CN107058950A - A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof - Google Patents
A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof Download PDFInfo
- Publication number
- CN107058950A CN107058950A CN201710238625.5A CN201710238625A CN107058950A CN 107058950 A CN107058950 A CN 107058950A CN 201710238625 A CN201710238625 A CN 201710238625A CN 107058950 A CN107058950 A CN 107058950A
- Authority
- CN
- China
- Prior art keywords
- evaporation source
- temperature
- bismuth telluride
- substrate
- nanometer sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Vapour Deposition (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention discloses bismuth telluride nanometer sheet film of a kind of helical structure and preparation method thereof, is realized by following technical process：In high vacuum thermal evaporation coating machine crucible, a certain amount of high-purity Bi is added2Te3Powder, is positioned over heating region.Substrate sample platform is adjusted to the distance of evaporation source to 10cm, the Fluororystal mica cleaned is placed on substrate sample platform.Open compound molecule pump assembly and be evacuated to 5*10‑5Pa, silicon is to 380 DEG C 400 DEG C, and thermal evaporation sources temperature is heated to 340 DEG C 360 DEG C, starts plated film.5 120min are reacted at this temperature, and evaporation source and underlayer temperature are adjusted to 0 DEG C by control panel, waited after instrument Temperature fall, product is obtained.The method have the characteristics that：The method can directly prepare the bismuth telluride nanometer sheet film of helical structure；Product morphology spiral growth, step is high-visible；Without other products, environmental pollution is small.
Description
Technical field
It is a kind of direct by height the present invention relates to bismuth telluride nanometer sheet film of a kind of helical structure and preparation method thereof
Vacuum thermal evaporation equipment carries out the method that plated film prepares the bismuth telluride nanometer sheet film of helical structure on Fluororystal mica substrate,
Belong to semiconductor nano material technical field.
Background technology
Bismuth telluride is as V-VI group element compounds, and room temperature energy gap is 0.145 eV.Bismuth telluride is trigonal system
Crystal structure, arranged between layers according to the Te-Bi-Te-Bi-Te order repetition periods along c-axis direction.Bismuth telluride belongs to half
Conductor material, is the more room temperature thermoelectricity of domestic and international research performance it is characterized in that the mutual conversion of heat energy and electric energy can be realized
Material.Bismuth telluride material has a wide range of applications in terms of thermo-electric generation and thermoelectric cooling.Bismuth telluride system nano pyroelectric material
Wide in recent years concerned, its nano thin-film and superlattice device directly can be combined with microelectronic processing technique, applied to micro- electricity
The cooling of sub- device and micro battery device.Therefore bismuth telluride thermoelectric material has higher researching value.
The method for preparing bismuth telluride nano film existing at present has a lot, and it, which studies to be concentrated mainly on, prepares thermoelectric figure of merit
（ZT）High bismuth telluride nano material, such as:Chemical vapour deposition technique（CVD）, solvent-thermal method etc..
Chemical vapour deposition technique：2013, Bacel Hamdou et al. were successfully prepared using gold with CVD and are used as catalyst
Catalytic growth bismuth telluride nano-wire structure, after annealing, prepares monocrystalline bismuth telluride nano-wire of good performance.There is text
Offer middle report, the ZT values that theoretical calculation goes out one-dimensional nano line are strongly depend on the diameter of nano wire.When bismuth telluride nano-wire diameter
During less than 5, the ZT values of X-axis orientation nano line can reach 15.Refering to Thermoelectric Characterization of
Bismuth Telluride Nanowires, Synthesized Via Catalytic Growth and Post-
Annealing. Bacel Hamdou, Adv. Mater. 2013,25,239-244 documents.
Solvent-thermal method：2015, Lei Yang et al. were prepared for the side of bismuth telluride six that thickness is 20 nanometers with solvent-thermal method
Piece, sample passes through plasma agglomeration, within the temperature range of 300K to 550K, and its thermal conductivity κ reduces.In 400 K, ZT values reach
To maximum 0.88.Refering to Enhanced Thermoelectric Performance of Nanostructured Bi2Te3
Through Significant Phonon Scattering. Lei Yang, ACS Appl. Mater. Interfaces
2015,7. 23694-23699 documents.
Reported from literature survey and document above, prepare the complex process of bismuth telluride nanostructured, need to be by retreating
Other processing such as fire or plasma agglomeration, take longer, cost height.And prepare helical structure using vacuum thermal evaporation one-step method
Bismuth telluride nanometer sheet film have not been reported, the method technological process is relatively simple, pollutes small, is that one kind prepares bismuth telluride and received
The method of the rice new pattern of structure.Because V-VI group element compounds are layer growth structure, therefore it can be applied to V-VI
The preparation of race's other elements compound, and other layer structures growth element compound preparation.
The content of the invention
It is an object of the invention to provide bismuth telluride nanometer sheet film of a kind of helical structure and preparation method thereof.
The present invention is realized by following technique：
In multi-source high vacuum thermal evaporation coating machine special copple, a certain amount of high-purity Bi is added2Te3Powder, is positioned over multi-source
High vacuum thermal evaporation coating machine evaporation source heating region.Substrate sample platform is adjusted to the distance of evaporation source to 10cm, by sample stage
It is locked in directly over evaporation source.Fluororystal mica is placed on substrate sample platform, is cleaned by ultrasonic before placing using absolute ethyl alcohol, then
Fluororystal mica is positioned in plasma cleaner and cleans and dries using nitrogen.Closed respectively below substrate sample platform before reaction
With baffle plate above evaporation source.Start compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by silicon to 380 DEG C -400
℃.Heating evaporation source after underlayer temperature is stable, is heated to 340 DEG C -360 DEG C, treats that instrument is evacuated to 5*10-5Pa, opens substrate
The baffle plate of lower section, starts plated film.5-120min is reacted at this temperature, is closed evaporation source and substrate shutter, is passed through control panel
Evaporation source and underlayer temperature are adjusted to 0 DEG C, is waited after instrument Temperature fall, product is obtained.
Compared with prior art, the method have the characteristics that：Spiral is directly prepared using high vacuum thermal evaporation coating method
The bismuth telluride nanometer sheet film of structure.This experimental technique flow is simple, and controllability is good, it is easy to operation and popularization；Product morphology spiral shell
Rotation growth, step is high-visible；Without other products, environmental pollution is small, thus with important researching value and wide
Application prospect.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of gained sample in embodiment 1.
Fig. 2 is the scanning electron microscope diagram piece of gained sample in embodiment 1；
Fig. 3 is the scanning electron microscope diagram piece of gained sample in embodiment 2；
Fig. 4 is the scanning electron microscope diagram piece of gained sample in embodiment 3.
Embodiment
The present invention is described in further details below by example, these examples are only used for illustrating the present invention, do not limit
The scope of the present invention processed.
Embodiment 1
Before experiment, Fluororystal mica is placed in absolute ethyl alcohol and is cleaned by ultrasonic, then be positioned in plasma cleaner and be passed through nitrogen
Clean and dry.In crucible, 2.5mmol Bi is added2Te3High-purity powder, is positioned at instrument evaporation source heating tank.Will be clear
Washed Fluororystal mica is fixed on sample stage.Sample stage, which is positioned over above evaporation source, can fix the region of sample stage, adjust
The distance of substrate sample platform and evaporation source is saved to 10cm.Open compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by substrate
It is heated to 380 DEG C.Heating evaporation source after underlayer temperature is stable, temperature is heated to 360 DEG C, treats that instrument is evacuated to 5*10-5Pa, beats
The baffle plate below substrate is opened, starts plated film.The 10min times are reacted at this temperature, evaporation source and substrate shutter is closed, and pass through control
Panel regulation evaporation source and underlayer temperature processed wait after instrument Temperature fall to 0 DEG C, obtain product.The X-ray of products therefrom is spread out
Penetrate map analysis result and show that sample is bismuth telluride thin film, as shown in Figure 1；Scanning electron microscope diagram is shown by above-mentioned technique system
It is standby go out product be helical structure bismuth telluride nanometer sheet film, as shown in Figure 2.
Embodiment 2
Before experiment, Fluororystal mica is placed in absolute ethyl alcohol and is cleaned by ultrasonic, then be positioned in plasma cleaner and be passed through nitrogen
Clean and dry.In crucible, 2.5mmol Bi is added2Te3High-purity powder, is positioned at instrument evaporation source heating tank.Will be clear
Washed Fluororystal mica is fixed on sample stage.Sample stage, which is positioned over above evaporation source, can fix the region of sample stage, adjust
The distance of substrate sample platform and evaporation source is saved to 10cm.Open compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by substrate
It is heated to 380 DEG C.Heating evaporation source after underlayer temperature is stable, temperature is heated to 360 DEG C, treats that instrument is evacuated to 5*10-5Pa, beats
The baffle plate below substrate is opened, starts plated film.The 30min times are reacted at this temperature, evaporation source and substrate shutter is closed, and pass through control
Panel regulation evaporation source and underlayer temperature processed wait after instrument Temperature fall to 0 DEG C, obtain product.Scanning electron microscope diagram
The bismuth telluride nanometer sheet film that the product prepared by above-mentioned technique is helical structure is shown, as shown in Figure 3.
Embodiment 3
Before experiment, Fluororystal mica is placed in absolute ethyl alcohol and is cleaned by ultrasonic, then be positioned in plasma cleaner and be passed through nitrogen
Clean and dry.In crucible, 2.5mmol Bi is added2Te3High-purity powder, is positioned at instrument evaporation source heating tank.Will be clear
Washed Fluororystal mica is fixed on sample stage.Sample stage, which is positioned over above evaporation source, can fix the region of sample stage, adjust
The distance of substrate sample platform and evaporation source is saved to 10cm.Open compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by substrate
It is heated to 380 DEG C.Heating evaporation source after underlayer temperature is stable, temperature is heated to 340 DEG C, treats that instrument is evacuated to 5*10-5Pa, beats
The baffle plate below substrate is opened, starts plated film.The 10min times are reacted at this temperature, evaporation source and substrate shutter is closed, and pass through control
Panel regulation evaporation source and underlayer temperature processed wait after instrument Temperature fall to 0 DEG C, obtain product.Scanning electron microscope diagram
The bismuth telluride nanometer sheet film that the product prepared by above-mentioned technique is helical structure is shown, as shown in Figure 4.
Embodiment 4
Before experiment, Fluororystal mica is placed in absolute ethyl alcohol and is cleaned by ultrasonic, then be positioned in plasma cleaner and be passed through nitrogen
Clean and dry.In crucible, 2.5mmol Bi is added2Te3High-purity powder, is positioned at instrument evaporation source heating tank.Will be clear
Washed Fluororystal mica is fixed on sample stage.Sample stage, which is positioned over above evaporation source, can fix the region of sample stage, adjust
The distance of substrate sample platform and evaporation source is saved to 10cm.Open compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by substrate
It is heated to 380 DEG C.Temperature is heated to 360 DEG C, treats that instrument is evacuated to 5*10-5Pa, opens the baffle plate below substrate, starts plating
Film.The 60min times are reacted at this temperature, evaporation source and substrate shutter is closed, and evaporation source and substrate are adjusted by control panel
Temperature is waited after instrument Temperature fall to 0 DEG C, obtains product.
Claims (10)
1. bismuth telluride nanometer sheet film of a kind of helical structure and preparation method thereof, it is characterised in that real by following technical process
It is existing：In multi-source high vacuum thermal evaporation coating machine special copple, a certain amount of high-purity Bi is added2Te3Powder, is positioned over multi-source high
Vacuum thermal evaporation coating machine evaporation source heating region；Substrate sample platform is adjusted to the distance of evaporation source to 10cm, by sample stand lock
It is scheduled on directly over evaporation source；Fluororystal mica is placed on substrate sample platform, is cleaned by ultrasonic before placing using absolute ethyl alcohol, then will
Fluororystal mica, which is positioned in plasma cleaner, to be cleaned and is dried using nitrogen；Closed respectively before reaction below substrate sample platform with
Baffle plate above evaporation source；Open compound molecule pump assembly to vacuumize, be evacuated to 9*10-5Pa, by silicon to 380 DEG C -400 DEG C；
Heating evaporation source after underlayer temperature is stable, temperature is heated to 340 DEG C -360 DEG C, treats that instrument is evacuated to 5*10-5Pa, opens substrate
The baffle plate of lower section, starts plated film；5-120min is reacted at this temperature, is closed evaporation source and substrate shutter, is passed through control panel
Evaporation source and underlayer temperature are adjusted to 0 DEG C, is waited after instrument Temperature fall, product is obtained.
2. the method as described in claim 1, it is characterised in that bismuth telluride source used is commercially available Bi2Te3Powder.
3. the method as described in claim 1, it is characterised in that substrate used is commercially available Fluororystal mica.
4. the method as described in claim 1, it is characterised in that preparation facilities used is multi-source high vacuum thermal evaporation coating machine.
5. the method as described in claim 1, it is characterised in that the distance of the substrate to evaporation source is 10cm.
6. the method as described in claim 1, it is characterised in that the evaporation source reaction temperature is 340 DEG C -360 DEG C.
7. the method as described in claim 1, it is characterised in that the substrate reaction temperature is 380 DEG C -400 DEG C.
8. the method as described in claim 1, it is characterised in that the plated film reaction time is 10 minutes ~ 2 hours.
9. the method as described in claim 1, it is characterised in that products therefrom is thin for a kind of bismuth telluride nanometer sheet of helical structure
Film.
10. the method as described in claim 1, it is characterised in that the helical structure platform of resulting bismuth telluride nanometer sheet film
Rank is clear, without other products.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710238625.5A CN107058950A (en) | 2017-04-13 | 2017-04-13 | A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710238625.5A CN107058950A (en) | 2017-04-13 | 2017-04-13 | A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107058950A true CN107058950A (en) | 2017-08-18 |
Family
ID=59600985
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710238625.5A Pending CN107058950A (en) | 2017-04-13 | 2017-04-13 | A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107058950A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041677A (en) * | 2022-06-24 | 2022-09-13 | 湘潭大学 | Chemical vapor deposition of Bi on mica 2 O 2 Method for preparing Te nanosheet |
| CN115418716A (en) * | 2022-09-20 | 2022-12-02 | 哈尔滨工业大学 | CVD preparation method of two-dimensional bismuth telluride single crystal wafer |
| CN115579424A (en) * | 2022-10-31 | 2023-01-06 | 内蒙古工业大学 | Preparation method of flexible bismuth ferrite film |
-
2017
- 2017-04-13 CN CN201710238625.5A patent/CN107058950A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041677A (en) * | 2022-06-24 | 2022-09-13 | 湘潭大学 | Chemical vapor deposition of Bi on mica 2 O 2 Method for preparing Te nanosheet |
| CN115041677B (en) * | 2022-06-24 | 2024-02-02 | 湘潭大学 | Chemical vapor deposition on mica to generate Bi 2 O 2 Te nano-sheet method |
| CN115418716A (en) * | 2022-09-20 | 2022-12-02 | 哈尔滨工业大学 | CVD preparation method of two-dimensional bismuth telluride single crystal wafer |
| CN115418716B (en) * | 2022-09-20 | 2024-01-30 | 哈尔滨工业大学 | CVD preparation method of two-dimensional bismuth telluride single crystal wafer |
| CN115579424A (en) * | 2022-10-31 | 2023-01-06 | 内蒙古工业大学 | Preparation method of flexible bismuth ferrite film |
| CN115579424B (en) * | 2022-10-31 | 2024-01-26 | 内蒙古工业大学 | Preparation method of flexible bismuth ferrite film |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Luo et al. | Chemical vapor deposition of perovskites for photovoltaic application | |
| Shaili et al. | Synthesis of the Sn-based CaSnS3 chalcogenide perovskite thin film as a highly stable photoabsorber for optoelectronic applications | |
| CN107058950A (en) | A kind of bismuth telluride nanometer sheet film of helical structure and preparation method thereof | |
| CN105568253B (en) | A kind of method of apparatus for plasma chemical vapor deposition growth hexagonal boron nitride | |
| Olgar et al. | Impact of sulfurization parameters on properties of CZTS thin films grown using quaternary target | |
| CN103555986B (en) | Method for preparing (Bi0.8Sb0.2)2Te3 nano thermoelectric material | |
| Rabaoui et al. | Structural, optical and electrical properties of Cu 2 SnS 3 nanoparticles synthesized by simple solvothermal technique | |
| CN103787284A (en) | Method for preparing bismuth telluride nanosheet | |
| CN102925866A (en) | Preparation technology for single-phase Mg2Si semiconductor film | |
| CN106185897B (en) | A method of the controllable preparation graphene nanobelt in a variety of substrates | |
| KR20130017589A (en) | Method for synthesizing a bixsb2-xte3 thermoelectric nanocompound and the thermoelectric nanocompound thereof | |
| CN101823702A (en) | Preparation method of Cu2CdSnSe4 nano crystals | |
| CN110344025A (en) | A kind of two dimension Zn doping Ca2Si nano thin-film and its chemical vapor deposition method | |
| CN107699856B (en) | Using evaporation coating-electric field induction controllable preparation orientation Bi-Te-Se nano column array method | |
| Ullah et al. | Growth and characterization of Ag–Al2O3 composites thin films for thermoelectric power generation applications | |
| Zuo et al. | CuAgSe nanocrystals: colloidal synthesis, characterization and their thermoelectric performance | |
| CN101434455B (en) | Method for preparing bismuth telluride nano-wire array by physical vapour deposition | |
| CN113104885B (en) | Non-lamellar Sn 2 P 2 S 6 Preparation method of nanosheet and application of nanosheet in field of photocatalytic hydrogen evolution | |
| Liu et al. | The influence of substrate temperature on spray-deposited CuSbS2 thin films | |
| CN108842142B (en) | Film composed of micron-sized pentagonal stannous oxide and preparation method thereof | |
| CN112481593A (en) | Method for preparing antimony trisulfide copper film on solar cell absorption layer through gas-solid reaction | |
| Harris et al. | Using single source precursors and spray chemical vapor deposition to grow thin-film CuInS/sub 2/[solar cells] | |
| CN108103439A (en) | Utilize the method for vacuum vapor plating controllable preparation structure gradient oriented growth Sb-Bi-Te films | |
| CN113122809B (en) | Method for controllably preparing amorphous flexible Bi-Te-Se film by adopting vacuum evaporation coating | |
| CN100549221C (en) | A kind of preparation method of barium strontium titanate film material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170818 |
|
| WD01 | Invention patent application deemed withdrawn after publication |