CN103243382A - Hot wall epitaxy device and method for growing bismuth telluride nano film - Google Patents
Hot wall epitaxy device and method for growing bismuth telluride nano film Download PDFInfo
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- CN103243382A CN103243382A CN2013101507521A CN201310150752A CN103243382A CN 103243382 A CN103243382 A CN 103243382A CN 2013101507521 A CN2013101507521 A CN 2013101507521A CN 201310150752 A CN201310150752 A CN 201310150752A CN 103243382 A CN103243382 A CN 103243382A
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Abstract
The invention discloses a hot wall epitaxy device and method for growing a bismuth telluride nano film. The device comprises a vacuum cavity, a growth furnace, an atmosphere compensation furnace, a substrate bracket, a stainless steel baffle, a growth quartz tube and a porous quartz baffle, wherein the growth furnace comprises a compensation source furnace body, a growth source furnace body and a hot wall furnace body; the growth quartz tube with the quartz baffle is placed in the growth furnace; and the atmosphere compensation furnace is a furnace with a single temperature zone and provides a compensation atmosphere for a cooled epitaxy film after the growth is completed. The hot wall epitaxy method for growing the bismuth telluride nano film comprises the following steps: firstly, successively putting a compensation source, a growth source and the porous quartz baffle in the growth quartz tube; after the growth furnace is heated to a preset temperature, removing the stainless steel baffle at a furnace mouth, and lowering the substrate bracket to a growth quartz tube mouth so as to enable the growth to start; and after the growth is completed, rotating a substrate to the atmosphere compensation furnace and cooling down the substrate at a certain speed. By adopting the device and the method, the epitaxial growth of the monocrystal bismuth telluride nano film with stoichiometric proportion can be achieved.
Description
Technical field
The present invention relates to a kind of apparatus and method of hot wall epitaxy semiconductor compound nano film, be particularly suitable for the preparation of Tellurobismuthite or other II-VI family, IV-VI compounds of group nano thin-film, nanostructure.
Background technology
Hot wall extension (HWE) is wall and the substrate of heating source material, growth tube under vacuum condition, carries out thin film epitaxial growth.The key distinction of it and thermal evaporation techniques is that the hot wall between evaporation source and the substrate forms the deposition system near thermodynamic(al)equilibrium, thereby can carry out the single crystal epitaxial growth.From the seventies in 20th century, the hot wall extension has been widely used in epitaxy and the preparation of devices thereof of II-VI family, IV-VI family, III-compounds such as V family, as CdTe, PbTe, GaAs etc.V-VI compounds of group Tellurobismuthite is a kind of traditional thermoelectric material, begins the nineties to utilize the hot wall extension to prepare bismuth telluride thin film.Foretold and confirm to be the three-dimensional topology isolator from Tellurobismuthite, bismuth selenide and bismuth antimonide in 2009, it becomes the new research focus in Condensed Matter Physics field again.Because Tellurobismuthite block materials defective causes its carrier concentration too high, study its topological insulator surface attitude and electronic structure and become difficult.Therefore need preparation thickness at Tellurobismuthite materials such as the film of a few to tens of nanometers, nanometer plate, nano belt, nano wires.
Because growth tube and lid substrate have above it constituted the space of a relative closure in the hot wall epitaxial system, cause the interior air pressure of growth tube than 2-3 order of magnitude of vacuum chamber height of its outside, the source steam forms big supersaturation vapor pressure at substrate surface, thereby make film with bigger speed growth, under optimum growth temp, growth velocity is generally at 1-10 μ m/h.Therefore the hot wall epitaxial method is fit to the thick film of several microns to tens microns of preparations, is not suitable for the growth of nano thin-film.If reduce the growth source temperature merely or improve underlayer temperature and reduce growth velocity, growth conditions can depart from optimised process, causes quality of materials to descend.In addition, because the equilibrium vapor pressure ratio Bi's of Te is big, Te can volatilize in the process of growth and cooling, thereby causes Tellurobismuthite compound nonstoichiometry ratio, forms defectives such as Te room and Bi antiposition, increases carrier concentration, influences its electric property.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide that a kind of growth velocity is controlled, hot wall epitaxial apparatus and the method in band compensation source, the bismuth telluride thin film that epitaxy is ultra-thin, the compensation atmosphere in growth and the temperature-fall period prevents the volatilization of Te, the stoichiometric ratio of control Tellurobismuthite.
A kind of hot wall epitaxial apparatus of the Tellurobismuthite nano thin-film of growing, this device comprise vacuum cavity 1, growth furnace 2, atmosphere compensation stove 3, substrate support 4, stainless steel baffle plate 5, growth quartz tube 6 and quartz baffle with holes 7:
Described vacuum cavity 1 comprises N
2Inlet mouth 11, N
2The venting port 13 of air outlet 12, connection pumped vacuum systems; Described growth furnace 2 places vacuum cavity 1 inside, comprises compensation source body of heater 21, growth source body of heater 22 and hot wall body of heater 23, and they are vertically axle center arrangement successively from the bottom up, and are heat insulation with ceramic plate 24 between compensation source body of heater 21 and the growth source body of heater 22; Described atmosphere compensation stove 3 is single warm area stove, be symmetrically distributed along vacuum cavity 1 central shaft with growth furnace 2, its objective is to the epitaxial film of lowering the temperature behind the growth ending provides a compensation atmosphere, prevents that the element volatilization that equilibrium vapor pressure is big in the compound from causing stoichiometric ratio to depart from; Described substrate support 4 is above growth furnace 2 and atmosphere compensation stove 3 fire doors, comprise overlapping plate-like heater strip 41, Soaking disk 42 and substrate bracket 43 up and down, motor 44 controls by vacuum cavity 1 outside its up and down and rotatablely move, regulate substrate respectively apart from the height and the conversion of realization growth front and back substrate at different furnace rooms of fire door, the material of wherein said Soaking disk 42 and substrate bracket 43 is molybdenum; Described stainless steel baffle plate 5 is put in directly over the fire door of growth furnace 2 and atmosphere compensation stove 3, and is manually mobile by magnetictransmission, and its purpose is to prevent that the source material that evaporates in the heating-cooling process is to the pollution of substrate, epitaxial film; Described growth quartz tube (6) is positioned in the growth furnace (2), by two sections different nested forming of silica tube of diameter, put into growth source and compensation source respectively, put the nozzle position of silica tube 61 in compensation source than the high 50mm in silica tube 62 bottoms of putting growth source, these growth quartz tube 6 mouths of pipe are inlayed a quartz ring 63, be supported on the growth furnace 2, the place of growth quartz tube 6 inner distance mouth of pipe 50mm also has a quartz ring 64 to be used for supporting quartz baffle 7 with holes; Described quartz baffle with holes 7 is positioned over the position of hot wall body of heater 23 correspondences in the growth quartz tube 6, on quartz baffle 7 with holes, open the aperture of certain number equably, owing to be in the hot wall body of heater 23, quartz baffle 7 with holes can increase the elastic collision of gas molecule or atom and baffle plate, reduce the speed that vaporised gas rushes at substrate 45, thereby reduce the supersaturation vapor pressure on substrate 45 surfaces, control growth velocity by diameter and the number of regulating aperture, finally realize the epitaxy of nano thin-film.
A kind of method of hot wall extension of the Tellurobismuthite nano thin-film of growing, its step is as follows:
1. the quartz baffle with holes of 5N Tellurobismuthite compound growth source, 7NTe compensation source and required specification is put into growth quartz tube, then growth quartz tube is put into growth furnace, the silica tube that atmosphere compensates stove is put in Te compensation source, and with the stainless steel baffle plate two fire doors are sealed;
2. after used substrate passes through matting and corrosion, N
2Dry up and put into substrate bracket, and substrate support is placed the baffle plate top of growth furnace;
3. earlier the vacuum cavity that seals is led to N
230 minutes, begin then to vacuumize;
4. vacuum tightness reaches 1 * 10
-4Behind the Pa, begin to heat hot wall, Tellurobismuthite growth source, Te compensation source and substrate, optimum growth temp is respectively 460-520 ℃, 450-510 ℃, 250-350 ℃ and 320-380 ℃, after treating all to reach preset temp, remove the baffle plate of growth furnace, substrate is down to the growth quartz tube mouth of pipe begins epitaxy;
5. after treating that growth finishes, block baffle plate again, to the atmosphere compensation stove fire door that reaches preset temp, epitaxial film and atmosphere compensation stove are with certain speed cooling with the substrate rotation.
Advantage of the present invention is:
1. by regulating little hole number and the diameter of quartz baffle, the control growth velocity realizes hot wall extension nano film material, and improves the sample surfaces pattern, improves crystal mass;
2. the compensation source in growth and the temperature-fall period provides a compensation atmosphere to epitaxial film, prevents that the element volatilization that equilibrium vapor pressure is big in the compound from causing stoichiometric ratio to depart from;
3. be easy to epitaxy II-VI family, IV-VI family, V-compounds such as VI family, be convenient to control stoichiometric ratio;
4. equipment cost is low, and technology is simple, and is easy to operate.
Description of drawings
Fig. 1 is the hot wall epitaxial apparatus structural representation of invention.1-vacuum cavity wherein, 2-growth furnace, 3-atmosphere compensation stove, 4-substrate support, 5-stainless steel baffle plate, 6-growth quartz tube, 7-quartz baffle with holes.
Fig. 2 is the growth quartz tube structural representation.
Fig. 3 is quartz baffle schematic top plan view with holes.
Embodiment
Elaborate the method for hot wall epitaxial apparatus of the present invention and epitaxy Tellurobismuthite nano thin-film below in conjunction with accompanying drawing and specific embodiment:
Fig. 1 is the hot wall epitaxial apparatus structural representation of inventing.This device comprises vacuum cavity 1, growth furnace 2, atmosphere compensation stove 3, substrate support 4, stainless steel baffle plate 5, growth quartz tube 6 and quartz baffle with holes 7:
Described vacuum cavity 1 comprises N
2Inlet mouth 11, N
2The venting port 13 of air outlet 12, connection pumped vacuum systems; Described growth furnace 2 places vacuum cavity 1 inside, comprises compensation source body of heater 21, growth source body of heater 22 and hot wall body of heater 23, and they are vertically axle center arrangement successively from the bottom up, and are heat insulation with ceramic plate 24 between compensation source body of heater 21 and the growth source body of heater 22; Described atmosphere compensation stove 3 is single warm area stove, be symmetrically distributed along vacuum cavity 1 central shaft with growth furnace 2, its objective is to the epitaxial film of lowering the temperature behind the growth ending provides a compensation atmosphere, prevents that the element volatilization that equilibrium vapor pressure is big in the compound from causing stoichiometric ratio to depart from; Described substrate support 4 is above growth furnace 2 and atmosphere compensation stove 3 fire doors, comprise overlapping plate-like heater strip 41, Soaking disk 42 and substrate bracket 43 up and down, motor 44 controls by vacuum cavity 1 outside its up and down and rotatablely move, regulate substrate respectively apart from the height and the conversion of realization growth front and back substrate at different furnace rooms of fire door, the material of wherein said Soaking disk 42 and substrate bracket 43 is molybdenum; Described stainless steel baffle plate 5 is put in directly over the fire door of growth furnace 2 and atmosphere compensation stove 3, and is manually mobile by magnetictransmission, and its purpose is to prevent that the source material that evaporates in the heating-cooling process is to the pollution of substrate, epitaxial film.
Fig. 2 is the structural representation of growth quartz tube 6.By different nested the forming of two ends silica tube of diameter, put into growth source and compensation source respectively, put the nozzle position of silica tube 61 in compensation source than the high 50mm in silica tube 62 bottoms of putting growth source, these growth quartz tube 6 mouths of pipe are inlayed a quartz ring 63, be supported on the growth furnace 2, the place that growth quartz tube 6 inner distance are given birth to mouth of pipe 50mm also has a quartz ring 64 to be used for supporting quartz baffle 7 with holes.
Fig. 3 is quartz baffle 7 schematic top plan view with holes.Described quartz baffle with holes 7 is positioned over the position of hot wall body of heater 23 correspondences in the growth quartz tube 6, on quartz baffle 7 with holes, open the aperture of certain number equably, owing to be in the hot wall body of heater 23, quartz baffle 7 with holes can increase the elastic collision of gas molecule or atom and baffle plate, reduce the speed that vaporised gas rushes at substrate 45, thereby reduce the supersaturation vapor pressure on substrate 45 surfaces, control growth velocity by diameter and the number of regulating aperture, finally realize the epitaxy of nano thin-film.
Embodiment 1, and its step is as follows:
1. be that 0.3mm, number are that 550 quartz baffle with holes 7 is put into growth quartz tube 6 with 5N Tellurobismuthite compound growth source, 7NTe compensation source and hole diameter, then growth quartz tube 6 is put into growth furnace 2, the silica tube that atmosphere compensates stove 3 is put in 7NTe compensation source, and with stainless steel baffle plate 5 two fire doors are sealed;
2.GaAs(111) substrate 45 is earlier with acetone, dehydrated alcohol and deionized water ultrasonic cleaning 15 minutes, then at 80 ℃ H
2SO
4: H
2O
2: H
2O(3:1:1) corroded 30 seconds in the corrosive fluid, behind deionized water rinsing, use N again
2Put into substrate bracket 43 after drying up, and substrate support 4 is placed baffle plate 5 tops of growth furnace 2;
3. earlier the vacuum cavity 1 that seals is led to N
230 minutes, begin then to vacuumize;
4. vacuum tightness reaches 1 * 10
-4Behind the Pa, begin to heat hot wall, Tellurobismuthite growth source, Te compensation source and substrate 45, after temperature reaches 520 ℃, 510 ℃, 350 ℃ and 380 ℃ respectively, remove the baffle plate 5 of growth furnace 2, substrate 45 is down to growth quartz tube 6 mouths of pipe begins epitaxy, growth time is 1 hour;
5. after treating that growth finishes, block baffle plate 5 again, substrate 45 is rotated to being heated to 300 ℃ atmosphere compensation stove 3 fire doors and having begun cooling, epitaxial film and Te compensation source all lower the temperature with the speed of 2 ℃/min.
1. be that 0.2mm, number are that 800 quartz baffle with holes 7 is put into growth quartz tube 6 with 5N Tellurobismuthite compound growth source, 7NTe compensation source and hole diameter, then growth quartz tube 6 is put into growth furnace 2, the silica tube that atmosphere compensates stove 3 is put in 7NTe compensation source, and with stainless steel baffle plate 5 two fire doors are sealed;
2.GaAs(111) substrate 45 is earlier with acetone, dehydrated alcohol and deionized water ultrasonic cleaning 15 minutes, then at 80 ℃ H
2SO
4: H
2O
2: H
2O(3:1:1) corroded 30 seconds in the corrosive fluid, behind deionized water rinsing, use N again
2Put into substrate bracket 43 after drying up, and substrate support 4 is placed baffle plate 5 tops of growth furnace 2;
3. earlier the vacuum cavity 1 that seals is led to N
230 minutes, begin then to vacuumize;
4. vacuum tightness reaches 1 * 10
-4Behind the Pa, begin to heat hot wall, Tellurobismuthite growth source, Te compensation source and substrate 45, after temperature reaches 500 ℃, 490 ℃, 285 ℃ and 360 ℃ respectively, remove the baffle plate 5 of growth furnace 2, substrate 45 is down to growth quartz tube 6 mouths of pipe begins epitaxy, growth time is 1 hour;
5. after treating that growth finishes, block baffle plate 5 again, substrate 45 is rotated to being heated to 285 ℃ atmosphere compensation stove 3 fire doors and having begun cooling, epitaxial film and Te compensation source all lower the temperature with the speed of 2 ℃/min.
Embodiment 3, and its step is as follows:
1. be that 0.15mm, number are that 1000 quartz baffle with holes 7 is put into growth quartz tube 6 with 5N Tellurobismuthite compound growth source, 7NTe compensation source and hole diameter, then growth quartz tube 6 is put into growth furnace 2, the silica tube that atmosphere compensates stove 3 is put in 7NTe compensation source, and with stainless steel baffle plate 5 two fire doors are sealed;
2.GaAs(111) substrate 45 is earlier with acetone, dehydrated alcohol and deionized water ultrasonic cleaning 15 minutes, then at 80 ℃ H
2SO
4: H
2O
2: H
2O(3:1:1) corroded 30 seconds in the corrosive fluid, behind deionized water rinsing, use N again
2Put into substrate bracket 43 after drying up, and substrate support 4 is placed baffle plate 5 tops of growth furnace 2;
3. earlier the vacuum cavity 1 that seals is led to N
230 minutes, begin then to vacuumize;
4. vacuum tightness reaches 1 * 10
-4Behind the Pa, begin to heat hot wall, Tellurobismuthite growth source, Te compensation source and substrate 45, after temperature reaches 460 ℃, 450 ℃, 250 ℃ and 320 ℃ respectively, remove the baffle plate 5 of growth furnace 2, substrate 45 is down to growth quartz tube 6 mouths of pipe begins epitaxy, growth time is 1 hour;
5. after treating that growth finishes, block baffle plate 5 again, substrate 45 is rotated to being heated to 250 ℃ atmosphere compensation stove 3 fire doors and having begun cooling, epitaxial film and Te compensation source all lower the temperature with the speed of 2 ℃/min.
Claims (2)
1. the hot wall epitaxial apparatus of the Tellurobismuthite nano thin-film of growing, this device comprises vacuum cavity (1), growth furnace (2), atmosphere compensation stove (3), substrate support (4), stainless steel baffle plate (5), growth quartz tube (6) and quartz baffle with holes (7), it is characterized in that:
Described vacuum cavity (1) comprises N
2Inlet mouth (11), N
2Air outlet (12) and the venting port that is connected pumped vacuum systems (13); Described growth furnace (2) places vacuum cavity (1) inside, the compensation source body of heater (21) of growth furnace (2), growth source body of heater (22) and hot wall body of heater (23) be vertically axle center arrangement successively from the bottom up, and be heat insulation with ceramic plate (24) between compensation source body of heater (21) and the growth source body of heater (22); Described atmosphere compensation stove (3) is single warm area stove, is symmetrically distributed along vacuum cavity (1) central shaft with growth furnace (2); Described substrate support (4) is in growth furnace (2) and atmosphere compensation stove (3) fire door top, comprise overlapping plate-like heater strip (41), Soaking disk (42) and substrate bracket (43) up and down, control it up and down and rotatablely move by the motor (44) of vacuum cavity (1) outside, the material of wherein said Soaking disk (42) and substrate bracket (43) is molybdenum; Described stainless steel baffle plate (5) is positioned over directly over the fire door of growth furnace (2) and atmosphere compensation stove (3), and is by magnetictransmission, manually mobile; Described growth quartz tube (6) is positioned in the growth furnace (2), by two sections different nested forming of silica tube of diameter, put into growth source and compensation source respectively, put the nozzle position of silica tube (61) in compensation source than the high 50mm in the silica tube of putting growth source (62) bottom, this growth quartz tube (6) mouth of pipe is inlayed a quartz ring (63), be supported on the growth furnace (2), the place of growth quartz tube (6) inner distance mouth of pipe 50mm also has a quartz ring (64) to be used for supporting quartz baffle with holes (7); Described quartz baffle with holes (7) is positioned over the corresponding position of the interior hot wall body of heater of growth quartz tube (6) (23), opens the aperture of certain number on quartz baffle with holes (7) equably.
2. hot wall epitaxy method based on the growth Tellurobismuthite nano thin-film of the described device of claim 1 is characterized in that may further comprise the steps:
1) quartz baffle with holes (7) of 5N Tellurobismuthite compound growth source, 7NTe compensation source and required specification is put into growth quartz tube (6), then growth quartz tube (6) is put into growth furnace (2), the silica tube that atmosphere compensates stove (3) is put in Te compensation source, and with stainless steel baffle plate (5) two fire doors are sealed;
2) after used substrate (45) process matting and the corrosion, N
2Dry up and put into substrate bracket (43), and substrate support (4) is placed baffle plate (5) top of growth furnace (2);
3) earlier the vacuum cavity (1) that seals is led to N
230 minutes, begin then to vacuumize;
4) vacuum tightness reaches 1 * 10
-4Behind the Pa, begin to heat hot wall, Tellurobismuthite growth source, Te compensation source and substrate (45), optimum growth temp is respectively 460-520 ℃, 450-510 ℃, 250-350 ℃ and 320-380 ℃, after treating all to reach preset temp, remove the baffle plate (5) of growth furnace (2), substrate (45) is down to growth quartz tube (6) mouth of pipe begins epitaxy;
5) treat that growth finishes after, block baffle plate (5) again, to atmosphere compensation stove (3) fire door that has reached preset temp, epitaxial film and atmosphere compensation stove are with certain speed cooling with substrate (45) rotation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115613131A (en) * | 2022-10-17 | 2023-01-17 | 江苏汉印机电科技股份有限公司 | Vacuum chamber of silicon carbide epitaxial chemical vapor deposition system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0218383A (en) * | 1988-07-05 | 1990-01-22 | Fujitsu Ltd | Device for hot-wall epitaxial growth |
| JPH07221397A (en) * | 1994-02-02 | 1995-08-18 | Honda Motor Co Ltd | Pbte lattice matching material and its manufacture |
| JPH09184064A (en) * | 1995-12-29 | 1997-07-15 | Honda Motor Co Ltd | Production of chalcopyrite base thin film |
| JP4096418B2 (en) * | 1998-09-25 | 2008-06-04 | ヤマハ株式会社 | Method for depositing group III nitride semiconductor |
| CN203320181U (en) * | 2013-04-26 | 2013-12-04 | 中国科学院上海技术物理研究所 | Hot wall epitaxy device for growth of bismuth telluride nano-films |
-
2013
- 2013-04-26 CN CN2013101507521A patent/CN103243382A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0218383A (en) * | 1988-07-05 | 1990-01-22 | Fujitsu Ltd | Device for hot-wall epitaxial growth |
| JPH07221397A (en) * | 1994-02-02 | 1995-08-18 | Honda Motor Co Ltd | Pbte lattice matching material and its manufacture |
| JPH09184064A (en) * | 1995-12-29 | 1997-07-15 | Honda Motor Co Ltd | Production of chalcopyrite base thin film |
| JP4096418B2 (en) * | 1998-09-25 | 2008-06-04 | ヤマハ株式会社 | Method for depositing group III nitride semiconductor |
| CN203320181U (en) * | 2013-04-26 | 2013-12-04 | 中国科学院上海技术物理研究所 | Hot wall epitaxy device for growth of bismuth telluride nano-films |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115613131A (en) * | 2022-10-17 | 2023-01-17 | 江苏汉印机电科技股份有限公司 | Vacuum chamber of silicon carbide epitaxial chemical vapor deposition system |
| CN115613131B (en) * | 2022-10-17 | 2023-11-28 | 江苏汉印机电科技股份有限公司 | Vacuum chamber of silicon carbide epitaxial chemical vapor deposition system |
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Application publication date: 20130814 |