CN101100763A - Growth device for preparing IV-VI species semiconductor single-crystal thin film - Google Patents
Growth device for preparing IV-VI species semiconductor single-crystal thin film Download PDFInfo
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- CN101100763A CN101100763A CNA2007100688632A CN200710068863A CN101100763A CN 101100763 A CN101100763 A CN 101100763A CN A2007100688632 A CNA2007100688632 A CN A2007100688632A CN 200710068863 A CN200710068863 A CN 200710068863A CN 101100763 A CN101100763 A CN 101100763A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 32
- 239000013078 crystal Substances 0.000 title claims abstract description 26
- 239000010409 thin film Substances 0.000 title claims description 16
- 239000000758 substrate Substances 0.000 claims abstract description 53
- 238000001816 cooling Methods 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims description 88
- 238000000034 method Methods 0.000 claims description 31
- 238000007872 degassing Methods 0.000 claims description 21
- 239000010408 film Substances 0.000 claims description 19
- 108010083687 Ion Pumps Proteins 0.000 claims description 10
- 238000000859 sublimation Methods 0.000 claims description 10
- 230000008022 sublimation Effects 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 9
- 238000002955 isolation Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- AEEAZFQPYUMBPY-UHFFFAOYSA-N [I].[W] Chemical compound [I].[W] AEEAZFQPYUMBPY-UHFFFAOYSA-N 0.000 claims description 6
- 230000008676 import Effects 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000000872 buffer Substances 0.000 abstract description 2
- 229910002665 PbTe Inorganic materials 0.000 description 8
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 8
- 229910016036 BaF 2 Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000002207 thermal evaporation Methods 0.000 description 4
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003955 hot wall epitaxy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910005642 SnTe Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000097 high energy electron diffraction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004943 liquid phase epitaxy Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910002059 quaternary alloy Inorganic materials 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008400 supply water Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A IV-VI groups of semiconductor crystal film growth apparatus includes growth unit, vacuum unit, heating unit, cooling unit, and control unit. The growth unit consists of a feeding chamber, a pre-growing chamber and a growing chamber connected sequentially. Gate valves are used to separate the said chambers each other. Cushion substrates are transferred between the adjacent chambers by transferring bars. Liftable and rotary tables are respectively set in the pre-growing chamber and growing chamber. 2-8 beam source furnaces are installed under the tables in the growing chamber with buffers separating the tables from the furnaces. Water cooling or liquid nitrogen cooling can bused in the growing chamber. It can produce quality product of 3 inch diameter with low cost.
Description
Technical field
The invention belongs to the technical field of semiconductor material growth apparatus, be specifically related to a kind of under ultra-high vacuum environment on different substrate materials the growing apparatus of growing high-quality IV-VI family narrow gap semiconductor monocrystal thin films and heterojunction structure thereof.
Background technology
IV-VI family semiconductor material comprises the PbSe of two component system, PbTe, SnSe, the PbSrSe of SnTe and three component system, PbSrTe, PbSnSe, PbSnTe, PbEuSe, the preparation equipment and technology of PbMnTe and their heterojunction structure thereof etc. are the keys that obtains high-quality material, say traditionally, they have several growth methods and device, as thermal evaporation techniques, and liquid phase epitaxial technique, hot wall epitaxy technology etc., Shanghai Institute of Technical Physics uses optical thin film plated film machine, include growth apparatus, pumped vacuum systems, heating system, cooling system, Controlling System and computer control system.With thermal evaporation method 2.6 * 10
-3On silicon substrate, grown under the environment of Pa the PbTe film [document 1: Li Bin etc., infrared and millimeter wave journal, 2005, Vol.24, No.1, p.23-26].Only with a vacuum chamber deposition, sample of every growth need be exposed to vacuum chamber in the air growth apparatus, and vacuum tightness is low.The method of traditional thermal evaporation can't the grown quantum trap and problem such as superlattice, makes the application of IV-VI family semiconductor crystal film be very restricted.The hot wall epitaxy technology then is the improvement of thermal evaporation method, though crystal mass can have bigger improvement, sample size is little.Liquid phase epitaxy method then is a heat balance growing method, though can grow small size (1 * 1cm
-2) monocrystal thin films, but can not growing large-size (for example 2 inches, 3 inches), and can not the grown quantum trap, low dimensional structures such as superlattice.IV-VI family semiconductor single crystal thin film and heterojunction structure [document 2:H.Z.Wu etc. thereof though traditional molecule epitaxial growth method can be grown, J.Vac.Sci.Technol.B, 1999,17 (3), p.1263-1266], but all adopt low temperature environment, need special equipment to keep low temperature, make the cost of manufacturing very expensive in cooled with liquid nitrogen.
The growing apparatus of existing semiconductor single crystal thin film often has only a vacuum chamber deposition, an electron gun stove, can't obtain high-quality IV-VI family semiconductor single crystal thin film, can only obtain polycrystalline or noncrystal membrane, surface irregularity, and, can only be used for infrared fileter owing to slight crack occurs on the surface easily in the nucleating growth process, can not be applied to the development of high-end product, for example middle infrared laser and detector etc.
Summary of the invention
The present invention seeks at existing IV-VI family's semiconductor crystal film device or be not suitable for preparing shortcomings such as large size, cost height, a kind of IV-VI family semiconductor crystal film growing apparatus that is is provided.
Preparation IV-VI of the present invention family semiconductor crystal film growing apparatus, include growth apparatus, pumped vacuum systems, heating system, cooling system, power control system and computer control system, it is characterized in that: described growth apparatus is by Sample Room, the growth preparation room, three vacuum chambers in growth room connect and compose successively, reach between growth preparation room and the growth room between Sample Room and the growth preparation room and isolate by slide valve, Sample Room has the sample driven rod to transmit substrate with the growth preparation room, and growth preparation room and growth room have the sample driven rod to transmit substrate, and there is the specimen holder of liftable and rotation growth preparation room and growth room, there be 2-8 electron gun stove in growth room specimen holder bottom, isolates specimen holder and electron gun stove by baffle plate.
The Sample Room of growth apparatus of the present invention includes: the pumped vacuum systems of being made up of mechanical pump and composite molecular pump; Place the specimen holder of substrate, substrate is by in the specimen holder holder of packing in the clean by laminar flow worktable; The measurement of vacuum ion gauge; The tungsten-iodine lamp that the substrate bake out is used; Sample Room links to each other between the preparation room with growth, is isolated by the vacuum lock plate valve; Sample Room sample driven rod, the degasification back substrate is imported the growth preparation room into by Sample Room sample transmission pole.
The growth preparation room of growth apparatus of the present invention includes: the specimen holder of liftable and rotation, a plurality of sample holders are arranged on the specimen holder, and can store, handle a plurality of samples; Graphite heater furnace; Sputter ion pump; Have a viewing window; The growth preparation room links to each other with the growth room, is isolated by the vacuum lock plate valve; Growth preparation room sample driven rod, substrate imports the growth room by growth preparation room sample driven rod into by the growth preparation room.
The growth room of growth apparatus of the present invention includes: the pumped vacuum systems of being made of the growth room sputter ion pump and titanium sublimation pump; The ion gauge of measurement of vacuum; Have growth room's viewing window; Have the specimen holder of liftable and rotation to be connected with stepper-motor, stepper-motor is connected with computer, the speed of rotation of control specimen holder; Substrate tantalum piece well heater; There are many electron gun stoves in growth room specimen holder bottom; The line of measurement size line rule are arranged; The adopting process cooling-water machine constitutes cooling system around the electron gun stove.
There is a shutter at each electron gun fire door place of the present invention, with at the bottom of the baffle plate isolation liner with the electron gun stove, the electron gun stove be 2-8 only, accuracy of temperature control is ± 0.5 ℃, room temperature to 1200 is ℃ continuous adjustable controlled, the cooling recirculated water cooling of electron gun stove.
Stepper-motor of the present invention, the controllable speed of rotation when sample grown are 0～30 rev/min of stepless speed regulation.
Heating system of the present invention, Sample Room process furnace are tungsten-iodine lamp, and be ℃ controllable in room temperature～200; Pretreatment chamber's process furnace is a graphite heating, and is ℃ controllable in room temperature～350; Growth room's process furnace is tantalum piece heating, and ℃ controllable in room temperature～800, temperature fluctuation is in ± 1 ℃.
Cooling system of the present invention, the cooling system of electron gun stove and growth room are to provide recirculated cooling water by the technology cooling-water machine, and wherein 5 ℃～20C of supply water temperature is adjustable controlled, and the growth room also can use cooled with liquid nitrogen.
The in situ detection device can also be installed by growth room of the present invention, and for example the refletcion high-energy electron diffraction instrument situation, the quadrupole mass spectrometer that are used to observe growth surface is used to detect the gas ingredients in the growth room.
Controlling System of the present invention: by power supply, temperature control power supply, stepper-motor rotation control power supply, the digital display vacuumometer, series rotary sheet type mechanical pump, compound molecule pumping source, the plasma sputter pumping source, the sublimation pump power supply is formed, by the computer system accuracy controlling.
The working process for preparing IV-VI family semiconductor crystal film growing apparatus of the present invention is:
To pack on the Sample Room specimen holder, and vacuumize with mechanical pump, composite molecular pump, heating makes the substrate degasification;
On the specimen holder with substrate liftable and rotation in import the growth preparation room into the magnetic force transmission pole after the degasification, close the slide valve between Sample Room and the growth preparation room, take out ultrahigh vacuum(HHV) in the preparation room of growing, the substrate bake out;
With the different high-purity variant electron gun stove of source material intensification degasification are housed, measure molecular beam with ion gauge, in degasification and process of growth, all electron gun stove and growth room's outer wall are cooled off with recirculated water always;
The substrate of growth in the preparation room at room temperature imported on the specimen holder of liftable and rotation in the growth room with the magnetic force transmission pole, isolate growth room and growth preparation room with slide valve, and take out growth room's vacuum to the ultrahigh vacuum(HHV) degree with ionic pump and sublimation pump, with tantalum piece substrate is heated, use at the bottom of the baffle plate isolation liner and the electron gun stove;
Underlayer temperature is adjusted to growth temperature, keeps the underlayer temperature fluctuation in ± 1 ℃, open stepper-motor, the control rotating speed is opened 2-8 electron gun fender plate as required simultaneously, opens the specimen holder baffle plate, begins growth;
When the monocrystal thin films growth is finished, close the electron gun stove, finish growth, and underlayer temperature reduced to room temperature, spread out of the growth room to the preparation room of growing by the sample that it is good that the magnetic force transfer system will be grown, have the growth preparation room to pass to Sample Room again, Sample Room is filled high pure nitrogen to 1 normal atmosphere, open the dress sample door of Sample Room, take out sample.
The monocrystal thin films growth comprises the electron gun furnace temperature by computer control, fast door opened/closed state, and the stepper-motor rotating speed control of sample rotation, the control of underlayer temperature etc. all has computer software control.
The present invention's advantage compared with prior art is: be the preparation and the middle infrared laser of IV-VI family semiconductor crystal film, the growth of optoelectronic device structure such as middle infrared eye provides the growth apparatus of ultrahigh vacuum(HHV), in conjunction with mechanical pump, molecular pump, ionic pump, working successively of sublimation pump equipment, make Sample Room, these three vacuum chambers that link to each other of growth preparation room and growth room reach high vacuum and ultra-high vacuum state, isolate mutually with the vacuum lock plate valve between the level before and after three vacuum chambers and assurance wherein the variation of the vacuum tightness of any one vacuum chamber can not impact other two Room, thereby reached for preparing the required ultrahigh vacuum(HHV) degree of epitaxial material sound assurance is provided, the handing-over of sample between Sample Room and growth preparation room, handing-over between growth preparation room and the growth room is finished by the magnetic force driven rod, and the handing-over of sample and operation are all finished in ultrahigh vacuum(HHV) like this.Make the growth of IV-VI family sample in ultrahigh vacuum(HHV), to finish.The growth room of this equipment is under the condition that does not adopt cooled with liquid nitrogen, but the cooling of equipment is carried out in the circulation of employing water coolant, and this greatly reduces the cost of equipment operation; Loading amount of the present invention has many electron gun stoves, opens 2 electron gun fender plates two component system IV-VI semi-conductors such as PbSe, PbTe of can growing simultaneously; Open 3 electron gun fender plates three component system IV-VI semi-conductors such as PbSrSe, PbMnTe of can growing simultaneously; Open 4 electron gun fender plates PbMnSeTe that can grow simultaneously, PbSrTeSe quaternary system IV-VI semi-conductor is respectively at BaF
2(111) cover CaF on monocrystalline, Si (111) monocrystalline
2, BaF
2Buffer layer has successfully made high-quality IV-VI family narrow gap semiconductor monocrystal thin films on CdTe monocrystalline and the MgO single crystalline substrate, the sample size size is 2 inches or 3 inches, and good uniformity.
Description of drawings:
Accompanying drawing 1: the structural representation that is Sample Room in apparatus of the present invention.
Accompanying drawing 2: the structural representation that is growth preparation room in apparatus of the present invention.
Accompanying drawing 3: the structural representation that is growth room in apparatus of the present invention.
1-Sample Room among the figure, 2-Sample Room specimen holder, slide valve between 3-Sample Room and the growth preparation room, connecting passage between 4-Sample Room and the growth preparation room, 5-Sample Room substrate process furnace, 6-composite molecular pump, the 7-mechanical pump, 8-magnetic force transmission pole, 9-ion gauge, 10-sample turret operation handle arm, the 11-preparation room of growing, 12-sample turret, 13-growth preparation room viewing window, 14-growth preparation room substrate heater, slide valve between 15-growth preparation room and the growth room, connecting passage between 16-growth preparation room and the growth room, 17-sputter ion pump, 18-sample turret operation handle arm, the 19-stepper-motor, the 20-growth room, 21-computer, 22-growth room viewing window, at the bottom of the 23-isolation liner with electron gun fender plate, 24-electron gun fire door shutter, 25-electron gun stove, 26-circulating water cooling system, 27-growth room substrate process furnace, the 28-ion gauge, 29-titanium sublimation pump, 30-sputter ion pump.
Embodiment
Below in conjunction with accompanying drawing the growing apparatus that the present invention prepares IV-VI family semiconductor single crystal thin film is carried out the detail description:
Embodiment 1
A kind of growing apparatus for preparing IV-VI family semiconductor single crystal thin film includes growth apparatus, pumped vacuum systems, heating system, cooling system, Controlling System and computer control system, the Sample Room of described growth apparatus, the growth preparation room, the structure of growth room is as follows:
Referring to accompanying drawing 1, Sample Room 1 includes: Sample Room sample driven rod 8 adopts the magnetic force driven rod, adopts series rotary sheet type mechanical pump 7 and composite molecular pump 6 to form the pumped vacuum systems of Sample Room, and Sample Room specimen holder 2 is placed substrate; The Sample Room vacuum measurement is measured by ion gauge 9, Sample Room substrate heating tungsten-iodine lamp 5, Sample Room links to each other by connecting passage 4 between the preparation room with growth, and by the Sample Room and slide valve 3 isolation between the preparation room of growing, the degasification back substrate is imported the preparation room 11 of growing into by magnetic force transmission pole 8.The major function of Sample Room 1 is substrate to be packed into have in the system of high vacuum and ultrahigh vacuum(HHV) vacuum≤5 * 10 from atmosphere
-5Pa will be adsorbed on air scavenge on the substrate by tungsten-iodine lamp heating, and temperature is ℃ adjustable from room temperature～200.
Referring to accompanying drawing 2, the growth preparation room 11 of growth apparatus includes: sample turret operation handle arm 10 and sample turret 12 connect and compose the growth preparation room specimen holder of liftable and rotation, three sample holders are arranged on the specimen holder 12, can store, handle three samples, rotate specimen holder 12 can be convenient to the to grow sample of sample and Sample Room or growth room of preparation room and join; Growth preparation room substrate process furnace 14 adopts graphite, and is ℃ controllable to substrate heating temperature room temperature～800; Sputter ion pump 17 is connected with growth preparation room 11, keeps the ultrahigh vacuum(HHV) of growth preparation room; Growth preparation room viewing window 13 is convenient to the transfer operation of sample; Link to each other by connecting passage 4 between growth preparation room and the Sample Room, by slide valve 3 isolation between preparation room and the Sample Room of growing; Growth links to each other by connecting passage 16 between preparation room and the growth room, by slide valve 15 isolation between preparation room and the growth room of growing; Sample substrate is imported growth room 20 by magnetic force driven rod 8 into by growth preparation room 11.The major function of growth preparation room is: possess very clean ultra-high vacuum environment, can reach 6.6 * 10
-8Pa; 2) to the further degasification of gas of substrate absorption, the highest degasification temperature can reach 800 ℃.
Referring to accompanying drawing 3, the growth room 20 of growth apparatus includes: the growth preparation room specimen holder that is made of liftable and rotation sample turret lifting handle 17 and sample turret 22, sample turret lifting handle 18 connects 19 by stepper-motor and drives, stepper-motor 19 is connected with computer 21, the speed of rotation of control specimen holder; Adopt sputter ion pump 30 and titanium sublimation pump 29 to form the pumped vacuum systems of growth room; Ion gauge 28 measurement of vacuum; Growth room's viewing window 22 is examined the situation in the growth room; Growth room's specimen holder and substrate process furnace are 27, and room temperature～800 are ℃ controllable, and temperature fluctuation is in ± 1 ℃; There is electron gun stove 25 (totally 8 in electron gun stove) in specimen holder 27 bottoms, and each electron gun stove is equipped with different high-purity source materials, with at the bottom of master shield 23 isolation liner with the electron gun stove, there is a shutter 24 at each electron gun fire door place, closing and spray in order to the control line; The speed of line size decision growth has ion gauge 28 to measure the line size.Cooling circulates around 26 pairs of electron gun stoves of circulating water cooling system adopting process cooling-water machine of the present invention.The function of growth room mainly is to finish the growth of high-quality IV-VI family's semiconductor crystal film and heterojunction structure thereof, and the size of sample can be 2 inches or 3 inches or bigger.
Embodiment 2:
The preparation IV-VI family semiconductor crystal film growing apparatus of utilization inventive embodiments 1 is at BaF
2(111) operating process of growth PbTe monocrystal thin films is as follows on the substrate:
● with BaF
2Substrate is placed in the vertical laminar flow clean work station, along (111) face cleavage, blows off with high pure nitrogen;
● with BaF
2Substrate is packed on the Sample Room specimen holder 4, take out 10 minutes with mechanical pump 3 after, take out half hour with composite molecular pump 8 again, be evacuated to≤5 * 10
-5Pa, Sample Room process furnace 7 tungsten-iodine lamp heated substrate was 150-200 ℃ of degasification 30 minutes;
● after the degasification with the BaF on the Sample Room specimen holder 2
2Substrate, at room temperature import on the rotation specimen holder 12 substrate lifting tables of growth in the preparation room 11 in three sample holders by magnetic force transmission pole 8, and close Sample Room 1 and the slide valve 3 of growth between the preparation room 11, guarantee ultrahigh vacuum(HHV) in the growth preparation room 11 with sputter ion pump 17, growth preparation room substrate heater 14 usefulness graphite are heated to 600 ℃ of degasification 30 minutes with substrate;
● to electron gun stove 25 degasification of PbTe source material are housed in the growth room 20, PbTe electron gun stove 25 is warming up to about 700 ℃, and is being higher than 15 ℃ of growth line temperature electron gun stove degasification 10 minutes; To electron gun stove 25 degasification of Te source, Te electron gun stove 25 is warming up to about 350 ℃, degasification 10 minutes, measure molecular beam with ion gauge 28, line size decision growth velocity, by regulating electron gun furnace temperature control molecular beam line size, in degasification and process of growth, all use 26 pairs of electron gun stoves of recirculated water, growth room's outer wall refrigeration always, the maintenance of ultrahigh vacuum(HHV) is realized by ionic pump 30;
● the BaF in the preparation room 11 of will growing
2Substrate, at room temperature import on the rotation specimen holder 27 in the growth room 21 by magnetic force transmission pole 8, slide valve 15 between growth preparation room and the growth room is isolated growth room and growth preparation room, and takes out growth room's vacuum to≤5 * 10 with sputter ion pump 30 and titanium sublimation pump 29
-8The ultrahigh vacuum(HHV) degree of Pa;
● come heated substrate with substrate tantalum piece well heater, making its temperature is 470 ℃ of degasification 10 minutes, therebetween the substrate and the electron gun stove 25 of isolating on the specimen holder 27 with baffle plate 23;
● underlayer temperature is adjusted to 450 ℃, keeps the underlayer temperature fluctuation in ± 1 ℃, open stepper-motor 19, the control rotating speed changes at per minute 3.Open PbTe and Te electron gun stove shutter 24 simultaneously, open specimen holder baffle plate 23, begin growth;
● when PbTe monocrystal thin films growth time reaches 1 hour, close the electron gun stove, finish growth, and underlayer temperature is reduced to room temperature.
● spread out of the growth room to the preparation room of growing by the sample that it is good that the magnetic force transfer system will be grown, have the growth preparation room to pass to Sample Room again, Sample Room is filled high pure nitrogen to 1 normal atmosphere, open the dress sample door of Sample Room, take out sample.
Claims (9)
1, a kind of preparation IV-VI family semiconductor crystal film growing apparatus, include growth apparatus, pumped vacuum systems, heating system, cooling system, Controlling System, it is characterized in that: described growth apparatus is by Sample Room, the growth preparation room, three vacuum chambers in growth room connect and compose successively, reach between growth preparation room and the growth room between Sample Room and the growth preparation room and isolate by slide valve, Sample Room has the sample driven rod to transmit substrate with the growth preparation room, and growth preparation room and growth room have the sample driven rod to transmit substrate, and there is the specimen holder of liftable and rotation growth preparation room and growth room, there be 2-8 electron gun stove in growth room specimen holder bottom, isolates specimen holder and electron gun stove by baffle plate.
2, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that the Sample Room of described growth apparatus, include: the pumped vacuum systems of forming by mechanical pump and composite molecular pump; Place the specimen holder of substrate, substrate is by in the specimen holder holder of packing in the clean by laminar flow worktable; The measurement of vacuum ion gauge; Sample Room links to each other between the preparation room with growth, is isolated by the vacuum lock plate valve; The sample driven rod.
3, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that the growth preparation room of described growth apparatus, include: the specimen holder of liftable and rotation has a plurality of sample holders on the specimen holder; Process furnace; Sputter ion pump; Have a viewing window; The growth preparation room links to each other with the growth room, is isolated by the vacuum lock plate valve; Growth preparation room sample driven rod.
4, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that the growth room of described growth apparatus, include: the pumped vacuum systems of forming the growth room by sputter ion pump and titanium sublimation pump; The ion gauge of measurement of vacuum; Have growth room's viewing window; Have the specimen holder of liftable and rotation to be connected with stepper-motor, stepper-motor is connected with computer, the speed of rotation of control specimen holder; Substrate tantalum piece process furnace; There are many electron gun stoves in growth room specimen holder bottom; The line of measurement size line rule are arranged; The adopting process cooling-water machine constitutes cooling system around the electron gun stove.
5, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that described electron gun stove, there is a shutter at each electron gun fire door place, with at the bottom of the baffle plate isolation liner with the electron gun stove, the electron gun stove be 2-8 only, accuracy of temperature control is ± 0.5 ℃, and is ℃ continuous adjustable controlled in room temperature～1200.
6,, it is characterized in that the controllable speed of rotation of described stepper-motor when sample grown is 0～30 rev/min of stepless speed regulation according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus.
7, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that described heating system, the Sample Room process furnace is a tungsten-iodine lamp, and is ℃ controllable in room temperature～200; Pretreatment chamber's process furnace is a graphite heating, and is ℃ controllable in room temperature～350; Growth room's process furnace is tantalum piece heating, and is ℃ controllable in room temperature～800.
8, according to the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus, it is characterized in that described Controlling System, by power supply, temperature control power supply, stepper-motor rotation control power supply, the digital display vacuumometer, the series rotary sheet type mechanical pump, compound molecule pumping source, plasma sputter pumping source, the sublimation pump power supply is formed, by the computer system accuracy controlling.
9, the working process of the described preparation of claim 1 IV-VI family semiconductor crystal film growing apparatus the steps include:
● substrate is packed on the Sample Room specimen holder, vacuumize with mechanical pump, composite molecular pump, heating makes the substrate degasification;
● on the specimen holder with substrate liftable and rotation in import the growth preparation room into the magnetic force transmission pole after the degasification, close the slide valve between Sample Room and the growth preparation room, take out ultrahigh vacuum(HHV) in the preparation room of growing, the substrate bake out;
● the different high-purity variant electron gun stove of source material intensification degasification will be housed, measure molecular beam, in degasification and process of growth, all electron gun stove and growth room's outer wall be cooled off always with recirculated water with ion gauge;
● the substrate in the preparation room of will growing at room temperature imports on the specimen holder of liftable and rotation in the growth room with the magnetic force transmission pole, isolate growth room and growth preparation room with slide valve, and take out growth room's vacuum to the ultrahigh vacuum(HHV) degree with ionic pump and sublimation pump, with tantalum piece substrate is heated, use at the bottom of the baffle plate isolation liner and the electron gun stove;
● underlayer temperature is adjusted to growth temperature, keeps the underlayer temperature fluctuation in ± 1 ℃, drive stepper-motor, the control rotating speed is opened 2-8 electron gun fender plate as required simultaneously, opens the specimen holder baffle plate, begins growth;
● when the monocrystal thin films growth is finished, close the electron gun stove, finish growth, and underlayer temperature reduced to room temperature, spread out of the growth room to the preparation room of growing by the sample that it is good that the magnetic force transfer system will be grown, have the growth preparation room to pass to Sample Room again, Sample Room is filled high pure nitrogen to 1 normal atmosphere, open the dress sample door of Sample Room, take out sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100688632A CN100549242C (en) | 2007-05-17 | 2007-05-17 | A kind of growing apparatus for preparing IV-VI family semiconductor single crystal thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101236905B (en) * | 2008-03-05 | 2010-10-13 | 浙江大学 | A method for making IV-VI sector semiconductor single crystal film on CdZnTe underlay |
| CN102393468A (en) * | 2011-08-28 | 2012-03-28 | 大连齐维科技发展有限公司 | Multistage differential pumped ultrahigh vacuum sample transmission mechanism |
| CN102677162A (en) * | 2012-05-09 | 2012-09-19 | 中国科学院上海技术物理研究所 | Full-automatic control liquid phase epitaxy device and control method |
| CN103594096A (en) * | 2012-08-17 | 2014-02-19 | 西部数据传媒公司 | Dual single sided sputter chambers with sustaining heater |
| CN106367806A (en) * | 2016-10-09 | 2017-02-01 | 中国工程物理研究院激光聚变研究中心 | Method for reducing concentration of impurities of GaAs material and growth process of GaAs material |
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| CN109402732A (en) * | 2017-08-17 | 2019-03-01 | 中国科学院物理研究所 | Molecular beam epitaxy system |
| CN111379021A (en) * | 2018-12-29 | 2020-07-07 | 中国科学院上海微系统与信息技术研究所 | Sample holder |
| CN112289711A (en) * | 2020-10-23 | 2021-01-29 | 西北工业大学 | Low-temperature substrate heating table for growing semiconductor film and manufacturing method thereof |
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- 2007-05-17 CN CNB2007100688632A patent/CN100549242C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101236905B (en) * | 2008-03-05 | 2010-10-13 | 浙江大学 | A method for making IV-VI sector semiconductor single crystal film on CdZnTe underlay |
| CN102393468A (en) * | 2011-08-28 | 2012-03-28 | 大连齐维科技发展有限公司 | Multistage differential pumped ultrahigh vacuum sample transmission mechanism |
| CN102677162A (en) * | 2012-05-09 | 2012-09-19 | 中国科学院上海技术物理研究所 | Full-automatic control liquid phase epitaxy device and control method |
| CN103594096A (en) * | 2012-08-17 | 2014-02-19 | 西部数据传媒公司 | Dual single sided sputter chambers with sustaining heater |
| CN106367806A (en) * | 2016-10-09 | 2017-02-01 | 中国工程物理研究院激光聚变研究中心 | Method for reducing concentration of impurities of GaAs material and growth process of GaAs material |
| CN106367806B (en) * | 2016-10-09 | 2019-02-01 | 中国工程物理研究院激光聚变研究中心 | A kind of growth technique of the method reducing GaAs impurities of materials concentration and GaAs material |
| CN108068118A (en) * | 2016-11-14 | 2018-05-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of sample conveyance system applied to vacuum interacted system |
| CN108068118B (en) * | 2016-11-14 | 2021-06-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Sample conveying system applied to vacuum interconnection system |
| CN109402732A (en) * | 2017-08-17 | 2019-03-01 | 中国科学院物理研究所 | Molecular beam epitaxy system |
| CN108060458A (en) * | 2017-12-12 | 2018-05-22 | 沈阳理工大学 | A kind of preparation facilities and method of nonpolar indium nitride nano-crystal film |
| CN111379021A (en) * | 2018-12-29 | 2020-07-07 | 中国科学院上海微系统与信息技术研究所 | Sample holder |
| CN112289711A (en) * | 2020-10-23 | 2021-01-29 | 西北工业大学 | Low-temperature substrate heating table for growing semiconductor film and manufacturing method thereof |
| CN112289711B (en) * | 2020-10-23 | 2024-04-26 | 西北工业大学 | Low-temperature substrate heating table for growing semiconductor film and manufacturing method thereof |
| CN113279063A (en) * | 2021-04-23 | 2021-08-20 | 南昌大学 | IV-VI family infrared semiconductor film and preparation method thereof |
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