CN1731594A - Method for preparing nano-micrometer lacunaris SiGe thermoelectric material - Google Patents
Method for preparing nano-micrometer lacunaris SiGe thermoelectric material Download PDFInfo
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- CN1731594A CN1731594A CN 200510012295 CN200510012295A CN1731594A CN 1731594 A CN1731594 A CN 1731594A CN 200510012295 CN200510012295 CN 200510012295 CN 200510012295 A CN200510012295 A CN 200510012295A CN 1731594 A CN1731594 A CN 1731594A
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Abstract
The invention discloses a method for making a nano-micro meter multi holes germanium-silicon alloy pyroelectric material. The invention involve the preparation of nano-micro meter multi holes germanium-silicon alloy chips that contain silicon of nanometer size, In, InSb or Sb quantum wire or points. The silicon of nanometer and germanium-silicon quantum wires can be prepared by exploiting electrochemical corrosion, physical vapor phase deposition and secondary chemical corrosion. The multi holes germanium-silicon alloy metal chip comprises In, InSb or Sb and the general weight percentage of them is less than 2%; it has quantized structure of real-hollow combination for separating the actions of electrons and acoustic phonon and improving pyroelectricity property.
Description
Technical field
The invention belongs to thermoelectricity (thermoelectric) technical field of semiconductor, a kind of preparation method of nano-micrometer lacunaris SiGe thermoelectric material particularly is provided, has related to the Si that contains nanoscale, Ge, In, the nano-micrometer lacunaris SiGe sheet (Si of InSb or Sb quantum wire or point
1-xGe
x(x=0-0.35)) preparation.
Background technology
The thermoelectric material that has obtained practical application from the last century since the fifties is semi-conducting material.Wherein the problem of Cun Zaiing is that conversion efficiency of thermoelectric is low.For the conversion efficiency scientists that improves thermoelectric material has been carried out number of research projects, but never have big progress, the dimensionless figure of merit (ZT) of thermoelectric material is paced up and down about 1 always, is research and the expection that representative is applied to the solid quantum theory thermoelectric material up to the last century nineties with U.S. scientist: the thermoelectric material with quantum structure-comprise quantum dot, quantum wire will have far above current material even be higher than the heat-photoelectric transformation efficiency of existing hot machine.This result makes the research of the thermoelectric material with quantum-dot structure become the interior main direction of studying of world today's scope.Yet lot of experiment results but with theoretical expect differ greatly.
Silicon-Germanium alloy semiconductor material adopts floating zone method or pressure sintering production more, is the thermoelectric material that is applied to space probe (SNAP-10A number) the earliest.Be characterized in high temperature resistant, the high temperature coefficient of expansion is little, and the elevated temperature heat electrical property is higher, the high temperature of its n type material (927 ℃) ZT value reaches 0.938, the high temperature of P-type material (827K ℃) ZT value reaches 0.505, its problem be thermal conductivity higher-be respectively 4.2 and 4.14 (W/MK) (document Rowe D.M., CRC Handbook of Thermoelectrics, p334-335).If can further reduce its thermal conductivity, certainly will its thermoelectricity capability will be improved further, it is basis material that this patent then adopts high electricity to lead the sige alloy thin slice, adds method preparation that physical vapour deposition (PVD) adds chemical corrosion by electrochemical corrosion and receives the micrometer lacunaris SiGe sheet.
In addition, it has been generally acknowledged that at present and have only methods such as adopting chemical vapour deposition (CVD) or ion beam sputtering just might obtain to have the material of quantum well, line and dot structure, these methods are compared with the simple physics vapour deposition process all to be had equipment and has high input complex process, characteristics such as production cost height.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-micrometer lacunaris SiGe thermoelectric material, can increase substantially SiGe series (Si
1-xGe
x(x=0-0.35)) thermoelectricity capability of thermoelectric material, and preparation technology is simple, and cost is low.
The method that the present invention adopts electrochemical corrosion, physical vapor evaporation, secondary chemical corrosion to combine, obtain a series of silicon or SiGe quantum wires that contain nanoscale, in the hole of lacunaris SiGe sheet, contain In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point, the nano-micrometer lacunaris SiGe material of formation reality-empty binding capacity minor structure.Concrete processing step is as follows:
1, adopts high conductivity sige alloy (Si
1-xGe
x(x=0-0.35)) sheet is raw material;
2, adopt washing agent respectively, it is as follows that deionized water and ultrasonic method are thoroughly cleaned sige alloy sheet cleaning step:
(1) with washing agent and washed with de-ionized water sige alloy sheet,
(2) cleaned 20～25 minutes with ultrasonic wave (interior dress deionized water), ultrasonic frequency is 20～25KHz;
3, adopt the method for electrochemical corrosion that the sige alloy sheet is carried out the corrosion first time, current density is 10～30mA/cm
2Etching time is 0.5～20 minute, and corrosive liquid consists of the hydrofluoric acid of concentration 10%～20%, is thorough the cleaning 30～35 minutes of ultrasonic environment ultrasonic wave of 20～25KHz in condition with deionized water afterwards;
4, the sige alloy sheet that will clean with air-heater is dried rapidly and is placed on the sample stage of vacuum chamber, then vacuum chamber is begun to vacuumize until working vacuum degree 2-3 * 10
-3Pa;
5, selecting the method for single source physical vapour deposition (PVD), and be that 1/1 InSb alloy is a vapor deposition source with atomic ratio, is the InSb film of 600～900nm at lacunaris SiGe sheet surface deposition thickness, and concrete technological parameter is as shown in table 1:
The technological parameter of the single source of table 1 physical vapour deposition (PVD) InSb film
| Evaporation source temperature ℃ | Substrate temperature ℃ | Evaporation time, minute | Vacuum degree, Pa |
| 1200-1300 | 150-200 | 10-20 | 2-3×10 -3 |
6, heat treatment lacunaris SiGe sheet 3～6 hours in 100～500 ℃ temperature range;
7, heat treated porous silicon chip is carried out the corrosion second time, etching time is 3～12 minutes, and corrosive liquid consists of: HF/HNO
3/ H2O=1/3/20-1/3/30;
8, adopt deionized water to carry out ultrasonic waves for cleaning 20～25 minutes, ultrasonic frequency is 20～25Hz;
9, the sige alloy sheet that will clean with air-heater is dried rapidly, obtains containing a series of silicon with nanoscale, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.
In the prepared lacunaris SiGe sheet that goes out of the present invention: In, the weight total content of InSb or Sb is less than 2%, they are with In, the form of InSb or Sb quantum wire or point is present in the hole of lacunaris SiGe sheet, and this result can be achieved by the solution composition of corrosion for the second time and the control of etching time fully.
The present invention is on the basis of the design philosophy of the hollow quantum effect (structure) of thermoelectric material and occupied space binding capacity minor structure (effect), the silicon that contains a series of nanoscales or the SiGe that are obtained, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point, make electronics and phonon moved apart by this structure, thereby realize increasing substantially of thermoelectricity capability, and find that by the mensuration of thermoelectricity capability this structure nano-micrometer lacunaris SiGe sheet has the much higher thermoelectricity capability of more original sige alloy, this result of study can be applicable to the research of superior performance SiGe laser.
The present invention adopts single source physical gas-phase deposite method, and to have technology easy for the methods such as chemical vapour deposition (CVD) of conventional preparation quantum well, quantum wire or quantum dot, the advantage that cost is low.
Description of drawings
Fig. 1 is high-resolution-ration transmission electric-lens nano-micrometer lacunaris SiGe sheet germanium alloy of the present invention (embodiment 3) microstructure photo figure, contains In, InSb or the Sb quantum wire of nanoscale in visible its hole of the table of comparisons 5 data.
Fig. 2 is the SPM shape appearance figure of embodiments of the invention 3 samples.Visible nano-pore that wherein exists of the SPM microstructure analysis result of sample and outstanding nano-silicon or SiGe quantum wire or dot structure.
Embodiment
Embodiment 1
1) adopts high conductivity, and the sige alloy (Si of oxide film protection is arranged
1-xGe
x(x=0)) be raw material;
2) adopt abluent respectively, deionized water and ultrasonic method are thoroughly cleaned the sige alloy sheet, and cleaning step is as follows:
(1) with washing agent and washed with de-ionized water sige alloy sheet,
(2) cleaned 20 minutes with ultrasonic wave (interior dress deionized water), ultrasonic frequency is 20KHz;
3) adopt the method for electrochemical corrosion that the sige alloy sheet is carried out the corrosion first time, current density is 10mA/cm
2Etching time is 0.5 minute, and corrosive liquid consists of the hydrofluoric acid of concentration 10%, is thorough the cleaning 35 minutes of ultrasonic environment ultrasonic wave of 20KHz in condition with deionized water afterwards;
4) the sige alloy sheet that will clean with air-heater is dried rapidly and is placed on the sample stage of vacuum chamber, then vacuum chamber is begun to vacuumize until the working vacuum degree;
5) selecting the method for single source physical vapour deposition (PVD), and be that 1/1 InSb alloy is a vapor deposition source with atomic ratio, is the InSb film of 600-700nm at lacunaris SiGe sheet surface deposition thickness, and concrete technological parameter is as shown in table 1:
The technological parameter of the single source of table 2 physical vapour deposition (PVD) InSb film
| Evaporation source temperature ℃ | Substrate temperature ℃ | Evaporation time, minute | Vacuum degree, Pa |
| 1200 | 150 | 10 | 3×10 -3 |
5) 100 ℃ of heat treatment lacunaris SiGe sheets 3 hours;
6) heat treated lacunaris SiGe sheet is corroded again, etching time is 3 minutes, and wherein corrosive liquid consists of HF/HNO
3/ H
2O=1/3/20;
7) adopt deionized water to carry out ultrasonic waves for cleaning 20 minutes, ultrasonic frequency is 20kHz;
8) the sige alloy sheet that will clean with air-heater is dried rapidly, obtains containing a series of silicon with nanoscale, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.
Embodiment 2
1) adopts high conductivity, and the sige alloy (Si of oxide film protection is arranged
1-xGe
x(x=0.35)) be raw material;
2) adopt abluent respectively, deionized water and ultrasonic method are thoroughly cleaned the sige alloy sheet, and cleaning step is as follows:
(1) with washing agent and washed with de-ionized water sige alloy sheet,
(2) cleaned 25 minutes with ultrasonic wave (interior dress deionized water), ultrasonic frequency is 25KHz;
3) adopt the method for electrochemical corrosion that the sige alloy sheet is carried out the corrosion first time, current density is 20mA/cm
2Etching time is 10 minutes, and corrosive liquid consists of the hydrofluoric acid of concentration 15%, is thorough the cleaning 30 minutes of ultrasonic environment ultrasonic wave of 20KHz in condition with deionized water afterwards;
4) the sige alloy sheet that will clean with air-heater is dried rapidly and is placed on the sample stage of vacuum chamber, then vacuum chamber is begun to vacuumize until the working vacuum degree;
5) selecting the method for single source physical vapour deposition (PVD), and be that 1/1 InSb alloy is a vapor deposition source with atomic ratio, is the InSb film of 700-800nm at lacunaris SiGe sheet surface deposition thickness, and concrete technological parameter is as shown in table 1:
The technological parameter of the single source of table 3 physical vapour deposition (PVD) InSb film
| Evaporation source temperature ℃ | Substrate temperature ℃ | Evaporation time, minute | Vacuum degree, Pa |
| 1250 | 125 | 15 | 3×10 -3 |
6) 300 ℃ of heat treatment lacunaris SiGe sheets are 4.5 hours;
7) heat treated lacunaris SiGe sheet is corroded again, etching time is 6 minutes, and wherein corrosive liquid consists of HF/HNO
3/ H
2O=1/3/25;
8) adopt deionized water to carry out ultrasonic waves for cleaning 20 minutes, ultrasonic frequency is 20KHz;
9) the sige alloy sheet that will clean with air-heater is dried rapidly, obtains containing a series of silicon or SiGes with nanoscale, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.
Embodiment 3
1) adopts high conductivity, and the sige alloy (Si of oxide film protection is arranged
1-xGe
x(x=0.05)) be raw material;
2) adopt abluent respectively, deionized water and ultrasonic method are thoroughly cleaned the sige alloy sheet, and cleaning step is as follows:
(1) with washing agent and washed with de-ionized water sige alloy sheet,
(2) cleaned 23 minutes with ultrasonic wave (interior dress deionized water), ultrasonic frequency is 25KHz;
3) adopt the method for electrochemical corrosion that the sige alloy sheet is carried out the corrosion first time, current density is 10-30mA/cm
2Etching time is 20 minutes, and corrosive liquid consists of the hydrofluoric acid of concentration 20%, is thorough the cleaning 30 minutes of ultrasonic environment ultrasonic wave of 20KHz in condition with deionized water afterwards;
4) the sige alloy sheet that will clean with air-heater is dried rapidly and is placed on the sample stage of vacuum chamber, then vacuum chamber is begun to vacuumize until the working vacuum degree;
5) selecting the method for single source physical vapour deposition (PVD), and be that 1/1 InSb alloy is a vapor deposition source with atomic ratio, is the InSb film of 850-900nm at lacunaris SiGe sheet surface deposition thickness, and concrete technological parameter is as shown in table 1:
The technological parameter of the single source of table 3 physical vapour deposition (PVD) InSb film
| Evaporation source temperature ℃ | Substrate temperature ℃ | Evaporation time, minute | Vacuum degree, Pa |
| 1300 | 200 | 20 | 2.5×10 -3 |
6) 500 ℃ of heat treatment lacunaris SiGe sheets 6 hours;
7) heat treated lacunaris SiGe sheet is corroded again, etching time is 12 minutes.Wherein corrosive liquid consists of HF/HNO
3/ H
2O=1/3/30;
8) adopt deionized water to carry out ultrasonic waves for cleaning 20 minutes, ultrasonic frequency is 25KHz;
9) the sige alloy sheet that will clean with air-heater is dried rapidly, obtains containing the silicon or the SiGe of nanoscale, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.See Fig. 1, adopt this method to form as can be seen from Figure and have receiving-the micrometer lacunaris SiGe sheet of reality-empty binding capacity minor structure (InSb or Sb quantum wire or point being the actual quantities minor structure for the silicon of nanoscale or SiGe, In, and nano-pore is empty quantum structure).Table 5 has provided among Fig. 1 the micro-analysis of components result corresponding to silicon or SiGe quantum wire zone (zone 1) and hole zone (regional 2).As seen be silicon and germanium at silicon or SiGe quantum wire or the Main Ingredients and Appearance that do not have a zone of obvious pore structure, then also contain metal In, InSb or Sb outside silica removal and the germanium in the hole zone.See Fig. 2, as can be seen the SPM microstructure analysis result of respective sample.As seen nano-pore that wherein exists and outstanding nano-silicon or SiGe quantum wire or dot structure.
Table 5 is corresponding to the micro-composition EDS analysis result in zone 1 in the accompanying drawing 1 and zone 2
| Element | Zone 1, atom % | Zone 2, atom % |
| Si | 95 | 90.58 |
| Ge | 5 | 4.76 |
| In | 3.43 | |
| Sb | 1.22 |
Table 6 has provided silicon that contains nanoscale or the SiGe that original sige alloy, embodiment 3 are obtained, In, the thermoelectricity capability of the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.As seen the thermoelectricity capability of lacunaris SiGe sheet is higher than original sige alloy far away.
Original sige alloy sheet of table 6 and the thermoelectricity capability (127 ℃) of lacunaris SiGe sheet after the corrosion repeatedly
| Conductivity (Ω cm) -1 | Seebeck coefficient (μ vK -1) | Power factor [μ W (mK 2) -1] | Thermal capacitance (J. (g.K) -1) | Thermal conductivity [W (m.K) -1] | Figure of merit ZT | |
| Original sige alloy sheet | 990.10 | -136 | 2490.55 | 0.647 | 4.45 | 0.165 |
| The lacunaris SiGe sheet | 840.51 | -195 | 3196.04 | 2.79 | 0.458 |
Claims (3)
1, a kind of preparation method of nano-micrometer lacunaris SiGe thermoelectric material, the method that adopts electrochemical corrosion, physical vapor evaporation, secondary chemical corrosion to combine, obtain a series of silicon or SiGe quantum wires that contain nanoscale, in the hole of lacunaris SiGe sheet, contain In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point, the nano-micrometer lacunaris SiGe material of formation reality-empty binding capacity minor structure; Concrete processing step is:
A, employing high conductivity sige alloy (Si
1-xGe
x(x=0-0.35)) sheet is raw material;
B, adopt washing agent respectively, deionized water and ultrasonic method are thoroughly cleaned the sige alloy sheet;
The method of c, employing electrochemical corrosion is carried out the corrosion first time to the sige alloy sheet, and current density is 10～30mA/cm
2Etching time is 0.5～20 minute, and corrosive liquid consists of the hydrofluoric acid of concentration 10%～20%, is the ultrasonic environment ultrasonic waves for cleaning 30～35 minutes of 20～25KHz in condition with deionized water afterwards;
D, the sige alloy sheet oven dry that will clean with air-heater also place on the sample stage of vacuum chamber, then vacuum chamber are begun to vacuumize until the working vacuum degree;
The method of e, the single source of selection physical vapour deposition (PVD), and be that 1/1 InSb alloy is a vapor deposition source with atomic ratio, at lacunaris SiGe sheet surface deposition thickness is the InSb film of 600～900nm, technological parameter is: the evaporation source temperature: 1200～1300 ℃, substrate temperature: 150～200 ℃, evaporation time: 10～20 minutes, vacuum degree: 2～3 * 10
-3Pa;
F, in 100～500 ℃ temperature range heat treatment lacunaris SiGe sheet 3～6 hours;
G, heat treated porous silicon chip is carried out second time corrosion, etching time is 3～12 minutes, and corrosive liquid consists of:
HF/HNO
3/H2O＝1/3/20～1/3/30；
H, employing deionized water carried out ultrasonic waves for cleaning 20～25 minutes, and ultrasonic frequency is 20～25Hz;
I, the sige alloy sheet that will clean with air-heater are dried rapidly, obtain containing a series of silicon with nanoscale, In, the nano-micrometer lacunaris SiGe sheet of InSb or Sb quantum wire or point.
2, according to the described preparation method of claim 1, it is characterized in that: cleaning sige alloy sheet cleaning step is: at first use washing agent and washed with de-ionized water sige alloy sheet, with adorning washed with de-ionized water 20～25 minutes in the ultrasonic wave, ultrasonic frequency is 20～25KHz then.
3, according to the described preparation method of claim 1, it is characterized in that: the In in the prepared lacunaris SiGe sheet that goes out, InSb or Sb weight total content are less than 2%, they are with In, and the form of InSb or Sb quantum wire or point is present in the hole of lacunaris SiGe sheet.
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| CN100459202C (en) * | 2007-07-02 | 2009-02-04 | 北京科技大学 | Method for preparing silicon-germanium pyroelectric material |
| CN104711444A (en) * | 2015-03-20 | 2015-06-17 | 武汉理工大学 | Method for rapidly preparing high-performance SiGe high-temperature thermoelectric alloy material |
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| KR20060130612A (en) * | 2003-12-19 | 2006-12-19 | 에스씨에프 테크놀로지스 에이/에스 | Systems for preparing fine particles and other substances |
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| CN100459202C (en) * | 2007-07-02 | 2009-02-04 | 北京科技大学 | Method for preparing silicon-germanium pyroelectric material |
| CN104711444A (en) * | 2015-03-20 | 2015-06-17 | 武汉理工大学 | Method for rapidly preparing high-performance SiGe high-temperature thermoelectric alloy material |
| CN107408618A (en) * | 2015-07-21 | 2017-11-28 | 株式会社Lg化学 | Compound semiconductor thermoelectric material and its manufacture method |
| US20180033939A1 (en) * | 2015-07-21 | 2018-02-01 | Lg Chem, Ltd. | Compound semiconductor thermoelectric material and method for manufacturing same |
| JP2018523294A (en) * | 2015-07-21 | 2018-08-16 | エルジー・ケム・リミテッド | Compound semiconductor thermoelectric material and manufacturing method thereof |
| CN107408618B (en) * | 2015-07-21 | 2020-07-07 | 株式会社Lg化学 | Compound semiconductor thermoelectric material and method for producing same |
| CN109607470A (en) * | 2018-11-19 | 2019-04-12 | 南京理工大学 | The preparation method of antimony alkene nanometer sheet |
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| CN110729392A (en) * | 2019-10-23 | 2020-01-24 | 华北电力大学（保定） | Layered silicon-germanium thermoelectric material |
| CN110729392B (en) * | 2019-10-23 | 2023-09-29 | 华北电力大学（保定） | Layered silicon-germanium thermoelectric material |
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