CN106006571B - Preparation method of hexagonal-structure ternary BiTe nanosheet - Google Patents
Preparation method of hexagonal-structure ternary BiTe nanosheet Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000002135 nanosheet Substances 0.000 title abstract 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000126 substance Substances 0.000 claims abstract description 13
- 229910004273 TeO3 Inorganic materials 0.000 claims abstract description 11
- SWAKCLHCWHYEOW-UHFFFAOYSA-N chloro selenohypochlorite Chemical compound Cl[Se]Cl SWAKCLHCWHYEOW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 27
- 239000000047 product Substances 0.000 abstract description 5
- 239000012467 final product Substances 0.000 abstract description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000011669 selenium Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A method for preparing hexagonal ternary BiTe nano-sheet includes preparing Bi (NO) by said method3)3、K2TeO3、SeCl2·5H2And O is mixed according to the chemical molar ratio of 2 (3-x) x, added into diethylene glycol to obtain reaction liquid, added with a pH value regulator and a surfactant, kept at the temperature of 245-265 ℃ in a closed state for 3-6 hours, naturally cooled, washed for multiple times by using an organic solvent, and dried to obtain a final product. The product obtained by the method has good platelet morphology, low cost and simple and convenient process.
Description
Technical field
The invention belongs to nano materials to synthesize field, and in particular to a kind of ternary BiTe systems nanometer sheet of hexgonal structure
Preparation method, suitable for reducing cost, simplifying technique.
Background technology
Thermoelectric material is the advanced material that a kind of movement by carrier statically realizes that thermal energy is mutually converted with electric energy.
It is also more and more with the relevant research of thermoelectric material with the raising of people's environmental protection and awareness of saving energy.Bi2Te3Compound is current
It is especially the best thermoelectric material of performance at 200 DEG C to room temperature section using most ripe one of commercialization thermoelectric material, but its
Maximum ZT values are hovered 1 or so always, if the commercial application prospect to have reached, are connected with traditional compressor refrigerating efficiency
Closely, ZT values need to be increased to 2 or so.Research in recent years finds to include mainly following two evolutionary approach：1）Material structure
Nanosizing such as nanometer sheet, nano dot, nano wire, nanocrystalline etc. have the potentiality for greatly improving ZT values；2）Ternary doping type BiTe systems
Material is significantly improved compared to binary pure phase ZT values.Nanostructure ternary BiTe pyroelectric materials combine above two improvement
The advantage of scheme, therefore, how to synthesize the nanostructure ternary BiTe pyroelectric materials of high quality becomes research emphasis.
Synthetic method about ternary BiTe pyroelectric materials, it has been disclosed that common methods be two step method：The first step passes through
Frit reaction legal system obtains binary pure phase Bi2Te3, second step is by third element pure phase simple substance Se by formula design molar ratio addition two
First pure phase Bi2Te3In, Bi is obtained by frit reaction2Te3-xSexTernary material.This method equipment complexity, expensive starting materials, technique
Link is more, energy consumption is big, and the ternary material structure being prepared belongs to micron order, exists compared with nanostructure in ZT values
Larger gap also needs to carry out the subsequent techniques such as ball milling if you need to obtain nano structural material.Other method is such as vapor-deposited
Method, molecular beam epitaxy, magnetron sputtering method, although the ternary material being prepared also belongs to nanometer materials, it is common scarce
Point is that of high cost, period is long.Therefore, it develops the synthetic method that at low cost, low energy consumption, the period is short, simple for process and has become material
Expect one of scientific research hot spot.
Chinese patent：Application publication number is CN105200520A, and data of publication of application is that the invention on December 30th, 2015 is special
Profit, which discloses, a kind of preparing Bi2(SexTe1-x)3The method of single crystal nanoplate, this method are that tellurium powder is added in autoclave
End, selenium powder and organic solvent, bismuth chloride is added after 15~35 minutes in stirring, after continuing stirring 15~35 minutes that reaction kettle is close
Envelope is kept for 12~48 hours at a temperature of being placed in 180~200 DEG C, solvent thermal reaction is carried out, by reaction product deionized water, nothing
Water-ethanol cleans 1~3 time, is dried in vacuo and collects, obtains final product Bi2(SexTe1-x)3Single crystal nanoplate.Although the invention
Bi is realized by one-step method2(SexTe1-x)3The preparation of single crystal nanoplate, but still have the following defects：
1, using telloy, selenium powder and bismuth chloride as predecessor, the use of tellurium, selenium pure phase simple substance will necessarily make this method
It is higher to obtain cost；
2, in the invention, entire reaction need to carry out in autoclave, that is, need to use hyperbaric environment, therefore anti-to its
Answer condition more harsh.
Invention content
The purpose of the present invention is overcoming the problems, such as of high cost, severe reaction conditions of the existing technology, provide it is a kind of at
The preparation method of the ternary BiTe systems nanometer sheet of this low and simple process hexgonal structure.
In order to achieve the above object, technical scheme is as follows：
A kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure, includes the following steps successively：
Step 1: first by Bi (NO3)3、K2TeO3、SeCl2·5H2O presses chemical molar ratio 2:(3-x):X is mixed to be mixed
Material is closed, then adds mixture into and obtains reaction solution in diglycol, wherein the x is more than 0 and is less than 0.5, the mixture
A concentration of 0.3~0.5mol/L in diglycol；
Step 2: pH adjusting agent and surfactant are first added into reaction solution, it is 10~12 to make the pH value of reaction solution,
It is kept the temperature to natural cooling after 3~6h at air-tight state, 245~265 DEG C again；
Step 3: first collecting black powder reaction product, then organic solvent is used to carry out repeatedly washing to remove to it
Then the reaction raw materials of its remained on surface dry the black powder reaction product after washing.
The pH adjusting agent is sodium hydroxide；
The surfactant is polyvinylpyrrolidone, and the mass volume ratio with reaction solution is 1g/L.
In the step 3, carrying out repeatedly washing to it using organic solvent refers to：Acetone, isopropyl acetone successively is respectively adopted
Washing is to supernatant liquid in colourless.
In the step 2, control mixing speed is 400~600r/min when heat preservation；
In the step 3, drying temperature is 70~90 DEG C, and drying time is 4~6h.
Compared with prior art, beneficial effects of the present invention are：
1, a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure of the present invention is with Bi (NO3)3、K2TeO3、
SeCl2·5H2O prepares width and the adjustable high pure phase Bi of thickness using diglycol as solvent as predecessor2Te3- xSex, it is width in 0.6~1.2 micron, hexagonal nano piece of the thickness at 30~80 nanometers to test it through SEM, XRD characterization, one
Aspect, this method use Bi salt, Te salt and Se salt for raw material, compared with its pure phase simple substance, significantly reduce cost, another party
Face, using product made from this method, not only purity is high, but also piece thickness is small, the wide uniformity of piece is good.Therefore, the present invention not only cost
It is low, and purity is high, piece thickness is small, platelet pattern is good.
2, in a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure of the present invention each raw material air-tight state,
3~6h is kept the temperature at 245~265 DEG C, reaction can be completed, be not only not necessarily to hyperbaric environment, simple process, and the reaction time is short, energy
It consumes low.Therefore, present invention process is easy, low energy consumption.
Description of the drawings
Fig. 1 is the SEM phenograms of product of the present invention.
Fig. 2 is the XRD characterization result of product of the present invention under different Se content ratios.
Specific implementation mode
The present invention is described in further detail with specific implementation mode for explanation below in conjunction with the accompanying drawings.
A kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure, includes the following steps successively：
Step 1: first by Bi (NO3)3、K2TeO3、SeCl2·5H2O presses chemical molar ratio 2:(3-x):X is mixed to be mixed
Material is closed, then adds mixture into and obtains reaction solution in diglycol, wherein the x is more than 0 and is less than 0.5, the mixture
A concentration of 0.3~0.5mol/L in diglycol；
Step 2: pH adjusting agent and surfactant are first added into reaction solution, it is 10~12 to make the pH value of reaction solution,
It is kept the temperature to natural cooling after 3~6h at air-tight state, 245~265 DEG C again；
Step 3: first collecting black powder reaction product, then organic solvent is used to carry out repeatedly washing to remove to it
Then the reaction raw materials of its remained on surface dry the black powder reaction product after washing.
The pH adjusting agent is sodium hydroxide；
The surfactant is polyvinylpyrrolidone, and the mass volume ratio with reaction solution is 1g/L.
In the step 3, carrying out repeatedly washing to it using organic solvent refers to：Acetone, isopropyl acetone successively is respectively adopted
Washing is to supernatant liquid in colourless.
In the step 2, control mixing speed is 400~600r/min when heat preservation；
In the step 3, drying temperature is 70~90 DEG C, and drying time is 4~6h.
The principle of the present invention is described as follows：
The present invention provides a kind of ternary Bi that hexagonal nano chip architecture being prepared by one-step method2Te3-xSexThermoelectricity
The method of material, with simple process, at low cost, reaction temperature is low, synthesis cycle is short, product purity is high, and shape, size
The advantages that controllable.Each step is described as follows：
Step 1：
In the step, diglycol is not only used as organic solvent, but also the reducing agent as reaction.
Step 2：
The step is controlled the pH value of reaction solution 10~12 using pH adjusting agent, can play reaction speed, control
The effect of crystal growth processed.
For reaction temperature, if temperature is excessively high, nanometer sheet material president thickens greatly, degradation；Temperature is too low, can lead
It causes reaction insufficient, influences reaction efficiency, therefore, which controls reaction temperature at 245~265 DEG C.
In addition, the present invention can control the width of nanometer sheet by the dosage of adjusting sodium hydroxide and polyvinylpyrrolidone
Degree and thickness.
Embodiment 1：
A kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure, includes the following steps successively：
Step 1: first by Bi (NO3)3、K2TeO3、SeCl2·5H2O presses chemical molar ratio 2:2.7:0.3 mixing is to be mixed
Material is closed, then adds mixture into and obtains reaction solution in diglycol, wherein the mixture is in diglycol
A concentration of 0.3mol/L；
Step 2: sodium hydroxide and polyvinylpyrrolidone are first added into reaction solution, it is 11 to make the pH value of reaction solution, then
It is kept the temperature at air-tight state, 255 DEG C to natural cooling after 5h, wherein the quality volume of polyvinylpyrrolidone and reaction solution
Than for 1g/L, control mixing speed is 600r/min when heat preservation；
Step 3: first pass through centrifugal process collect black powder reaction product, then acetone is successively respectively adopted, isopropyl acetone is washed
It is in colourless to wash to supernatant liquid, to remove the reaction raw materials of its remained on surface, then by the black powder reaction product after washing
In 80 DEG C, dry 5h.
Embodiment 2：
Step with embodiment 1, the difference is that：
In the step 1, Bi (NO3)3、K2TeO3、SeCl2·5H2The chemical molar ratio of O is 2:2.75:0.25, mixing
Expect a concentration of 0.5mol/L in diglycol；
In the step 2, reaction temperature is 245 DEG C, soaking time 6h, and control mixing speed is 400r/ when heat preservation
min；
In the step 3, drying temperature is 90 DEG C, drying time 4h.
Embodiment 3：
Step with embodiment 1, the difference is that：
In the step 1, Bi (NO3)3、K2TeO3、SeCl2·5H2The chemical molar ratio of O is 2:2.85:0.15, mixing
Expect a concentration of 0.4mol/L in diglycol；
In the step 2, the pH value of reaction solution is 12, and reaction temperature is 265 DEG C, soaking time 3h, and when heat preservation controls
Mixing speed is 500r/min；
In the step 3, drying temperature is 70 DEG C, drying time 6h.
Embodiment 4：
Step with embodiment 1, the difference is that：
In the step 1, Bi (NO3)3、K2TeO3、SeCl2·5H2The chemical molar ratio of O is 2:2.9:0.1, mixture
A concentration of 0.4mol/L in diglycol；
In the step 2, the pH value of reaction solution is 10, and control mixing speed is 400r/min when heat preservation；
In the step 3, drying temperature is 70 DEG C, drying time 6h.
Embodiment 5：
Step with embodiment 1, the difference is that：
In the step 1, Bi (NO3)3、K2TeO3、SeCl2·5H2The chemical molar ratio of O is 2:2.65:0.35.
Embodiment 6：
Step with embodiment 1, the difference is that：
In the step 1, Bi (NO3)3、K2TeO3、SeCl2·5H2The chemical molar ratio of O is 2:2.8:0.2.
The ZT values of reaction product made from above-described embodiment are used to carry out SEM, XRD characterization to it for 1.0~1.2（Referring to
Fig. 1, Fig. 2）, the results showed that：The reaction product is the high pure phase nanometer sheet of hexgonal structure（Piece thickness is at 30~80 nanometers）.
Claims (4)
1. a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure, it is characterised in that：
The preparation method includes the following steps successively：
Step 1: first by Bi (NO3)3、K2TeO3、SeCl2·5H2O presses chemical molar ratio 2:(3-x):X is mixed to be mixed
Material, then add mixture into and obtain reaction solution in diglycol, wherein the x is more than 0 and is less than 0.5, and the mixture exists
A concentration of 0.3~0.5mol/L in diglycol；
Step 2: pH adjusting agent and surfactant are first added into reaction solution, it is 10~12 to make the pH value of reaction solution, then will
It keeps the temperature natural cooling after 3~6h at air-tight state, 245~265 DEG C；
Step 3: first collecting black powder reaction product, then organic solvent is used to carry out repeatedly washing to remove its table to it
Then the remaining reaction raw materials in face dry the black powder reaction product after washing.
2. a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure according to claim 1, feature exist
In：
The pH adjusting agent is sodium hydroxide；
The surfactant is polyvinylpyrrolidone, and the mass volume ratio with reaction solution is 1g/L.
3. a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure according to claim 1 or 2, feature
It is：
In the step 3, carrying out repeatedly washing to it using organic solvent refers to：Acetone, isopropyl acetone washing is successively respectively adopted
To supernatant liquid in colourless.
4. a kind of preparation method of the ternary BiTe systems nanometer sheet of hexgonal structure according to claim 1 or 2, feature
It is：
In the step 2, control mixing speed is 400~600r/min when heat preservation；
In the step 3, drying temperature is 70~90 DEG C, and drying time is 4~6h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526638A (en) * | 2003-09-25 | 2004-09-08 | 浙江大学 | Prepn of Bi2Te3-base nano thermoelectric material powder containing RE element |
| CN103910341A (en) * | 2014-03-21 | 2014-07-09 | 东风商用车有限公司 | Method for manufacturing nano-scale hexagonal flaky bismuth telluride thermoelectric material |
| CN105200520A (en) * | 2015-10-09 | 2015-12-30 | 广东工业大学 | Method for preparing Bi2(SexTe[1-x])3 monocrystal nanosheets |
-
2016
- 2016-07-01 CN CN201610502360.0A patent/CN106006571B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526638A (en) * | 2003-09-25 | 2004-09-08 | 浙江大学 | Prepn of Bi2Te3-base nano thermoelectric material powder containing RE element |
| CN103910341A (en) * | 2014-03-21 | 2014-07-09 | 东风商用车有限公司 | Method for manufacturing nano-scale hexagonal flaky bismuth telluride thermoelectric material |
| CN105200520A (en) * | 2015-10-09 | 2015-12-30 | 广东工业大学 | Method for preparing Bi2(SexTe[1-x])3 monocrystal nanosheets |
Non-Patent Citations (2)
| Title |
|---|
| 多尺度Bi2Te3系热电材料的制备及性能优化研究;肖承京;《中国博士学位论文全文数据库工程科技1辑》;20101115(第11期);B020-33 * |
| 微波湿化学法制备Bi-,2-Te-,3-系化合物固溶体热电材料;黄建新;《中国优秀硕士学位论文全文数据库 工程科技1辑》;20111215(第82期);B020-189 * |
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