its b) surfactant described in the step is the magnesium base, one or more in these three kinds of compounds of zinc-base and indium base; The aluminum gallium nitride of rich aluminium, aluminium content is greater than 20%.
Described method, its described stress compensation resilient coating, the little lattice constant of the III group-III nitride of growth thereon of the lattice constant of this layer material, crystal structure is six side's phases, introduce compression in the III group-III nitride film that can grow thereon, thereby the tension stress that compensation and silicon substrate thermal mismatching are introduced stops the generation and the expansion in Interface Crack source.
Described method, its described III group-III nitride film is gallium nitride, aluminum gallium nitride, indium gallium nitrogen, aluminium gallium nitrogen a kind of thin-film material or their thin-film materials of being combined to form wherein.
Described method, the epitaxial growth equipment that it is suitable for is metal organic-matter chemical vapour phase epitaxy, molecular beam epitaxy, hydride gas-phase epitaxy and ion sputtering.
Because surfactant has reduced surface energy, the surface activity in aluminium source is increased, high-quality gallium nitride aluminium (AlGaN) layer can generate at a lower temperature, has increased the content of aluminium element simultaneously.Aluminium content many more, it is also big more that the lattice constant of the lattice constant of epitaxial film and gallium nitride (GaN) differs; Boron nitride (BN) also is a hexagonal structure, and lattice constant is also much smaller than the lattice constant of gallium nitride (GaN).Do the intermediate buffering layer by the film that these lattice constants are formed much smaller than the material of the hexagonal structure of gallium nitride (GaN), by " stress engineering " principle, can in III group-III nitride growth thereafter, introduce bigger compression, subsequently cooling procedure effectively compensation owing to silicon and III group-III nitride between the hot tensile stress introduced of bigger thermal expansion coefficient difference, thereby avoid the generation of crackle.So the present invention is with this resilient coating called after " stress compensation resilient coating ".
Stress compensation resilient coating of the present invention need use surfactant during growth, to reduce surface formation energy, improves crystalline quality.Surfactant comprises magnesium (Mg), all cpds of zinc (Zn) and indium (In).Must select suitable surfactant according to the difference of thin-film material.
Stress compensation resilient coating of the present invention must must be grown under 800 ℃ to 1000 ℃ growth temperature as aluminum gallium nitride (AlGaN) in lower temperature growth, and other material should be selected suitable growth temperature in this scope according to its characteristic.
The present invention adopts the method that increases activator, can be at lower growth temperature (less than 1000 ℃) growing flawless, have an even surface, low temperature aluminum gallium nitride (AlGaN) stress compensation layer of crystal mass height and high aluminium content (about 40%), without the method that multilayer is inserted, direct growth goes out flawless gallium nitride (GaN) film of 1.5 micron thickness; Find another kind of stress compensation layer material-hexagonal boron nitride (h-BN) simultaneously, hexagonal boron nitride is a hexagonal structure, lattice constant is 2.345nm, much smaller than the 3.514nm of gallium nitride (GaN), does the compression that stress compensation layer can be introduced the adequate remedy thermal stress with it.
The present invention compares with technology in the past, and this invention has following meaning:
1) be applicable to all kinds of epitaxial growth equipments commonly used at present, as metal organic-matter chemical vapour phase epitaxy (MOCVD), molecular beam epitaxy (MBE), hydride gas-phase epitaxy (HVPE) and ion sputtering etc.
2) utilized grow at low temperatures high-quality gallium nitride aluminium (AlGaN) film of higher aluminum content of activating agent technology.
3) utilize the intrinsic characteristic of aluminum gallium nitride (AlGaN) compound: its lattice constant is less than the lattice constant of gallium nitride (GaN).Find the hexagonal boron nitride (h-BN) of another kind of lattice constant simultaneously less than the hexagonal structure of gallium nitride (GaN).Do the intermediate buffering layer by the film that these lattice constants are formed much smaller than the material of the hexagonal structure of gallium nitride (GaN), by " stress engineering " principle, can in III group-III nitride growth thereafter, introduce bigger compression, subsequently cooling procedure effectively compensation owing to silicon and III group-III nitride between the hot tensile stress introduced of bigger thermal expansion coefficient difference, thereby avoid the generation of crackle.
4) do not need other ancillary techniques such as mask, photoetching, also need not introduce polycrystalline/monocrystalline interface, technology is simple, and cost is low, need not add any new process equipment and can finish.
5) can reach 1.5 microns the good silicon based gallium nitride film of flawless, crystal mass by direct growth thickness.
Description of drawings
Fig. 1 is the structural representation that stress compensation resilient coating of the present invention prepares the silica-based III group-III nitride of large tracts of land flawless film;
Fig. 2 a is the comparison diagram that insertion stress compensation resilient coating and Fig. 2 b do not insert silica-based 1.5 micron thickness gallium nitride (GaN) the epitaxial film surface topographies of stress compensation resilient coating;
Fig. 3 is a stress compensation resilient coating when not using activating agent, 1.5 microns gallium nitride of its extension (GaN) film surface appearance figure;
Fig. 4 is the comparison diagram that inserts stress compensation resilient coating a and do not insert silica-based 1.5 micron thickness gallium nitride (GaN) the epitaxial film X-ray double crystal diffraction XRD swing curves of stress compensation resilient coating b.
Embodiment
Detailed introduction that below provides and the accompanying drawing that only provides by explanation can make the present invention be easier to understand fully, but are not to limit the present invention thus.Hereinafter, will introduce the present invention in detail and on silicon substrate, insert stress compensation resilient coating low temperature aluminum gallium nitride (AlGaN) the structure 1.5 microns flawless III group-III nitride films of growing in advance, and adopt activating agent to prepare an example of its method.
With the metal-organic chemical vapor deposition equipment method is example.
As shown in Figure 1, behind high-temperature ammonolysis aluminium (AlN) resilient coating 3 of silicon substrate 1 surface deposition 1 ~ 2nm fine aluminium (Al) layer 2 and 20 ~ 30nm, be cooled to about 950 ℃, feed unstripped gass such as ammonia, trimethyl gallium and trimethyl aluminium, feed a kind of indium (In) class activating agent simultaneously, growing low temperature stress compensation resilient coating 4, the thickness of this layer is regulated according to the flow velocity and the temperature of unstripped gas, can in 50 ~ 500nm scope, change, in order to strengthen the stress compensation effect, aluminium (Al) content should be greater than 20%, the certain thickness III group-III nitride film 5 of growing at last.
The present invention has utilized grow at low temperatures high-quality gallium nitride aluminium (AlGaN) film of higher aluminum content of activating agent technology, and utilize the intrinsic characteristic of aluminum gallium nitride (AlGaN) compound: its lattice constant is less than the lattice constant of gallium nitride (GaN).Find the hexagonal boron nitride (h-BN) of another kind of lattice constant simultaneously less than the hexagonal structure of gallium nitride (GaN).Do the intermediate buffering layer by the film that these lattice constants are formed much smaller than the material of the hexagonal structure of gallium nitride (GaN), by " stress engineering " principle, can in III group-III nitride growth thereafter, introduce bigger compression, subsequently cooling procedure effectively compensation owing to silicon and III group-III nitride between the hot tensile stress introduced of bigger thermal expansion coefficient difference, thereby avoid the generation of crackle.Success growth on silicon substrate obtains thickness and reaches 1.5 microns flawless gallium nitrides (GaN) film.
Compare with other technology of growing silica-based flawless III group-III nitride epitaxial film, present technique does not need other ancillary techniques such as mask, photoetching, need not introduce multilayer polycrystalline/monocrystalline interface yet, technology is simple, the stress compensation effect is obvious, its principle has universality applicable to multiple epitaxy technology (comprising MOCVD, MBE and HVPE etc.) and multiple material system.Compare with existing method simultaneously, can grow thicker flawless silicon based gallium nitride (GaN) film (reaching 1.5 microns), adopt the luminescent properties of the gallium nitride (GaN) of aluminum gallium nitride (AlGaN) the stress compensation resilient coating technology growth that activates that obvious enhancing (accompanying drawing 4) is arranged, illustrate that the performance of the basic gallium nitride of silicon (Si) (GaN) has clear improvement.
Implement main method of the present invention and comprise various semiconductor film membrane preparation methods, as metal organic-matter chemical vapour phase epitaxy (MOCVD), molecular beam epitaxy (MBE), hydride gas-phase epitaxy (HVPE) and ion sputtering etc., to different semiconductor film preparing systems, various growth parameter(s)s are adjusted as the case may be.
The III group-III nitride comprises: the structural material that thin-film material such as gallium nitride, aluminum gallium nitride, indium gallium nitrogen, aluminium gallium nitrogen or they are combined to form.
Embodiment 1:
With the metal-organic chemical vapor deposition equipment mocvd method is example.
1) be substrate with monocrystalline silicon silicon (Si) (111) face;
2) be warmed up to 1000 ~ 1100 ℃, feed trimethyl aluminium TMAl, form thin aluminium (Al) layer at silicon face; Feed ammonia then, form aluminium nitride (AlN) layer about 30nm;
3) cool to 800 ~ 1000 ℃, growing gallium nitride aluminium (AlGaN) stress compensation resilient coating.Ammonia, trimethyl gallium and trimethyl aluminium are used as unstrpped gas: wherein the flow velocity of ammonia is 4L/min, and the flow velocity of trimethyl gallium is 10umol/min, and the flow velocity of trimethyl aluminium is 10umol/min.Feed indium (In) the class activating agent of trace simultaneously.The thickness of this layer is 100nm;
4) be warmed up to 1000 ~ 1100 ℃ high temperature, growing gallium nitride (GaN) epitaxial film, thickness is 1.5um.
The surface topography that inserts the stress compensation resilient coating and do not insert 1.5 microns silicon based gallium nitrides of stress compensation resilient coating (GaN) epitaxial film is adopted in contrast, shown in the accompanying drawing 2, found that Fig. 2 b has many parallel to each other with gallium nitride (GaN) surface of conventional method growth, crisscross crackle, through behind certain process optimization, can in 10um * 10um square range, there be crackle to produce greatly; And behind aluminum gallium nitride (AlGaN) the stress compensation resilient coating of Fig. 2 a employing insertion activating process growth, gallium nitride (GaN) by identical technology growth same thickness, the quantity of its face crack has reduction significantly, seldom can find crackle in the range of observation shown in Fig. 2 a, and surfacing.Simultaneously, we have provided the employing activating process and have not adopted the influence of activating process to gallium nitride (GaN) film surface appearance.When growing gallium nitride aluminium (AlGaN) stress compensation resilient coating, do not use activator, a large amount of crackles still appear in its gallium nitride of growing subsequently (GaN) surface, and the surface is very uneven, many round projections occur, as shown in Figure 3.ω swing curve with twin crystal X-ray diffraction (XRD spectrum) is studied the crystal mass of gallium nitride (GaN) epitaxial film, as shown in Figure 4.Found that curve a inserts that the halfwidth FWHM at growing gallium nitride (GaN) film XRD (0002) peak is 11.2arcmin behind aluminum gallium nitride (AlGaN) the stress compensation resilient coating, the halfwidth of gallium nitride (GaN) film that does not insert the stress compensation resilient coating than curve b is narrow, after insertion aluminum gallium nitride (AlGaN) stress compensation resilient coating is described, epitaxially grown gallium nitride (GaN) film not only face crack reduces in a large number, and crystal mass is greatly improved simultaneously, the halfwidth FWHM that its optical property research is also found its PL spectrum reduces, and illustrates that optical property also makes moderate progress.General low temperature aluminum gallium nitride (AlGaN) and aluminium nitride (AlN) make the crystal mass of epitaxial film descend though the insert layer technology can reduce the generation of crackle simultaneously.The present invention can reduce the generation of crackle, can improve the crystal mass and the optical property of film again, and this is one of its advantage.Studies show that further the use of surfactant can improve the performance of stress compensation resilient coating, thereby make the performance improvement of epitaxial film.When not using activating agent, the surface of stress compensation resilient coating is more coarse, and the PL glow peak is very weak; When using activating agent, the surface of stress compensation resilient coating is more smooth, PL glow peak intensity height, and halfwidth is narrow.These experimental result instruction card surface-active agents can significantly reduce aluminum gallium nitride (AlGaN) surface formation energy, improve the surface activity of aluminium element when lower temperature, extenuate surface stress, make the stress compensation resilient coating be easy to form, and good crystal mass is arranged.
Claims (6)
1. the method for a growing flawless III group-III nitride on silicon substrate, it is characterized in that, between silicon substrate and III group-III nitride film, insert the stress compensation resilient coating at low temperatures by introducing activating agent, growth obtains the flawless III group-III nitride film that thickness≤1.5 micron, device can be used on the stress compensation resilient coating again.
2. the method for claim 1 is characterized in that, comprises step:
A) temperature is in the time of 1000 ~ 1100 ℃, in surface of silicon earlier behind the thick aluminum layer of deposition 1 ~ 2nm, and regrowth aluminum nitride buffer layer 20 ~ 30nm;
B) be cooled to 900～950 ℃, feed ammonia, trimethyl gallium, trimethyl aluminium or other unstripped gas, feed surfactant simultaneously, the aluminum gallium nitride of growing aluminum nitride or rich aluminium or boron nitride stress compensation resilient coating 50 ~ 500nm, the thickness of stress compensation resilient coating is regulated according to the flow velocity and the temperature of unstripped gas;
C) last, be warmed up to 1000 ~ 1100 ℃, growing flawless III group-III nitride film on the stress compensation resilient coating.
3. method as claimed in claim 2 is characterized in that, b) surfactant described in the step is the magnesium base, one or more in these three kinds of compounds of zinc-base and indium base; The aluminum gallium nitride of rich aluminium, aluminium content is greater than 20%.
4. method as claimed in claim 1 or 2, it is characterized in that, described stress compensation resilient coating, the little lattice constant of the III group-III nitride of growth thereon of the lattice constant of this layer material, crystal structure is six side's phases, introduce compression in the III group-III nitride film that can grow thereon, thereby the tension stress that compensation and silicon substrate thermal mismatching are introduced stops the generation and the expansion in Interface Crack source.
5. method as claimed in claim 1 or 2 is characterized in that, described III group-III nitride film is gallium nitride, aluminum gallium nitride, indium gallium nitrogen, aluminium gallium nitrogen a kind of thin-film material or their thin-film materials of being combined to form wherein.
6. method as claimed in claim 1 or 2 is characterized in that, the epitaxial growth equipment that is suitable for is metal organic-matter chemical vapour phase epitaxy, molecular beam epitaxy, hydride gas-phase epitaxy and ion sputtering.
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