CN100583397C - Doping method for III-v aluminum contained compound composed by direct or indirect band-gap - Google Patents
Doping method for III-v aluminum contained compound composed by direct or indirect band-gap Download PDFInfo
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- CN100583397C CN100583397C CN200510029096A CN200510029096A CN100583397C CN 100583397 C CN100583397 C CN 100583397C CN 200510029096 A CN200510029096 A CN 200510029096A CN 200510029096 A CN200510029096 A CN 200510029096A CN 100583397 C CN100583397 C CN 100583397C
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Abstract
The invention relates to the doping of ternary system III-V group aluminous arsenicals and antimonide formed by binary system with direct band gaps and binary system with indirect band gaps and its method, in particular the multi-system epitaxial as AlInAs, AlGaAs, and AlGaAsSb, as well as their donor doping in full range of aluminous components and relative method. The inventive characters comprise the donor doping method, in the range of full aluminous component (0<<XAl<<1), of three aluminous multi-system III-V group chemical compound epitaxial materials as aluminous indium arsenic, aluminous gallium arsenide, and aluminous gallium stibium, which grow epitaxially on the substrate of indium phosphide and gallium arsenide with gas-state source or solid-state source molecular beam. The donor doping gaps exist in full Al component range, while the stationary donor beam strength, the concentration of donor can be variable from 2-4 magnitude orders with the variation of the AL component. The three aluminous ternary system materials as mid-infrared, far infrared (THz) laser barrier layer and waveguide wall also are the barrier layer of high-speed device.
Description
Technical field
The present invention relates on indium phosphide, gallium arsenide substrate three kinds of donor doping and methods that contain the polynary based III-V group compound epitaxial material of aluminium with gaseous source or the full aluminium component of Solid State Source molecular beam epitaxial growth excursion.Relate to the III-V compounds of group ternary system epitaxial material AlInAs, the AlGaAs that form by direct band gap and indirect band gap binary system and AlGaAsSb polynary system epitaxial material or rather and in the donor doping and the method for full aluminium component excursion.Belong to semi-conducting material and devices field.
Background technology
InP base AlInAs/GaInAs is that INFRARED QUANTUM CASCADE LASERS preferred material among the 4-14 μ m, GaAs base AlGaAs/GaAs are that quantum cascade laser preferred material, GaSb base AlGaAsSb/InGaAsSb are infrared multiple quantum well laser preferred material among the 2-3.6 μ m to 30-300 μ m far infrared THZ tera hertz now.These three important materials that material system also is high-speed microwave, millimetric wave device.Al
xIn
1-xAs, Al
xGa
1-xAs, Al
xGa
1-xAs
0.02Sb
0.98In above-mentioned mid and far infrared laser as active area barrier material and waveguide wrapper material, and the barrier material of heterostructure high-speed electronic components [1. R.Koller, A.Tredicucci, F.Beltram, H.E.Beere, E.H.Linfield, G.Davies, D.A.Ritchie, S.Dillon, and C.Sirtori, " High-performance continuous-wave operation ofsuperlattice terahertz quantum-cascade lasers; " Appl.Phys.Lett.82,1518 (2003). 2. H.K.Choi, S.J.Eglash, and G.W.Turner, " Double-heterostructure diodelasers emitting at 3 μ m with a metastable GaInAsSb active and AlGaAsSbcladding layers, " Appl.Phys.Lett.74,1194 (1994) .].Usually the plain heterogeneous structure material of lattice match is selected at the trap and the base of laser active area for use, and lattice match doping heterogeneous structure material is selected at the trap of injection region and base for use, the barrier material layer Al of this moment
0.48In
0.52As, Al
0.25Ga
0.7As, Al
0.2Ga
0.8As
0.02Sb
0.98Be the direct band gap material, find unusual donor doping behavior [1. J.Faist, F.Capasso, D.L.Sivco, C.Sirtori, A.L.Hutchinson, and A.Y.Cho, " Quantum cascadelaser; " Science 264,553 (1994). 2. S.J.Eglash and H.K.Choi, " EfficientGaInAsSb/AlGaAsSb diode lasers emitting at 2.29 μ m; " Appl.Phys.Lett.57,1292 (1990). 3. L.Ajili, G.Scalari, D.Hofstetter, M Beck, J.Faist, H.Beere, G.Davies, E.Linfield, and D.Ritchie, " Continuous-wave operation of far-infraredquantum cascade lasers, " Electron.Lett.38,1675 (2002) .], the waveguide integument of multiple quantum well laser is then selected high potential barrier component, heavily doped material.
Improving the laser population inversion is the core key that improves laser performance.Just must realize effectively restriction for improving the gain of light to free carrier and photon, therefore, improving the light restriction of the free carrier injection efficiency of injection region, the refringence that increases base and trap, increase waveguide integument and reducing optical loss is that free carrier and photon are realized the effective key that limits, for this reason, the raising injection region is built layer donor doping concentration and in active area introducing strain structure, is improved a base layer Al component and become to attach most importance to scientific and technical crucial.But in red many outer multiple quantum well laser bodies, discovery is mixed among the tellurium n type AlGaAsSb and is had Te donor doping concentration limit in development GaSb base AlGaAsSb/InGaAsSb the semiduation on the last century the nineties, and donor doping concentration only is 1 * 10
17Cm
-3, think to be derived from the relation of tellurium saturated solubility limit in AlGaAsSb, and the relation that may have deep energy level, thereby become a long-term undecided and not revealed difficult problem.For light restriction and the minimizing optical loss that improves the waveguide integument, the nineties later stage in last century, in order to improve the band rank, increase infrared shortwave end 3-4 μ m InP base AlInAs/GaInAs quantum cascade laser in the active area gain of light and the development, and introduce strain compensation at active area AlInAs/GaInAs, the X of the Al component of AlInAs barrier layer from lattice match
Al=0.48 brings up to X
Al=0.53-0.65.The Al component of layer is directly relevant with refractive index because active area, injection/relaxation district, ducting layer are built, and the doping content of building layer is relevant with the injection efficiency of free carrier, and they have determined power, the threshold value of laser.Therefore, research Al
xIn
1-xAs/InP, Al
xGa
1-xAs/GaAs and Al
xGa
1-xAs
0.02Sb
0.98/ GaAs is in the donor doping and the method for full Al change of component scope (0≤Al≤1), correct announcement donor doping behavior to advance semi-conducting material and device science and technology development, to improve device quality imperative, has very urgent application value realistic.This is general thought of the present invention and starting point.
Summary of the invention
The object of the present invention is to provide the ternary based III-V group compound formed by direct band gap binary system and indirect band gap binary system doping and method in the excursion of full al composition.Specifically, be provided for preparing mid and far infrared wave band Multiple Quantum Well, quantum cascade laser, and n type InP base, GaAs base, the GaSb base of high-speed electronic components contain the donor doping method of aluminium ternary system barrier layer material.Its feature has comprised Al
xIn
1-xAs/InP, Al
xGa
1-xAs/GaAs and Al
xGa
1-xAs
0.02Sb
0.98/ GaAs is in the donor doping method of full al composition excursion (0≤Al≤1); The relation of donor doping concentration and aluminium component; The relation of donor doping concentration and ionization energy.
One, at full al composition excursion (0≤Al≤1) Al
xIn
1-xThe donor doping of As
With gas source molecular beam epitaxy technology (GSMBE) epitaxially grown Al on semi-insulating InP substrate
xIn
1-xThe donor doping of As material is characterized in that being is 0≤X in Al component excursion
Al≤ 1 donor doping method adopts silicon (Si) as n type (alms giver) dopant, and the temperature of dopant Si is 1190 ℃, and growth temperature is 455 ℃, keeps constant in whole samples of being grown.The extension bed thickness is 0.5-1.0 μ m.Survey epitaxy layer thickness with the step instrument, the Hall method is surveyed the donor doping concentration of epitaxial loayer, records Al component content among the AlInAs with x-ray double crystal diffraction swing curve.The doping result shows that Si is at Al
xIn
1-xDonor doping concentration among the As is " W " type with the variation of Al component and distributes and the donor doping crack, is that 0.537-0.574 and 0.596-0.611 scope exist two doping cracks at the Al component, and epitaxial loayer is semi-insulating or incorgruous conducting.Concrete doping process step sees embodiment 1 for details.
Two, at full al composition excursion (0≤Al≤1) Al
xGa
1-xThe donor doping method of As
With gas source molecular beam epitaxy technology epitaxially grown Al on the Semi-insulating GaAs substrate
xGa
1-xThe donor doping method of As material is characterized in that being is 0＜X in Al component excursion
Al＜1 donor doping method adopts silicon (Si) as n type (alms giver) dopant, and the temperature of n type dopant Si is 1190 ℃, and growth temperature is 610 ℃, keeps constant in whole samples of being grown.The extension bed thickness is 0.5-1.0 μ m.Survey epitaxy layer thickness with the step instrument,, measure Al component content among the AlGaAs with x-ray double crystal diffraction swing curve with the donor doping concentration of Hall method measurement epitaxial loayer.The doping result shows at GSMBE and mixes SiAl
xGa
1-xDonor doping concentration among the As is " W " type with the variation of Al component and distributes and the donor doping crack: at the Al component is 0＜X
Al＜0.24 scope, donor doping concentration are (3.8-3.1-1.8) * 10
18Cm
-3At the Al component is the 0.3-0.6 scope, and donor doping concentration is (0.78-1.8) * 10
17Cm
-3, reduce about 1-1.5 order of magnitude, be the 0.7-0.75 scope at the Al component, there is the doping crack, it is semi-insulating that epitaxial loayer is, and is the 0.76-0.97 scope at the Al component, and donor doping concentration is (1-2.6) * 10
18Cm
-3Concrete doping process step sees embodiment 2 for details.
Three, full al composition excursion (0≤Al≤1) Al
xGa
1-xAs
0.02Sb
0.98The donor doping method
With Solid State Source molecular beam epitaxy technique (SSMBE) epitaxially grown Al on the Semi-insulating GaAs substrate
xGa
1-xAs
0.02Sb
0.98The donor doping method of material is characterized in that being is 0≤X in Al component excursion
Al≤ 1 donor doping method, adopt tellurium (Te) as n type (alms giver) dopant, the temperature of n type dopant Te is 330 ℃, growth temperature is 530 ℃, or the temperature of n type dopant Te is 340 ℃, growth temperature is 500 ℃, and the component of arsenic is fixed on 0.02, and it is constant that above-mentioned growth conditions keeps in whole samples of being grown.The extension bed thickness is 1.5-1.7 μ m.Survey epitaxy layer thickness with the step instrument, record the donor doping concentration of epitaxial loayer, record Al with x-ray double crystal diffraction swing curve with the measurement of Hall method
xGa
1-xAs
0.02Sb
0.98Middle Al component content.The doping result shows that the temperature of (1) n type dopant Te is 330 ℃, and growth temperature is under 530 ℃ of conditions, mixes the n type Al of Te at SSMBE
xGa
1-xAs
0.02Sb
0.98Donor doping concentration in the layer is " W " type with the variation of Al component and distributes.At 0.17＜X
Al＜0.3 and 0.56＜X
Al＜0.71 place's donor doping concentration is minimum.At the Al component is the 0-0.17 scope, and donor doping concentration is (2.0-0.7) * 10
18Cm
-3At the Al component is the 0.56-0.71 scope, and donor doping concentration is (3.0-6.0) * 10
15Cm
-3, reduce about 3 orders of magnitude, be the 0.8-0.86 scope at the Al component, donor doping concentration is (1-2) * 10
18Cm
-3(2) temperature at dopant Te is 340 ℃, and growth temperature is under 500 ℃ of conditions, Al
xGa
1-xAs
0.02Sb
0.98Epitaxial material is at Al component excursion 0≤X
AlDonor doping concentration and Al in≤1
xGa
1-xAs
0.02Sb
0.98The relation of layer Al component.At 0.24＜X
Al＜0.39 and 0.5＜X
AlThere are two donor doping cracks in＜0.6 place, and epitaxial loayer is semi-insulating electrology characteristic.Concrete doping process step sees embodiment 3 for details.
The present invention is applicable to that the optimal design of the multiple quantum well laser relevant with above-mentioned material, quantum cascade laser, high strain microwave, millimeter wave material and device and quality improve, but its thought also is applicable to other III-V compound material and device.
Description of drawings
Fig. 1 is for mixing Si n-Al
xIn
1-xThe relation of the free electronic concentration of As and AlAs component
Fig. 2 is for mixing Si n-Al
xGa
1-xThe relation of the free electronic concentration of As and AlAs component
Fig. 3 is for mixing Te n-Al
xGa
1-xAs
0.02Sb
0.98In growth temperature is that 530 ℃, Te furnace temperature are the relation of 330 ℃ free electronic concentration and AlSb component
Fig. 4 is for mixing Te n-Al
xGa
1-xAs
0.02Sb
0.98In growth temperature is that 500 ℃, Te furnace temperature are the relation of 340 ℃ free electronic concentration and AlSb component
Fig. 5 is for mixing Te n-Al
xGa
1-xAs
0.02Sb
0.98The alms giver's ionization energy of Te and the relation of AlSb component
Fig. 6 is the AlGaAsSb/InGaAsSb laser structure that works in 2.0 μ m
Fig. 7 is AlGaAsSb/InGaAsSb ridge waveguide laser pulse Output optical power-electric current (P-I) curve of 2.0 μ m under the different temperatures
Embodiment
Further specifying substantive distinguishing features of the present invention and obvious improvement in conjunction with the accompanying drawings below by embodiment, but limit the present invention absolutely not, also is that the present invention absolutely not only is confined to embodiment.
Embodiment 1: adopt GSMBE growing method epitaxial growth Al on semi-insulating InP substrate
xIn
1-xThe As material, the step of concrete growth is:
1. will be contained in the Sample Room that the semi-insulating InP substrate of Fe is put into the GSMBE system of mixing in the molybdenum holder.Vacuumize with turbomolecular pump.
2. treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of GSMBE system, be warming up to 250 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption and reduce to 50-100 ℃ again.The electron gun degasification: when pretreatment chamber's degasification, the indium of growth room, aluminium, dopant silicon, phosphine, the degasification simultaneously of arsine pyrolysis furnace.Electron gun stove shutter is opened during degasification, 15-30 minute degasification time.Usually the degasification temperature compares the high 30-50 of temperature ℃ that adopts when growing.The electron gun indium is at 900 ℃, and aluminium was 1200 ℃ of difference degasification 20-30 minute.With the line of line instrumentation indium and aluminium, draw indium, aluminium furnace temperature and indium, aluminium beam intensity relation and with the relation of AlInAs growth rate.Silicon stove degasification temperature is 1230-1250 ℃, degasification half an hour, reduces to 1190 ℃ then.In our V80 GSMBE system, the cracking temperature of phosphine is 1000 ℃, and the degasification temperature is 1050 ℃, degasification half an hour.Degasification finishes, and closes the electron gun stove and opens the door.
With substrate transfer to the sample heating station of GSMBE system growth room, close after observing InP surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, feed the 500Torr arsine, the vacuum degree of growth room is (1-3) * 10
-5, monitor surface desorption with RHEED when rising to 450-480 ℃, treat that surface texture transfers 4 * 4 o'clock surfaces to by 2 * 2 and is absorbed in surperficial CO, CO
2And P
2O
5Desorb stops the 3-5 branch and makes its abundant desorb.Usually the desorption temperature of mixing the semi-insulating InP of Fe is 480-500 ℃.
4. underlayer temperature is reduced to 455 ℃, when being the AlInAs growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, wait to grow temperature and indium furnace temperature, aluminium furnace temperature, silicon furnace temperature stable after, open arsine, close phosphine, open In, Al and As electron gun stove shutter again, beginning epitaxial growth Al
xIn
1-xAs, epitaxial growth speed is 0.7-0.9 μ m/ hour.Epitaxial growth finishes, and closes indium stove, aluminium stove, silicon stove shutter, reduces to 500 ℃ simultaneously.Turn off arsine when substrate heater is cooled to 300 ℃, pump is walked growth room's residue arsine simultaneously, and the arsine pyrolysis furnace maintains 1000 ℃.Reduce to 50-100 ℃ when underlayer temperature, epitaxial wafer is passed to Sample Room.This moment, arsine pyrolysis furnace temperature was reduced to 600 ℃.
5. the taking-up epitaxial wafer carries out Al component, epitaxy layer thickness and electrical parameter test.
Fig. 1 is the prepared Al of present embodiment
xIn
1-xThe As epitaxial material is at Al component excursion 0≤X
AlDonor doping concentration and Al in≤1
xIn
1-xThe relation of A layer Al component.From the visible Si of Fig. 1 at Al
xIn
1-xDonor doping concentration among the As is " W " type with the variation of Al component and distributes and the donor doping crack, is that 0.537-0.574 and 0.596-0.611 scope exist two doping cracks at the Al component, and epitaxial loayer is semi-insulating or incorgruous conducting.
Embodiment 2: adopt GSMBE growing method epitaxial growth Al on the GaAs substrate
xGa
1-xThe As material, the step of its concrete growth is:
1. will be contained in the Sample Room of the Semi-insulating GaAs substrate threading GSMBE system in the molybdenum holder.Vacuumize with turbomolecular pump.
2. treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of GSMBE system, be warming up to 350 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption and reduce to 50-100 ℃ again.
The electron gun degasification: when pretreatment chamber's degasification, the aluminium of growth room, gallium, dopant silicon, the degasification simultaneously of arsine pyrolysis furnace.Electron gun stove shutter is opened during degasification, 15-30 minute degasification time.Usually the degasification temperature compares the high 30-50 of temperature ℃ that adopts when growing.The electron gun gallium is at 1030 ℃, and aluminium was 1200 ℃ of difference degasification 20-30 minute.Silicon stove degasification temperature is 1230-1250 ℃, degasification half an hour, reduces to 1190 ℃ then.Arsine pyrolysis furnace intensification degasification simultaneously half an hour, whether cracking is complete with online four-electrode spectrum observation arsine when rising to 900 ℃, does not occur the arsine spectral line on spectrogram, shows that cracking is complete, and arsine can fully be cracked into As under this temperature
2, this temperature is decided to be cracking temperature, being higher than 50 ℃ of degasification of cracking temperature, reduce to cracking temperature then.In our V80 GSMBE system, the cracking temperature of arsine is 1000 ℃, and the degasification temperature is 1050 ℃.Degasification finishes, and closes the electron gun stove and opens the door.
With substrate transfer to the sample heating station of GSMBE system growth room, close after observing GaAs surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, feed 500Torr arsine (AsH
3), the vacuum degree of growth room is (1-3) * 10
-5, monitor surface desorption with RHEED when rising to 580-610 ℃, treat that surface texture occurs at 2 * 4 o'clock, shows the CO, the CO that are absorbed in the surface
2With the oxide desorb of arsenic, stop and made its abundant desorb in 3-5 minute.Usually the desorption temperature of Semi-insulating GaAs is 620-630 ℃.
4. underlayer temperature is reduced to 610 ℃, when being the AlGaAs growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, after wait to grow temperature and gallium furnace temperature, aluminium furnace temperature, silicon furnace temperature are stable, open Ga, Al and Si electron gun stove shutter, beginning epitaxial growth Al
xGa
1-xAs, epitaxial growth speed is 0.7-0.9 μ m/ hour.Extension finishes, and closes gallium stove, aluminium stove, silicon stove shutter, and the gallium stove is reduced to 600 ℃, and the aluminium stove is reduced to 900 ℃, and the silicon stove is reduced to 900 ℃.Turn off arsine when substrate heater is cooled to 300 ℃, pump is walked growth room's residue arsine simultaneously, and the arsine pyrolysis furnace maintains 1000 ℃.Reduce to 50-100 ℃ when underlayer temperature, epitaxial wafer is passed to Sample Room.This moment, arsine pyrolysis furnace temperature was reduced to 600 ℃.
5. the taking-up epitaxial wafer carries out Al component, epitaxy layer thickness and electrical parameter test.
Fig. 2 is the prepared Al of present embodiment
xGa
1-xThe As epitaxial material is at Al component excursion 0＜X
AlDonor doping concentration and Al in≤1
xGa
1-xThe relation of A layer Al component.As seen mix Si Al at GSMBE from Fig. 2
xGa
1-xDonor doping concentration among the As is " W " type with the variation of Al component and distributes and the donor doping crack: at the Al component is 0＜X
Al＜0.24 scope, donor doping concentration are (3.8-3.1-1.8) * 10
18Cm
-3At the Al component is the 0.3-0.6 scope, and donor doping concentration is (0.78-1.8) * 10
17Cm
-3, reduce about 1-1.5 order of magnitude, be the 0.7-0.75 scope at the Al component, there is the doping crack, it is semi-insulating that epitaxial loayer is, and is the 0.76-0.97 scope at the Al component, and donor doping concentration is (1-2.6) * 10
18Cm
-3
Embodiment 3: adopt SSMBE method epitaxial growth Al on the Semi-insulating GaAs substrate
xGa
1-xAs
0.02Sb
0.98Material, the step of its concrete growth is:
1. will be contained in the Sample Room of the Semi-insulating GaAs substrate threading SSMBE system in the molybdenum holder.Vacuumize with turbomolecular pump.
2. treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of SSMBE system, be warming up to 350 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption; Reduce to 50-100 ℃.The electron gun degasification: when pretreatment chamber's degasification, the aluminium of growth room, gallium, arsenic, antimony, the degasification simultaneously of dopant tellurium.Electron gun stove shutter is opened during degasification, 15-30 minute degasification time.The temperature that adopts when the degasification temperature is than growth usually is high 30 ℃.The electron gun gallium is at 1030 ℃, and aluminium is at 1200 ℃, antimony at 500 ℃ and tellurium 250 ℃ of degasification 20-30 minute respectively.
With substrate transfer to the sample heating station of SSMBE system growth room, close after observing GaAs surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, open arsenic stove shutter.Usually the desorption temperature of Semi-insulating GaAs is 620-630 ℃.
4. underlayer temperature is reduced to 530 ℃ or 500 ℃, wherein underlayer temperature is Al
xGa
1-xAs
0.02Sb
0.98During growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, after wait to grow temperature and gallium furnace temperature, aluminium furnace temperature, arsenic stove, tellurium furnace temperature are stable, open electron gun stove shutter, beginning epitaxial growth Al
xGa
1-xAs
0.02Sb
0.98, epitaxial growth speed is 1.5 μ m/ hours.Extension finishes, and closes shutter.Reduce to 50-100 ℃ when underlayer temperature, epitaxial wafer is passed to Sample Room.
5. the taking-up epitaxial wafer carries out Al component, epitaxy layer thickness and electrical parameter test.
Fig. 3 is 330 ℃ for the temperature of the prepared n type dopant Te of present embodiment, and growth temperature is under 530 ℃, Al
xGa
1-xAs
0.02Sb
0.98Epitaxial material is at Al component excursion 0≤X
AlDonor doping concentration and Al in≤1
xGa
1-xAs
0.02Sb
0.98The relation of layer Al component.As seen mix the n type Al of Te at GSMBE from Fig. 3
xGa
1-xAs
0.02Sb
0.98Donor doping concentration in the layer is " W " type with the variation of Al component and distributes.At 0.17＜X
Al＜0.3 and 0.56＜X
Al＜0.71 place's donor doping concentration is minimum.At the Al component is the 0-0.17 scope, and donor doping concentration is (2.0-0.7) * 10
18Cm
-3At the Al component is the 0.56-0.71 scope, and donor doping concentration is (3.0-6.0) * 10
15Cm
-3, reduce about 3 orders of magnitude, be the 0.8-0.86 scope at the Al component, donor doping concentration is (1-2) * 10
18Cm
-3Fig. 4 is 340 ℃ for the temperature of the dopant Te of present embodiment preparation, and growth temperature is under 500 ℃, Al
xGa
1-xAs
0.02Sb
0.98Epitaxial material is at Al component excursion 0≤X
AlDonor doping concentration and Al in≤1
xGa
1-xAs
0.02Sb
0.98The relation of layer Al component.At 0.24＜X
Al＜0.39 and 0.5＜X
AlThere are two donor doping cracks in＜0.6 place, and epitaxial loayer is semi-insulating electrology characteristic.
Fig. 5 is the Al of present embodiment preparation
xGa
1-xAs
0.02Sb
0.98Alms giver's tellurium ionization energy E
DRelation with the Al component.From scheming the Al of visible different al component
xGa
1-xAs
0.02Sb
0.98Alms giver's ionization energy E of sample
DBeing " M " type with the Al component distributes.Its highest E
DThe value with minimum donor doping concentration Al component of living between corresponding.
Fig. 6 is that we have designed wavelength is the AlGaAsSb/InGaAsSb laser structure of 2.0 μ m according to Fig. 3,4 result.
Waveguide integument Al under the visible n type that we choose of Fig. 6
0.4-0.45Ga
0.6As
0.04Sb
0.96The Al component. not in the donor doping crack.Fig. 7 develops the Output optical power and the current relationship of the AlGaAsSb/InGaAsSb room temperature pulsed operation laser of 2.0 μ m with this structure.
Claims (9)
1, a kind of directly and the donor doping method of the III-V family aluminum contained compound formed of indirect band gap, adopt gas source molecular beam epitaxy method epitaxial growth Al on semi-insulating InP substrate
xIn
1-xThe As material is characterized in that the step of concrete growth is:
(1) will be contained in the Sample Room that the semi-insulating InP substrate of Fe is put into the gas source molecular beam epitaxy system of mixing in the molybdenum holder, and vacuumize with turbomolecular pump;
(2) treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of gas source molecular beam epitaxy system, be warming up to 250 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption, reduce to 50-100 ℃ then;
The electron gun degasification: when pretreatment chamber's degasification, the indium of growth room, aluminium, dopant silicon, phosphine, the degasification simultaneously of arsine pyrolysis furnace; Electron gun stove shutter is opened during degasification, 15-30 minute degasification time; The degasification temperature compares the high 30-50 of temperature ℃ that adopts when growing; The electron gun indium is at 900 ℃, and aluminium was 1200 ℃ of difference degasification 20-30 minute; With the line of line instrumentation indium and aluminium, draw the relation and and the Al of indium, aluminium furnace temperature and indium, aluminium beam intensity
xIn
1-xThe relation of As growth rate; Silicon stove degasification temperature is 1230-1250 ℃, degasification half an hour, reduces to 1190 ℃ then; In described gas source molecular beam epitaxy system, the cracking temperature of phosphine is 1000 ℃, and the degasification temperature is 1050 ℃, degasification half an hour; Degasification finishes, and closes the electron gun stove and opens the door;
(3) with substrate transfer to the sample heating station of gas source molecular beam epitaxy system growth room, close after observing InP surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, feed the 500Torr phosphine, the vacuum degree of growth room is (1-3) * 10
-5Torr is monitored surface desorption with RHEED when rising to 450-480 ℃, treats that surface texture transfers at 4 * 4 o'clock by 2 * 2, is absorbed in CO, the CO on surface
2And P
2O
5Desorb stops and made its abundant desorb in 3-5 minute; The desorption temperature of mixing the semi-insulating InP of Fe is 480-500 ℃;
(4) underlayer temperature is reduced to 455 ℃, be Al
xIn
1-xDuring the As growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, after wait to grow temperature and indium furnace temperature, aluminium furnace temperature, silicon furnace temperature are stable, open arsine, close phosphine, open In, Al and Si electron gun stove shutter again, beginning epitaxial growth Al
xIn
1-xAs, epitaxial growth speed is 0.7-0.9 μ m/ hour; Epitaxial growth finishes, and closes the shutter of indium stove, aluminium stove and silicon stove, reduces to 500 ℃ simultaneously; Turn off arsine when substrate heater is cooled to 300 ℃, pump is taken growth room's residue arsine away simultaneously, and the arsine pyrolysis furnace maintains 1000 ℃; Reduce to 50-100 ℃ when underlayer temperature, epitaxial wafer is passed to Sample Room; This moment, arsine pyrolysis furnace temperature was reduced to 600 ℃.
2, donor doping method as claimed in claim 1 is characterized in that epitaxial growth Al on semi-insulating InP substrate
xIn
1-xThe As material is to adopt Si as donor dopant, and the temperature of n type dopant Si is 1190 ℃, and growth temperature is 455 ℃, and Si is at Al
xIn
1-xDonor doping concentration among the As is " W " type with the variation of Al component and distributes and two donor doping cracks; Epitaxial loayer is semi-insulating or incorgruous conducting.
3, donor doping method as claimed in claim 2 is characterized in that described two alms giver's band gap are respectively X
AlComponent is 0.537-0.574 and 0.596-0.611.
4, a kind of directly and the donor doping method of the III-V family aluminum contained compound formed of indirect band gap, adopt gas source molecular beam epitaxy method epitaxial growth Al on the Semi-insulating GaAs substrate
xGa
1-xThe As material is characterized in that the step of concrete growth is:
(1) will be contained in the Sample Room that Semi-insulating GaAs substrate in the molybdenum holder is put into the gas source molecular beam epitaxy system, and vacuumize with turbomolecular pump.
(2) treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of gas source molecular beam epitaxy system, be warming up to 350 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption, reduce to 50-100 ℃;
The electron gun degasification: when pretreatment chamber's degasification, the indium of growth room, dopant silicon, the degasification simultaneously of arsine pyrolysis furnace; Electron gun stove shutter is opened during degasification, 15-30 minute degasification time; The degasification temperature compares the high 30-50 of temperature ℃ that adopts when growing; The electron gun gallium is at 1030 ℃, and aluminium was 1200 ℃ of difference degasification 20-30 minute; Silicon stove degasification temperature is 1230-1250 ℃, degasification half an hour, reduces to 1190 ℃ then; The degasification of As alkane pyrolysis furnace intensification simultaneously half an hour, whether cracking is complete with online four-electrode spectrum observation As alkane when rising to 900 ℃, does not occur the arsine spectral line on spectrogram, shows that cracking is complete, and arsine can fully be cracked into As under this temperature
2, this temperature is decided to be cracking temperature, in 50 ℃ of degasification of master-hand's cracking temperature, reduce to cracking temperature then, in described gas source molecular beam epitaxy system, the cracking temperature of arsine is 1000 ℃, the degasification temperature is 1050 ℃; Degasification finishes, and closes the electron gun stove and opens the door;
(3) with substrate transfer to the sample heating station of GSMBE system growth room, close after observing GaAs surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, feed the 500Torr arsine, the vacuum degree of growth room is (1-3) * 10
-5Torr is monitored surface desorption with RHEED when rising to 580-610 ℃, treats that surface texture occurs at 2 * 4 o'clock, is absorbed in CO, the CO on surface
2With the oxide desorb of arsenic, stop and made its abundant desorb in 3-5 minute, the desorption temperature of Semi-insulating GaAs is 620-630 ℃;
(4) underlayer temperature is reduced to 610 ℃, be Al
xGa
1-xDuring the As growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, after wait to grow temperature and gallium furnace temperature, aluminium furnace temperature, silicon furnace temperature are stable, open Ga, Al and Si electron gun stove shutter, beginning epitaxial growth Al
xGa
1-xAs, epitaxial growth speed is 0.7-0.9 μ m/ hour; Extension finishes, and closes gallium stove, aluminium stove, silicon stove shutter, and the gallium stove is reduced to 600 ℃, and the aluminium stove is reduced to 900 ℃, and the silicon stove is reduced to 900 ℃; Turn off arsine when substrate heater is cooled to 300 ℃, pump is taken growth room's residue arsine away simultaneously, and the arsine pyrolysis furnace maintains 1000 ℃; When underlayer temperature falls 50-100 ℃, epitaxial wafer is passed to Sample Room, this moment, arsine pyrolysis furnace temperature was reduced to 600 ℃.
5, donor doping method as claimed in claim 4 is characterized in that epitaxial growth Al on the Semi-insulating GaAs substrate
xGa
1-xThe As material is to adopt Si as donor dopant, and the temperature of n type dopant Si is 1190 ℃, and growth temperature is 610 ℃, and the donor concentration of doping is with X
AlThe component variation is " W " type and distributes, and at X
AlComponent is to have the donor doping crack in the 0.70-0.75 scope, and epitaxial loayer is half insulation.
6, as by the described donor doping method of claim 5, it is characterized in that at X
AlComponent is the 0.3-0.6 scope, and donor doping concentration is (0.78-1.8) * 10
17Cm
-3At X
AlComponent is the 0.76-0.97 scope, and donor doping concentration is (1-2.6) * 10
18Cm
-3
7, a kind of directly and the donor doping method of the III-V family aluminum contained compound formed of indirect band gap, adopt Solid State Source molecular beam epitaxial method epitaxial growth Al on the Semi-insulating GaAs substrate
xGa
1-xAs
0.02Sb
0.98Material is characterized in that the step of concrete growth is:
(1) will be contained in the Sample Room that Semi-insulating GaAs substrate in the molybdenum holder is put into the Solid State Source molecular beam epitaxy system, and vacuumize with turbomolecular pump;
(2) treat that Sample Room vacuum degree reaches 10
-6During Torr, with substrate transfer to the heating station of pretreatment chamber of SSMBE system, be warming up to 350 ℃, kept 2 hours, slough the aqueous vapor of surface adsorption, reduce to 50-100 ℃;
The electron gun degasification: when pretreatment chamber's degasification, the aluminium of growth room, gallium, arsenic, antimony, the degasification simultaneously of dopant tellurium; Electron gun stove shutter is opened during degasification, and 15-30 minute degasification time, the temperature that adopts during the growth of degasification temperature ratio is high 30 ℃; The electron gun gallium is at 1030 ℃, and aluminium is at 1200 ℃, antimony at 500 ℃ and tellurium 250 ℃ of degasification 20-30 minute respectively;
(3) with substrate transfer to the sample heating station of Solid State Source molecular beam epitaxy system growth room, close after observing GaAs surface hot spot with RHEED, begin to heat up, when waiting to rise to 300 ℃, open arsenic stove shutter, the desorption temperature of Semi-insulating GaAs is 620-630 ℃,
(4) will mix underlayer temperature and reduce to 530 ℃, donor dopant tellurium furnace temperature is stabilized in 330 ℃ or underlayer temperature reduced to 500 ℃, and donor dopant tellurium furnace temperature is stabilized in 340 ℃, and wherein underlayer temperature is Al
xGa
1-xAs
0.02Sb
0.98During growth temperature, simultaneously with the specimen holder steering surface to the electron gun stove, after wait to grow temperature and gallium furnace temperature, aluminium furnace temperature, arsenic stove, antimony stove, tellurium furnace temperature are stable, open electron gun stove shutter, beginning epitaxial growth Al
xGa
1-xAs
0.02Sb
0.98, epitaxial growth speed is 1.5 μ m/ hours; Extension finishes, and closes shutter; Reduce to 50-100 ℃ when underlayer temperature, epitaxial wafer is passed to Sample Room.
8, use donor doping method as claimed in claim 7, it is characterized in that epitaxial growth Al on the Semi-insulating GaAs substrate
xGa
1-xAs
0.02Sb
0.98Material is to adopt tellurium as donor dopant, and donor doping concentration is " W " type with the variation of Al component and distributes and the donor doping crack: the temperature of (1) dopant Te is 330 ℃, and growth temperature is 530 ℃ of series: at 0.17＜X
Al＜0.3 and 0.56＜X
Al＜0.71 place's donor doping concentration is minimum; At the Al component is the 0-0.17 scope, and donor doping concentration is (2.0-0.7) * 10
18Cm
-3At the Al component is the 0.56-0.71 scope, and donor doping concentration is (3.0-6.0) * 10
15Cm
-3, reduce by 3 orders of magnitude, be the 0.8-0.86 scope at the Al component, donor doping concentration is (1-2) * 10
18Cm
-3(2) temperature of dopant Te is 340 ℃, when growth temperature is 500 ℃, at 0.24＜X
Al＜0.39 and 0.5＜X
AlThere are two donor doping cracks in＜0.6 place, and epitaxial loayer is half insulation; Alms giver's ionization energy and Al component are the M type and distribute.
9,, it is characterized in that alms giver's ionization energy peak and minimum donor doping concentration Al component of living in is interval corresponding by the described donor doping method of claim 8.
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| The behavior of dopant incorporation andinternalstraininAlxGa1-xAs0.03Sb0.97 grown by molecularbeam epitaxy. LI AZ,WANG JX,ZHENG YL,et al.JOURNAL OF CRYSTAL GROWTH,Vol.127 No.1-4. 1993 * |
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