CN101538700A - Method and equipment for preparing II type quantum well with molecular beam epitaxial process - Google Patents
Method and equipment for preparing II type quantum well with molecular beam epitaxial process Download PDFInfo
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- CN101538700A CN101538700A CN200910020717A CN200910020717A CN101538700A CN 101538700 A CN101538700 A CN 101538700A CN 200910020717 A CN200910020717 A CN 200910020717A CN 200910020717 A CN200910020717 A CN 200910020717A CN 101538700 A CN101538700 A CN 101538700A
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Abstract
The invention relates to a method and equipment for preparing an II type quantum well with a molecular beam epitaxial process. A buffer layer, an isolation layer, a potential well layer, a potential barrier layer, a potential well layer, an isolation layer and a covering layer are grown on a substrate. The used equipment is a double-growing-chamber molecular beam epitaxial system which comprises an III-V family growing chamber and an II-VI family growing chamber, wherein each growing chamber is provided with a solid source evaporator, a five-dimensional adjustable sample rack, a four-pole mass spectrometry, a reflecting type high-energy electronic diffraction instrument, and the like; the two growing chambers are connected by an ultra-high vacuum transmission pipeline so as to facilitate the transmission of samples; the ultra-high vacuum transmission pipeline is provided with a gas pumping device and respectively separated from the two growing chambers connected to both ends by gate valves; and the sample rack and the solid source evaporator are respectively connected with the gas pumping device. The equipment can be used for the field of photovoltaic devices, such as optical communication, quantum information storage and process, semiconductor lasers, and the like.
Description
Technical field
The present invention relates to a kind of II of preparation type quantum well method and apparatus, particularly a kind of method and apparatus for preparing a kind of ZnSe/BeTe II type quantum well that constitutes by the II-VI compound semiconductor with molecular beam epitaxy accretion method.
Background technology
Because limited electronics, photon in the nanometer quantum structure present many and they new quantum appearance and effect very different, that physical content is very abundant in three-dimensional macrostructure, therefore, just cause people's extensive concern and keen interest more and more for the optical research in low dimension semiconductor field, and doing a large amount of work for this reason.
Quantum well structure is to observe and study the high-density phenomenon (as charged exciton, excitonic molecule, exciton polymkeric substance and Bose-Einstein condensation etc.) one of important means, just playing a part to become more and more important for luminous mechanism and the origin understood and verify the many two-phonon process that comprise spin state.The II type quantum well structure that mainly contains I type (type-I) quantum well and form according to disclosed quantum well structure kind by the III-V compound semiconductor.U.S.'s academic journal magazine " Physical Review B " (calendar year 2001, the 64th volume, the 245339th page, " Time-resolved photoluminescence of InxGal-xN/GaN multiplequantum well structures:Effect of Si doping in the barriers ") experimental result (C.K.Choi with I type quantum well structure research photoluminescence disclosed, et al., 64 (2001) 245339).But because the electronics and the hole of being excited to produce in this I type quantum well structure are to be in the same trap layer, their wave function almost completely overlaps, so the space is directly again in conjunction with (spatially direct recombination) luminescent lifetime less (generally being about psec (ps) order of magnitude at low temperatures).Therefore there is weak point in this structure for observing the condensed state phenomenon.U.S.'s academic journal magazine " Physical Review B " (2000, the 61st volume, the 10782nd page, " Theory of electronic and optical properties of bulk AlSb and InAs andInAs/AlSb superlattices ") experimental result (G.Theodorou of the II type quantum well structure research photoluminescence of forming with the III-V compound semiconductor disclosed, et al., 61 (2000) 10782).(the conduction band drop is about Δ E but because this structure has less conduction band (or valence band) drop at the heterojunction boundary place
C=1.35eV, the valence band drop is about Δ E
V=0.13eV), make the electronics be excited to produce still have bigger wave function overlapping at the interface with (being that electronics is in different trap layers respectively with the hole) after spatial isolation takes place in the hole, therefore though the life-span of the direct recombination radiation in space in the life-span of its indirect recombination radiation in space and the I type quantum well structure is compared bigger increase has been arranged, the condensed state phenomenon is still undesirable for observing.
Summary of the invention
For defective and the deficiency that overcomes existing structure, the present invention proposes a kind of method for preparing II type quantum well structure with II-VI compound semiconductor (ZnSe and BeTe) by molecular beam epitaxy (MBE) growth method.
A kind ofly prepare the method for II type quantum well, step following (with reference to the accompanying drawings 1 and accompanying drawing 2) with molecular beam epitaxial process:
1, the gallium arsenide substrate with (001) orientation is fixed in the holder of molybdenum (Mo) sample with indium (In);
2, logical cooled with liquid nitrogen growth room, confirm III-V family growth room's vacuum tightness be below 1 * 10-10 Torr after, by the magnetic force driven rod sample is sent in the III-V family growth room; With the sample holder, the K-cell container of As solid source is housed and the K-cell container heat temperature raising of Ga solid source is housed, the temperature that makes it to reach setting is respectively 300 ℃, 100 ℃ and 750 ℃;
3, adjust the temperature of As source K-cell container, after making it to begin to warm to 295 ℃ by 100 ℃, temperature with sample holder and Ga source K-cell container is set at 550 ℃ and 915 ℃ respectively again, and begin to heat up, open the baffle plate of As source K-cell container simultaneously, the As molecular beam is radiated on the substrate, the evaporation of the substrate surface As cause because of underlayer temperature raises with compensation, and make the evaporation of As on the substrate surface reach balance with adhering to;
4, treat that Ga source K-cell container rises to 915 ℃ after, again the sample holder is warming up to 620 ℃, can on [110] direction, observe by reflected high energy electron diffraction (RHEED instrument) instrument between temperature raising period, striped occurs if can observe clearly, the oxide compound of having removed substrate surface under this temperature then is described and obtains the orderly substrate surface of cleaning;
5, the generation of GaAs buffer layer: open the baffle plate that temperature has risen to 915 ℃ Ga source K-cell container, the Ga molecular beam is radiated on the substrate; This moment, the molecular beam of Ga and As was radiated at substrate surface simultaneously, the growth of GaAs buffer layer begins, growth time is 24 ~ 120 minutes, the thickness of GaAs buffer layer can reach 200 ~ 1000nm, turn off the Ga source this moment, and the temperature of Ga source K-cell container reduced to 750 ℃ by 915 ℃, reduce to 300 ℃ afterwards again, and a cleaning, smooth and orderly surface are arranged by the substrate that the RHEED instrument can be observed this moment;
6, stablize 5 minutes after, underlayer temperature is reduced to 580 ℃ gradually by 620 ℃, cool-down method is a staged, promptly each cooling is set at falls 5 ℃, sets next time when reaching design temperature again, divides and finishes cooling 8 times; After the cooling beginning, when observing image and do not have what ANOMALOUS VARIATIONS, the As source is turned off, and the As source temperature is transferred to 100 ℃ by 295 ℃ by the RHEED instrument;
7, underlayer temperature is reduced to 500 ℃ gradually by 580 ℃, cool-down method is a staged, falls 10 ℃ at every turn; Afterwards, again underlayer temperature is reduced to 300 ℃ gradually by 500 ℃, whole temperature-fall period divides and carries out for 10 times, and each cooling is spaced apart 20 ℃;
8, observe RHEED instrument image and do not have what ANOMALOUS VARIATIONS, can turn off the RHEED instrument this moment, after the vacuum tightness of determining III-V family growth room becomes below 7.5 * 10-9Torr, turn off being used for the power supply of heated substrate, and prepare substrate is passed to II-VI family growth room by the high vacuum transmission pipeline;
9, be below 1 * 10-10Torr and the temperature in the Zn in the II-VI family growth room, Be, Te, Se and Mg source is heated to respectively after 150,820,150,50 and 200 ℃ in the vacuum tightness of determining II-VI family growth room, again substrate be sent to II-VI family growth room by III-V family growth room by ultra-high vacuum transmission pipeline; Substrate is warming up to 300 ℃ ~ 350 ℃, and the temperature in Zn, Be, Te, Se and Mg source is warming up to 307,1065,320,202 and 322.5 ℃ more respectively;
10, the generation of BeTe buffer layer: after the temperature in Be, Te source reaches 1065 and 320 ℃ respectively, stablized 30 minutes, open the baffle plate in Be, Te source, Be molecular beam and Te molecular beam are radiated at the surface of substrate, and the BeTe buffer layer begins to grow this moment; Monitor (perhaps, set, control, down together) in real time with the RHEED instrument with computer according to the growth rate of each solid source that records in advance before the growth, when the growth thickness of BeTe buffer layer is about 5ML, growth ending is turned off the Be source then earlier, turns off the Te source subsequently again;
11, Zn
0.77Mg
0.15Be
0.08The growth of Se sealing coat: open the baffle plate in Zn source earlier, the baffle plate of opening Se, Be and Mg source again carries out Zn
0.77Mg
0.15Be
0.08The growth of Se sealing coat, there are this moment Zn molecular beam, Se molecular beam, Be molecular beam and Mg molecular beam to be radiated at the surface of substrate simultaneously respectively, when the sealing coat growth thickness is 200～1000nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 5～10 seconds;
12, the growth of ZnSe potential well layer: open Zn, Se source, make the two be radiated on the substrate surface simultaneously, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is 4～80ML, growth ending, close the Se source earlier, after about 5～10 seconds, close the Zn source again, so that form rich Zn upper layer;
13, the temperature in the growth of BeTe barrier layer: Be, Te source remains on 1065 and 320 ℃ respectively, open the Te source, through opening the Be source BeTe barrier layer that begins to grow after 5～10 seconds again, when the thickness of BeTe layer growth is about 10ML, growth ending is closed the Be source earlier, closes the Te source again after about 5～10 seconds, so that form rich Te upper layer, can reduce to 150 ℃ this moment with the temperature in Te source; Above-mentioned process of growth can be between ZnSe and BeTe the chemical bond that obtains the Zn-Te form at the interface;
14, the growth of ZnSe potential well layer: open the Zn source, opened Se source growing ZnSe potential well layer again after 5～10 seconds, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is 4～80ML, growth ending is successively closed Se source and Zn source; Above-mentioned process of growth can be between BeTe and ZnSe the chemical bond that obtains the Te-Zn form at the interface;
15, the process of growth of the sealing coat of repeating step 11 can obtain the thick Zn of 200～1000nm
0.77Mg
0.15Be
0.08The Se sealing coat; To close Se, Be, Mg source earlier during growth ending, close the Zn source again after about 10 seconds, can not corroded with the protection sample at grown on top one deck Zn of sample as tectum like this; Behind the growth ending, underlayer temperature is made as 150 ℃ and make it cooling, also the temperature in Zn, Se, Be and Mg source is set at simultaneously 100,50,820 and 150 ℃ and make it cooling respectively; Reduce to after 150 ℃ and the temperature of confirming the Se source reduce to below 100 ℃ when underlayer temperature, sample is taken out from the growth room, can obtain the quantum-well materials of complete ZnSe/BeTe/ZnSe form.
By above-mentioned process of growth, we can obtain the quantum well structure (that is, two potential well layers and a barrier layer being arranged) of ZnSe/BeTe/ZnSe form.If repeatedly repeat the process of growth of sputtering ZnS e and BeTe and be step 13 to step 14, we can obtain with ZnSe/BeTe is the superstructure in cycle; If repeatedly repeating step 13 is to step 15, we also can obtain Multiple Quantum Well.
RHEED instrument used in the present invention is the refletcion high-energy electron diffraction instrument.
Above-mentioned ML is the abbreviation of English words monolayer, i.e. molecular layer.For BeTe or ZnSe, 1ML is about 0.28nm.
The present invention organizes compound semiconductor (ZnSe and BeTe) with II-VI and prepares II type quantum well structure by molecular beam epitaxy (MBE) growth method, used II-VI compound semiconductor ZnSe and BeTe have very wide forbidden band (being about 2.8eV and 4.2eV respectively) and stronger ionic associative key, be a kind of defect concentration few (and being difficult for diffusion), the crystal that texture quality is high.Compared with other traditional heterojunction structure by the ZnSe/BeTe/ZnSe quantum well structure that they are formed, have following characteristics: (1) II type (type-II) can be with structure, and there is a big energy drop (Δ E on conduction band (or valence band) limit
CB:～2.3eV, Δ E
VB:～0.8eV) (seeing accompanying drawing 1); (2) its lattice mismatch at the interface is less than 0.5%; (3) occur in that the space indirect transition (spatially indirect transition is abbreviated as IT, i.e. the transition of II type) at heterojunction boundary place is luminous an optical anisotropy (in-plane optical anisotropy) in the very strong face; (4) very strong covalent bond structure has stronger bound energy.Spatial isolation takes place in electronics and hole that this constructional feature can cause being excited to produce, and is in respectively in the different trap layers.Because so dark potential well makes the wave function in electronics and hole that a very little overlapping scope be arranged, about 1～2ML is so this structure has the indirect recombination luminescence life-span of very long space.Therefore, ZnSe/BeTe/ZnSe II type quantum well structure is considered to observe and study the important materials and the structure of high-density phenomenon and making opto-electronic device.
The used growing system of the present invention has two growth rooms, is specifically designed to the epitaxy of III-V family and the epitaxy of II-VI family respectively.During with molecular beam epitaxial method growing ZnSe/BeTe heterojunction structure,, can obtain very precipitous interface by regulating the formation of heterojunction boundary place chemical bond.
The principle of work of the inventive method is as follows:
Choose II-VI compound semiconductor ZnSe and BeTe with broad stopband, utilizing them to locate at conduction band limit (or valence-band edge) can be with discontinuous and characteristics than the macro-energy drop are arranged, particularly utilize at the bottom of the conduction band of ZnSe not only low at the bottom of the conduction band than BeTe, simultaneously also low characteristics at the bottom of the valence band than BeTe at the bottom of the valence band of ZnSe form the ZnSe/BeTe quantum well (as shown in Figure 1) with II type energy band structure characteristics.Such constructional feature makes the electronics and the hole of being excited to produce in the ZnSe layer that spatial isolation can take place, and promptly electronics is still stayed in the original ZnSe layer, and the hole is transferred in the adjacent BeTe layer.Because they are in respectively in the different potential well layers, and very dark potential well has limited them each other to the infiltration of adjacent layers, make them have only very little wave function overlapping at the interface, therefore their the indirect recombination luminescence in space (being that the II type is luminous) life-span is very long, can reach microsecond level (~ μ s), be the ideal structure of observing, study the condensed state phenomenon.
A kind of equipment that is used for above-mentioned preparation method, promptly two growth rooms molecular beam epitaxy system, comprise two growth rooms of III-V family and II-VI family, it is characterized in that each growth room all has solid source vaporizer, five dimension adjustable specimen holder, quadrupole mass spectrometer and reflection high energy electron diffractions etc.; Wherein two solid source vaporizers in the III-V family growth room are Ga vaporizer and As vaporizer (seeing accompanying drawing 2), and five solid source vaporizers in the II-VI family growth room are Te, Zn, Se, Mg and Be source vaporizer; Connect so that the transmission of sample with ultra-high vacuum transmission pipeline between two growth rooms; Ultra-high vacuum transmission pipeline has air extractor, and two growth rooms that are connected with two ends separate with push-pull valve respectively; Specimen holder and solid source vaporizer all are connected to heater strip respectively, to satisfy thermoregulated requirement; All be furnished with the cooled with liquid nitrogen device near growth room's inwall and solid source vaporizer and the substrate, so that absorption indoor showy atom in growth room and molecule, thereby reduce the indoor air pressure in growth room and guarantee sample degree of cleaning on every side.
The ZnSe/BeTe quantum well structure that the inventive method is grown has crystal mass height, the characteristics of good, the II type energy band structure of lattice match at the interface.ZnSe and BeTe very big can be with drop having at the interface, can make electronics and hole be easy to take place spatial isolation.Darker potential well makes them that thereby the overlapping luminescent lifetime that has than length of less wave function be arranged each other, helps observing, research condensed state phenomenon (as charged exciton, excitonic molecule, exciton polymkeric substance and Bose-Einstein condensation etc.).In addition, during growing crystal by the suitably opening and closing of control material supply source molecular beam, can be at n-Te of the formation corresponding Z at the interface between potential well layer and the barrier layer or Te-Zn chemical bond, thus make this structure have very precipitous interface.Such structure also has very strong anisotropy, makes us can judge, distinguish the luminous composition from different interfaces in view of the above.
This structure not only is suitable for the physical study to phenomenons such as condensed states, aspect the photoelectric devices such as optical communication, quantum information storage and processing, photodiode, semiconductor laser important use is being arranged also.
Description of drawings
Fig. 1 is the crystalline structure of zinc selenide/zinc selenide of the present invention (ZnSe/BeTe/ZnSe) sample and can be with synoptic diagram.
Figure below wherein is the sectional view that comprises the entire sample structure of active layer ZnSe/BeTe/ZnSe, and last figure is the energy band structure corresponding to active layer and buffer layer.C.B and V.B represent conduction band and valence band respectively, and DT represents the direct transition in the space in the ZnSe layer (being the transition of I type), and IT represents the space indirect transition (being the transition of II type) between ZnSe layer and the BeTe layer.
Wherein: 1, GaAs substrate, 2, the GaAs buffer layer, 3, the BeTe buffer layer, 4, Zn
0.77Mg
0.15Be
0.08The Se sealing coat, 5, the ZnSe potential well layer, 6, the BeTe barrier layer, 7, the ZnSe potential well layer, 8, Zn
0.77Mg
0.15Be
0.08The Se sealing coat, 9, the Zn tectum.
Also have: E
S=3.0eV (Zn
0.77Mg
0.15Be
0.08The energy gap of Se), E
B=4.2eV (energy gap of BeTe), E
W=2.8eV (energy gap of ZnSe), Δ E
C=2.3eV (conduction band of BeTe and ZnSe is poor), Δ E
V=0.8eV (valence band of BeTe and ZnSe is poor), Δ E
C1=0.2eV (Zn
0.77Mg
0.15Be
0.08The conduction band of Se and ZnSe is poor), Δ E
V1=0.1eV (ZnSe and Zn
0.77Mg
0.15Be
0.08The valence band of Se is poor).
Fig. 2 is the internal structure synoptic diagram of the III-V family growth room in the used MBE device of the present invention.
Wherein: 10, the electron beam gun of RHEED instrument, 11, the window of tube of RHEED instrument, 12, quadrupole mass spectrometer, 13, specimen holder, 14, III-V family growth room, 15, the solid source baffle plate, 16, molecular beam, 17, heater strip, 18, Ga solid source, 19, the As solid source, 20, standby solid source (using).
Embodiment
Below in conjunction with accompanying drawing 1 and accompanying drawing 2 and embodiment making processes involved in the present invention is described further, but is not limited thereto.
Embodiment 1:(method embodiment)
A kind ofly prepare the method for II type quantum well with molecular beam epitaxial process, as shown in Figure 1, step is as follows:
1, the gallium arsenide substrate with (001) orientation is fixed in the holder of molybdenum (Mo) sample with indium (In);
2, confirm III-V family growth room's vacuum tightness be below 1 * 10-10Torr after, by the magnetic force driven rod sample is sent in the III-V family growth room; With the sample holder, the K-cell container of As solid source is housed and the K-cell container heat temperature raising of Ga solid source is housed, the temperature that makes it to reach setting is respectively 300 ℃, 100 ℃ and 750 ℃;
3, the temperature of independent control As source K-cell container, after making it to begin to warm to 295 ℃ by 100 ℃, temperature with sample holder and Ga source K-cell container is set at 550 ℃ and 915 ℃ respectively again, and begin to heat up, open the baffle plate of As source K-cell container simultaneously, the As molecular beam is radiated on the substrate, the evaporation of the substrate surface As cause because of underlayer temperature raises with compensation, and make the evaporation of As on the substrate surface reach balance with adhering to;
4, treat that Ga source K-cell container rises to 915 ℃ after, again the sample holder is warming up to 620 ℃, can on [110] direction, observe by reflected high energy electron diffraction (RHEED instrument) instrument between temperature raising period, striped occurs if can observe clearly, the oxide compound of having removed substrate surface under this temperature then is described and obtains the orderly substrate surface of cleaning;
5, the generation of GaAs buffer layer 2: open the baffle plate that temperature has risen to 915 ℃ Ga source K-cell container, the Ga molecular beam is radiated on the substrate; This moment, the molecular beam of Ga and As was radiated at substrate surface simultaneously, the growth of GaAs buffer layer begins, growth time is about 30 minutes, growth thickness is about the GaAs buffer layer of 250nm, turn off the Ga source this moment, and the temperature of Ga source K-cell container reduced to 750 ℃ by 915 ℃, reduce to 300 ℃ afterwards again, and a cleaning, smooth and orderly surface are arranged by the substrate that the RHEED instrument can be observed this moment;
6, stablize 5 minutes after, underlayer temperature is reduced to 580 ℃ gradually by 620 ℃, cool-down method is a staged, promptly each cooling is set at falls 5 ℃, sets next time when reaching design temperature again, divides and finishes cooling 8 times; After the cooling beginning, when observing image and do not have what ANOMALOUS VARIATIONS, the As source is turned off, and the As source temperature is transferred to 100 ℃ by 295 ℃ by the RHEED instrument;
7, underlayer temperature is reduced to 500 ℃ gradually by 580 ℃, cool-down method is a staged, falls 10 ℃ at every turn; Afterwards, again underlayer temperature is reduced to 300 ℃ gradually by 500 ℃, whole temperature-fall period divides and carries out for 10 times, and each cooling is spaced apart 20 ℃;
8, observe RHEED instrument image and do not have what ANOMALOUS VARIATIONS, can turn off the RHEED instrument this moment, after the vacuum tightness of determining III-V family growth room becomes below 7.5 * 10-9Torr, turn off being used for the power supply of heated substrate, and prepare substrate is passed to II-VI family growth room by the high vacuum transmission pipeline;
9, be below 1 * 10-10Torr and the temperature in the Zn in the II-VI family growth room, Be, Te, Se and Mg source is heated to respectively after 150,820,150,50 and 200 ℃ in the vacuum tightness of determining II-VI family growth room, again substrate be sent to II-VI family growth room by III-V family growth room by ultra-high vacuum transmission pipeline; Substrate is warming up to 320 ℃, and the temperature in Zn, Be, Te, Se and Mg source is warming up to 307,1065,320,202 and 322.5 ℃ more respectively;
10, the generation of BeTe buffer layer 3: after the temperature in Be, Te source reaches 1065 and 320 ℃ respectively, stablized 30 minutes, open the baffle plate in Be, Te source, Be molecular beam and Te molecular beam are radiated at the surface of substrate, and the BeTe buffer layer begins to grow this moment; Monitor in real time with the RHEED instrument, when the growth thickness of BeTe buffer layer was about 5ML, growth ending was turned off the Be source then earlier, turns off the Te source subsequently again;
11, the growth of Zn0.77Mg0.15Be0.08Se sealing coat 4: the baffle plate of opening the Zn source earlier, open the baffle plate in Se, Be and Mg source again, the growth of Zn0.77Mg0.15Be0.08Se sealing coat is carried out on the surface that have Zn molecular beam, Se molecular beam, Be molecular beam and Mg molecular beam to be radiated at substrate simultaneously this moment respectively, when the sealing coat growth thickness is about 200nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 5 seconds;
12, the growth of ZnSe potential well layer 5: open Zn, Se source, make the two be radiated on the substrate surface simultaneously, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is about 28ML, growth ending, close the Se source earlier, after about 5 seconds, close the Zn source again, so that form rich Zn upper layer;
13, the temperature in the growth of BeTe barrier layer 6: Be, Te source remains on 1065 and 320 ℃ respectively, open the Te source, through opening the Be source BeTe barrier layer that begins to grow after 5 seconds again, when the thickness of BeTe layer growth is about 10ML, growth ending is closed the Be source earlier, closes the Te source again after about 5 seconds, so that form rich Te upper layer, can reduce to 150 ℃ this moment with the temperature in Te source; Above-mentioned process of growth can be between ZnSe and BeTe the chemical bond that obtains the Zn-Te form at the interface;
14, the growth of ZnSe potential well layer 7: open the Zn source, open Se source growing ZnSe potential well layer again after 5, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is about 28ML, growth ending is successively closed Se source and Zn source; Above-mentioned process of growth can be between BeTe and ZnSe the chemical bond that obtains the Te-Zn form at the interface;
15, the process of growth of the sealing coat of repeating step 11 can obtain the Zn0.77Mg0.15Be0.08Se sealing coat 8 that the thick energy gap of 200nm is 3.0eV; To close Se, Be, Mg source earlier during growth ending, close the Zn source again after about 10 seconds, can not corroded with the protection sample at grown on top one deck Zn of sample as tectum 9 like this; Behind the growth ending, underlayer temperature is made as 150 ℃ and make it cooling, also the temperature in Zn, Se, Be and Mg source is set at simultaneously 100,50,820 and 150 ℃ and make it cooling respectively; Reduce to after 150 ℃ and the temperature of confirming the Se source reduce to below 100 ℃ when underlayer temperature, sample is taken out from the growth room, can obtain the quantum-well materials of complete ZnSe/BeTe/ZnSe form.
Embodiment 2:(method embodiment)
The embodiment of the invention 2 is identical with embodiment 1, just:
The growth time of the GaAs buffer layer in the step 5 is 38 minutes, and growth thickness is about 320nm;
Substrate in the step 9 is warming up to 330 ℃;
When the sealing coat growth thickness in the step 11 is 300nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 6 seconds;
When the thickness of the ZnSe layer growth in the step 12 was about 40ML, growth ending was closed the Se source earlier, closes the Zn source again after about 6 seconds, so that form rich Zn upper layer;
Growth ending in the step 13 is closed the Be source earlier, closes the Te source again after about 6 seconds;
When the thickness of the ZnSe layer growth in the step 14 is about 20ML, growth ending;
Separation layer thickness in the step 15 is 300nm.
Embodiment 3:(method embodiment)
The embodiment of the invention 3 is identical with embodiment 1, just:
The growth time of the GaAs buffer layer in the step 5 is 43 minutes, and growth thickness is about 360nm;
Substrate in the step 9 is warming up to 340 ℃;
When the sealing coat growth thickness in the step 11 is 330nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 7 seconds;
When the thickness of the ZnSe layer growth in the step 12 was about 28ML, growth ending was closed the Se source earlier, closes the Zn source again after about 7 seconds, so that form rich Zn upper layer;
Growth ending in the step 13 is closed the Be source earlier, closes the Te source again after about 7 seconds;
When the thickness of the ZnSe layer growth in the step 14 is about 14ML, growth ending;
Separation layer thickness in the step 15 is 330nm.
Embodiment 4:(method embodiment)
The embodiment of the invention 4 is identical with embodiment 1, just:
The growth time of the GaAs buffer layer in the step 5 is 50 minutes, and growth thickness is about 420nm;
Substrate in the step 9 is warming up to 310 ℃;
When the sealing coat growth thickness in the step 11 is 350nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 9 seconds;
When the thickness of the ZnSe layer growth in the step 12 was about 45ML, growth ending was closed the Se source earlier, closes the Zn source again after about 9 seconds, so that form rich Zn upper layer;
Growth ending in the step 13 is closed the Be source earlier, closes the Te source again after about 9 seconds;
When the thickness of the ZnSe layer growth in the step 14 is about 45ML, growth ending;
Separation layer thickness in the step 15 is 350nm.
Embodiment 5:(apparatus embodiments)
A kind of equipment that is used for above-mentioned preparation method, the equipment of use are two growth rooms molecular beam epitaxy systems, comprise two growth rooms of III-V family and II-VI family.Each all has solid source vaporizer, five dimension adjustable specimen holder, quadrupole mass spectrometer and reflection high energy electron diffractions etc.; Two Ga and As solid source 18,19 vaporizers (seeing accompanying drawing 2) are wherein arranged in the III-V family growth room, and five solid source vaporizers in the II-VI family growth room are Te, Zn, Se, Mg and Be source vaporizer.Connect so that the transmission of sample with ultra-high vacuum transmission pipeline between two growth rooms; Ultra-high vacuum transmission pipeline has air extractor, and two growth rooms that are connected with two ends separate with push-pull valve respectively; Specimen holder and solid source vaporizer all are connected to heater strip respectively, to satisfy thermoregulated requirement; Growth room's inwall, and all be furnished with the cooled with liquid nitrogen device near solid source vaporizer and the substrate, so that absorption indoor showy atom in growth room and molecule, thereby reduce the indoor air pressure in growth room and guarantee sample degree of cleaning on every side.
Claims (2)
1, a kind ofly prepare the method for II type quantum well with molecular beam epitaxial process, step is as follows:
1) gallium arsenide substrate with (001) orientation is fixed in the holder of molybdenum sample with indium;
2) logical cooled with liquid nitrogen growth room, confirm III-V family growth room's vacuum tightness be below 1 * 10-10Torr after, by the magnetic force driven rod sample is sent in the III-V family growth room; With the sample holder, the K-cell container of As solid source is housed and the K-cell container heat temperature raising of Ga solid source is housed, the temperature that makes it to reach setting is respectively 300 ℃, 100 ℃ and 750 ℃;
3) temperature of adjustment As source K-cell container, after making it to begin to warm to 295 ℃ by 100 ℃, temperature with sample holder and Ga source K-cell container is set at 550 ℃ and 915 ℃ respectively again, and begin to heat up, open the baffle plate of As source K-cell container simultaneously, the As molecular beam is radiated on the substrate, the evaporation of the substrate surface As cause because of underlayer temperature raises with compensation, and make the evaporation of As on the substrate surface reach balance with adhering to;
4) treat that Ga source K-cell container rises to 915 ℃ after, again the sample holder is warming up to 620 ℃, can exist by reflection high energy electron diffraction between temperature raising period
Observe on the direction, striped occurs if can observe clearly, the oxide compound of having removed substrate surface under this temperature then is described and obtains the orderly substrate surface of cleaning;
5) generation of GaAs buffer layer: open the baffle plate that temperature has risen to 915 ℃ Ga source K-cell container, the Ga molecular beam is radiated on the substrate; This moment, the molecular beam of Ga and As was radiated at substrate surface simultaneously, the growth of GaAs buffer layer begins, growth time is 24 ~ 120 minutes, the thickness of GaAs buffer layer can reach 200 ~ 1000nm, turn off the Ga source this moment, and the temperature of Ga source K-cell container reduced to 750 ℃ by 915 ℃, reduce to 300 ℃ afterwards again, and a cleaning, smooth and orderly surface are arranged by the substrate that the RHEED instrument can be observed this moment;
6) stablize 5 minutes after, underlayer temperature is reduced to 580 ℃ gradually by 620 ℃, cool-down method is a staged, promptly each cooling is set at falls 5 ℃, sets next time when reaching design temperature again, divides and finishes cooling 8 times; After the cooling beginning, when observing image and do not have what ANOMALOUS VARIATIONS, the As source is turned off, and the As source temperature is transferred to 100 ℃ by 295 ℃ by the RHEED instrument;
7) underlayer temperature is reduced to 500 ℃ gradually by 580 ℃, cool-down method is a staged, falls 10 ℃ at every turn; Afterwards, again underlayer temperature is reduced to 300 ℃ gradually by 500 ℃, whole temperature-fall period divides and carries out for 10 times, and each cooling is spaced apart 20 ℃;
8) observe RHEED instrument image and do not have what ANOMALOUS VARIATIONS, can turn off the RHEED instrument this moment, after the vacuum tightness of determining III-V family growth room becomes 7.5 * 10-9Torr below, turn off being used for the power supply of heated substrate, and prepare substrate by high vacuum transmission pipeline biography to II-VI family growth room;
9) be below 1 * 10-10Torr and the temperature in the Zn in the II-VI family growth room, Be, Te, Se and Mg source is heated to respectively after 150,820,150,50 and 200 ℃ in the vacuum tightness of determining II-VI family growth room, again substrate be sent to II-VI family growth room by III-V family growth room by ultra-high vacuum transmission pipeline; Substrate is warming up to 300 ℃ ~ 350 ℃, and the temperature in Zn, Be, Te, Se and Mg source is warming up to 307,1065,320,202 and 322.5 ℃ more respectively;
10) generation of BeTe buffer layer: after the temperature in Be, Te source reaches 1065 and 320 ℃ respectively, stablized 30 minutes, open the baffle plate in Be, Te source, Be molecular beam and Te molecular beam are radiated at the surface of substrate, and the BeTe buffer layer begins to grow this moment; Monitor in real time or set, control with computer with the RHEED instrument, when the growth thickness of BeTe buffer layer was about 5ML, growth ending was turned off the Be source then earlier, wait about 5 seconds after, turn off the Te source subsequently again, make surperficial rich Te;
11) growth of Zn0.77Mg0.15Be0.08Se sealing coat: the baffle plate of opening the Zn source earlier, the baffle plate of opening Se, Be and Mg source again carries out the growth of Zn0.77Mg0.15Be0.08Se sealing coat, have Zn molecular beam, Se molecular beam, Be molecular beam and Mg molecular beam to be radiated at the surface of substrate simultaneously this moment respectively, when the sealing coat growth thickness is 200 ~ 1000nm, finish growth, close Se, Be, Mg source earlier, close the Zn source again after about 5 ~ 10 seconds;
12) growth of ZnSe potential well layer: open Zn, Se source, make the two be radiated on the substrate surface simultaneously, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is 4 ~ 80ML, growth ending, close the Se source earlier, after about 5 ~ 10 seconds, close the Zn source again, so that form rich Zn upper layer;
13) temperature in the growth of BeTe barrier layer: Be, Te source remains on 1065 and 320 ℃ respectively, open the Te source, through opening the Be source BeTe barrier layer that begins to grow after 5 ~ 10 seconds again, when the thickness of BeTe layer growth is about 10ML, growth ending is closed the Be source earlier, closes the Te source again after about 5 ~ 10 seconds, so that form rich Te upper layer, can reduce to 150 ℃ this moment with the temperature in Te source; Above-mentioned process of growth can be between ZnSe and BeTe the chemical bond that obtains the Zn-Te form at the interface;
14) growth of ZnSe potential well layer: open the Zn source, opened Se source growing ZnSe potential well layer again after 5 ~ 10 seconds, the temperature of Zn, Se solid source remains on 307 and 202 ℃ respectively, when the thickness of ZnSe layer growth is 4 ~ 80ML, growth ending is successively closed Se source and Zn source; Above-mentioned process of growth can be between BeTe and ZnSe the chemical bond that obtains the Te-Zn form at the interface;
15) repeating step 11) the process of growth of sealing coat can obtain the thick Zn0.77Mg0.15Be0.08Se sealing coat of 200 ~ 1000nm; To close Se, Be, Mg source earlier during growth ending, close the Zn source again after about 10 seconds, can not corroded with the protection sample at grown on top one deck Zn of sample as tectum like this; Behind the growth ending, underlayer temperature is made as 150 ℃ and make it cooling, also the temperature in Zn, Se, Be and Mg source is set at simultaneously 100,50,820 and 150 ℃ and make it cooling respectively; Reduce to after 150 ℃ and the temperature of confirming the Se source reduce to below 100 ℃ when underlayer temperature, sample is taken out from the growth room, can obtain the quantum-well materials of complete ZnSe/BeTe/ZnSe form.
2, the equipment that uses in a kind of method according to claim 1, promptly two growth rooms molecular beam epitaxy system, comprise two growth rooms of III-V family and II-VI family, it is characterized in that each growth room all has solid source vaporizer, five dimension adjustable specimen holder, quadrupole mass spectrometer and reflection high energy electron diffractions etc.; Wherein two solid source vaporizers in the III-V family growth room are Ga vaporizer and As vaporizer, and five solid source vaporizers in the II-VI family growth room are Te, Zn, Se, Mg and Be source vaporizer; Connect so that the transmission of sample with ultra-high vacuum transmission pipeline between two growth rooms; Ultra-high vacuum transmission pipeline has air extractor, and two growth rooms that are connected with two ends separate with push-pull valve respectively; Specimen holder and solid source vaporizer all are connected to heater strip respectively, to satisfy thermoregulated requirement; All be furnished with the cooled with liquid nitrogen device near growth room's inwall and solid source vaporizer and the substrate, so that absorption indoor showy atom in growth room and molecule, thereby reduce the indoor air pressure in growth room and guarantee sample degree of cleaning on every side.
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| CN101712456B (en) * | 2009-11-13 | 2012-09-05 | 山东大学 | Method for eliminating intrinsic electric field in ZnSe/BeTe II quantum well |
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| CN101712456B (en) * | 2009-11-13 | 2012-09-05 | 山东大学 | Method for eliminating intrinsic electric field in ZnSe/BeTe II quantum well |
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| CN104711670A (en) * | 2015-04-02 | 2015-06-17 | 中国科学院上海微系统与信息技术研究所 | Sample support for molecular beam epitaxial growth and angle resolved photoelectron spectroscope testing |
| CN106637416A (en) * | 2016-12-28 | 2017-05-10 | 厦门大学 | Molecular beam epitaxy and in-situ characterization device under vector strong magnetic field |
| CN106637416B (en) * | 2016-12-28 | 2018-11-20 | 厦门大学 | Molecular beam epitaxy and its in-situ characterization device under vector high-intensity magnetic field |
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| CN111349911A (en) * | 2018-12-21 | 2020-06-30 | 广东众元半导体科技有限公司 | Molecular beam epitaxial film growth device with laser direct writing function and method |
| CN113710833A (en) * | 2019-04-22 | 2021-11-26 | 杜鹏 | Molecular beam epitaxy system for directly evaporating pump to cold plate |
| CN113710833B (en) * | 2019-04-22 | 2023-04-28 | 杜鹏 | Molecular beam epitaxy system with direct evaporation pump to cold plate |
| CN114284394A (en) * | 2022-03-04 | 2022-04-05 | 武汉高芯科技有限公司 | Growth method of superlattice detector material and superlattice infrared detector |
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