CN101602496B - Synchronic preparation method of lead telluride thin film and nano powder - Google Patents
Synchronic preparation method of lead telluride thin film and nano powder Download PDFInfo
- Publication number
- CN101602496B CN101602496B CN200910054457XA CN200910054457A CN101602496B CN 101602496 B CN101602496 B CN 101602496B CN 200910054457X A CN200910054457X A CN 200910054457XA CN 200910054457 A CN200910054457 A CN 200910054457A CN 101602496 B CN101602496 B CN 101602496B
- Authority
- CN
- China
- Prior art keywords
- thin film
- nano
- powder
- lead telluride
- film
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the lead telluride (PbTe) thin film and nano powder preparation method field. In a low temperature aqueous solution synchronic synthesis method of PbTe thin film and nano powder, inorganic salt containing lead and tellurium dioxide or sodium tellurite are taken as raw materials, potassium borohydride or sodium borohydride is taken as reducing agent, and PbTe thin film and nano powder are simultaneously synthesized in alkaline aqueous solution at room temperature to 50 DEG C. The invention initially synthesizes PbTe thin film and nano powder at normal atmosphere and below 100 DEG C, the prepared thin film is flat, compact and uniform; and powder product is small in grain diameter uniform in grain fineness distribution, and grain diameter size can be controlled by controlling reaction temperature. The raw materials used in the whole technology are available, the technology is simple, scale production is easy to realize, and organic solvent is not used in the reaction process, thus being beneficial to environmental protection. The synthesized PbTe thin film and nano powder can be widely applied to thermoelectric device, solar battery, fluorescence device, infrared optical element, infrared thin film device, semiconductor detector and the like and has a wide application prospect.
Description
Technical field
The invention belongs to the material field, relate to the synchronic preparation method of a kind of lead telluride thin film and nano-powder.
Background technology
Lead telluride (PbTe) has very good pyroelecthc properties, photoelectric characteristic and infrared optics characteristic, is widely used in thermo-electric device, infrared optical element, infrared thin-film device and semiconductor detector etc.Aspect film, the PbTe material is an ionic linkage compound unique in the IV-VI family low-gap semiconductor, in the specific refractory power of infrared spectral coverage up to 5.5, at present can be the highest in the actual infrared Coating Materials that uses, can effectively reduce the rete number of infrared optical thin film device, reduce stress, improve transmissivity.Simultaneously, PbTe has good stress to cooperate with low-index material retes such as ZnS, ZnSe, can make the firmness of rete good, and optical property is stable.The PbTe film adopts physical method preparations such as vacuum evaporation, laser flash distillation, magnetron sputtering usually, and these methods adopt expensive filming equipment, and cost is higher; Electrochemical method deposition PbTe film cost is relatively low, but shortcoming is the necessary conductive substrate that uses, and the scope of application is narrower.
In addition, after the material grains size reaches nanoscale, can produce quantum size effect, cause the material property sudden change, therefore, the nanostructure of PbTe is subjected to paying attention to widely.At present; the PbTe nano particle adopts methods such as hydrothermal method or solvent-thermal method, electrochemical process, emulsion method synthetic mostly; these methods are in building-up process or related to high-tension apparatus; perhaps adopted complicated instrument and related to tediously long technology, perhaps brought a difficult problem to aftertreatment and environment protection owing to introduce large amount of organic.In a word, these method conditions are harsh relatively, and perhaps output is few, and the cost height is unfavorable for suitability for industrialized production.
Summary of the invention
At the deficiencies in the prior art, the problem to be solved in the present invention provides a kind of environmental protection, simple and feasible method, synthetic synchronously lead telluride thin film and nano-powder.This method with alkaline aqueous solution as solvent, with leaded inorganic salt with low cost and telluride or tellurite as reactant, at normal pressure, room temperature to 50 ℃ synchronously synthetic PbTe film and nano particle.
The present invention relates to the preparation method of a kind of lead telluride nano-powder and film, this method is made up of batching, isothermal reaction, washing and dry four steps, it is characterized in that, described batching is meant plumbiferous inorganics and the compound that contains tellurium according to atomic ratio Pb: Te=1: 1 ratio adds and fills in the beaker of deionized water, add appropriate bases and complexing agent again, stirring is fully dissolved it, add right amount of boron potassium hydride KH or sodium borohydride then, fully stop after the dissolving stirring, put into substrate (tilt and become 20-70 ° of angle at the bottom of the beaker) and be used for deposit film; Described isothermal reaction is the water bath with thermostatic control of reaction system being put into room temperature to 50 ℃, and insulation is more than 12 hours; Described washing is meant after reaction reaches setting-up time with deionized water and dehydrated alcohol flushing film, and the product repetitive scrubbing that will be deposited in beaker bottom is 7 up to pH; Described drying is meant the film natural air drying is dried the gained powder under vacuum environment.
Wherein, plumbiferous inorganic salt are one of muriate, nitrate, acetate preferably, and the compound that contains tellurium is tellurium dioxide or sodium tellurite preferably.
Among the preparation method of above-mentioned PbTe film and nano-powder, added alkali is one of sodium hydroxide, potassium hydroxide, rubidium hydroxide.
Used complexing agent is preferably Trisodium Citrate, sodium oxalate, nitrilotriacetic acid, ethylenediamine tetraacetic acid (EDTA) etc. among the preparation method of PbTe film and nano-powder.
Film can deposit on multiple substrate, as: glass, aluminum oxide, metal, silicon chip and polymkeric substance etc.
Among the preparation method of above-mentioned PbTe film and nano-powder, heat-preserving equipment is the water-bath or the oil bath pan of energy temperature control.
Among the preparation method of above-mentioned PbTe film and nano-powder, the washing film is with deionized water and dehydrated alcohol flushing; The washing nano-powder is with cold or hot deionized water, adopts whizzer precipitation or pumping and filtering device to filter, and filtration product is disperseed in deionized water again, and filtering up to filtrate pH value repeatedly is 7, uses absolute ethanol washing with convenient and dry at last.The centrifugal settling rotating speed is 2000-4000 rev/min.
Among the preparation method of above-mentioned PbTe film and nano-powder, film adopts natural air drying, and the oven dry of powder is to carry out in vacuum drying oven, vacuum tightness＜133Pa, and temperature is 70 ℃, 12 hours time.
Raw material of the present invention cheaply is easy to get, and technology is simple, not with an organic solvent, helps environmental protection in the reaction process, accomplishes scale production easily.Products therefrom can be widely used in thermo-electric device, solar cell, fluorescent device, infrared optical element, infrared thin-film device and semiconductor detector etc.
Description of drawings
Fig. 1 for the X-ray diffracting spectrum that adopts synthetic lead telluride nano particle (a) of room temperature of the present invention and film (b) and (c) the PbTe standard diagram (JCPDS card file, No.077-0246).
Fig. 2 is for adopting the transmission electron microscope picture of the synthetic lead telluride nano particle of room temperature of the present invention.
Fig. 3 a is for adopting the field emission scanning electron microscope picture (low power) of the synthetic lead telluride thin film of room temperature of the present invention.
Fig. 3 b is for adopting the field emission scanning electron microscope picture (high power) of the synthetic lead telluride thin film of room temperature of the present invention.
Fig. 3 c is for adopting the field emission scanning electron microscope picture (side) of the synthetic lead telluride thin film of room temperature of the present invention.
Specific embodiment
Example 1
Synthetic synchronously lead telluride thin film of room temperature and nano particle
1 batching
(1) in beaker, adds the 100ml deionized water, put into and stir the magneton stirring.
(2) taking by weighing 0.379g lead acetate trihydrate and 0.159g tellurium dioxide adds in the beaker.
(3) take by weighing 1.4g KOH and add in the beaker, continue stirring and become transparent clarification up to solution.
(4) taking by weighing the 0.294g Trisodium Citrate adds in the beaker.
(5) take by weighing 0.5g KBH
4Slowly add in the beaker, continue in the adition process to stir.
(6) treat that institute adds whole KBH
4After the dissolving, take out and stir magneton, add deionized water to 200ml.
(7) put into glass substrate, tilt and become 30 ° of angles at the bottom of the beaker.
2 isothermal reactions
Seal the beaker mouth with preservative film and prevent that dust from entering, left standstill under the room temperature 12 hours.
3 washings
The gained film is washed with deionized water and dehydrated alcohol.
To adopt centrifugation behind the gained throw out deionized water wash, centrifugal sediment disperses in deionized water again, and it is 7 that recentrifuge separates up to filtrate pH value, uses absolute ethanol washing at last.The centrifugal settling rotating speed is 3000 rev/mins.
4 dryings:
With the film natural air drying after the washing.
The powder that filtration is obtained is placed on drying in 70 ℃ of vacuum drying ovens, obtains the lead telluride nano-powder.
X-ray diffraction result (Fig. 1) shows that experiment gained film and powdered product are a cube lead telluride, and transmission electron microscope observation (Fig. 2) shows that powder is the nano particle about particle diameter 20nm.Field emission scanning electron microscope is observed (Fig. 3) and is shown preparation film densification, even, the about 1 μ m of thickness.
Example 2
Lead telluride thin film and nano particle are synthesized in 50 ℃ of water-baths synchronously
1 batching
(1) in beaker, adds the 100ml deionized water, put into and stir the magneton stirring.
(2) taking by weighing 0.379g lead acetate trihydrate and 0.159g tellurium dioxide adds in the beaker.
(3) take by weighing 1.4g KOH and add in the beaker, continue stirring and become transparent clarification up to solution.
(4) taking by weighing the 0.292g ethylenediamine tetraacetic acid (EDTA) adds in the beaker.
(5) take by weighing 0.5g KBH
4Slowly add in the beaker, continue in the adition process to stir.
(6) treat that institute adds whole KBH
4After the dissolving, take out and stir magneton, add deionized water to 200ml.
(7) put into glass substrate, tilt and become 30 ° of angles at the bottom of the beaker.
2 isothermal reactions
Seal the beaker mouth with preservative film and prevent that dust from entering, put into 50 ℃ of waters bath with thermostatic control and left standstill 12 hours.
3 washings
The gained film is washed with deionized water and dehydrated alcohol.
To adopt centrifugation behind the gained throw out deionized water wash, centrifugal sediment disperses in deionized water again, and it is 7 that recentrifuge separates up to filtrate pH value, uses absolute ethanol washing at last.The centrifugal settling rotating speed is 3000 rev/mins.
4 dryings:
With the film natural air drying after the washing.
The powder that filtration is obtained is placed on drying in 70 ℃ of vacuum drying ovens, obtains the lead telluride nano-powder.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (8)
1. the synchronic preparation method of lead telluride thin film and nano-powder, comprise: batching, isothermal reaction, washing and dry four steps, it is characterized in that: described batching be with plumbiferous inorganics and the compound that contains tellurium according to atomic ratio Pb: Te=1: 1 ratio adds and fills in the beaker of solvent, add alkali and complexing agent again, stirring is fully dissolved it, add excessive slightly POTASSIUM BOROHYDRIDE or sodium borohydride then, fully stop after the dissolving stirring, put into substrate and be used for deposit film;
Described isothermal reaction is the water bath with thermostatic control of reaction system being put into room temperature to 50 ℃, and insulation is more than 12 hours;
Described washing is meant after reaction reaches setting-up time with solvent and dehydrated alcohol flushing film, and the product repetitive scrubbing that will be deposited in beaker bottom is 7 up to pH;
Described drying is meant the film natural air drying is dried the gained powder under vacuum environment;
Described alkali concn is 0.1～0.5mol/L, and the consumption of described complexing agent is 1～1.5 times of Pb atomic molar number, and the adding of described POTASSIUM BOROHYDRIDE or sodium borohydride makes BH
4 -: Pb
2+=6～8.
2. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1, it is characterized in that: described plumbiferous inorganic salt are one of muriate, nitrate, acetate, the compound that contains tellurium is tellurium dioxide or tellurite.
3. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1, it is characterized in that: described solvent is a deionized water; Described alkali is one of sodium hydroxide, potassium hydroxide, rubidium hydroxide; Described complexing agent is one of Trisodium Citrate, sodium oxalate, nitrilotriacetic acid, ethylenediamine tetraacetic acid (EDTA).
4. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1 is characterized in that: heat-preserving equipment is water-bath or oil bath pan that can temperature control, synthetic film and nano-powder under room temperature to 50 ℃ condition.
5. the preparation method of lead telluride thin film and nano-powder according to claim 1 is characterized in that: described substrate size and used beaker coupling, tilt to put into beaker, and and become 20-70 ° of angle at the bottom of the beaker.
6. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1 is characterized in that: with the film that makes with deionized water and dehydrated alcohol flushing, natural air drying.
7. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1, it is characterized in that: for nano-powder, described washing is with cold or hot deionized water, adopt whizzer precipitation or pumping and filtering device to filter, filtration product is disperseed in deionized water again, filtering up to filtrate pH value repeatedly is 7, uses absolute ethanol washing with convenient and dry at last.
8. the synchronic preparation method of lead telluride thin film and nano-powder according to claim 1, it is characterized in that: for nano-powder, dry in vacuum drying oven, the vacuum-drying condition is vacuum tightness＜133Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910054457XA CN101602496B (en) | 2009-07-07 | 2009-07-07 | Synchronic preparation method of lead telluride thin film and nano powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910054457XA CN101602496B (en) | 2009-07-07 | 2009-07-07 | Synchronic preparation method of lead telluride thin film and nano powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101602496A CN101602496A (en) | 2009-12-16 |
| CN101602496B true CN101602496B (en) | 2011-05-25 |
Family
ID=41468414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910054457XA Expired - Fee Related CN101602496B (en) | 2009-07-07 | 2009-07-07 | Synchronic preparation method of lead telluride thin film and nano powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101602496B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830446B (en) * | 2010-04-30 | 2011-07-27 | 西安交通大学 | Preparation method of PbTe colloid nanocrystalline self-assembly film |
| CN106634985A (en) * | 2016-09-22 | 2017-05-10 | 上海洞舟实业有限公司 | Preparation for novel down-conversion infrared emission material |
| CN109592652A (en) * | 2018-12-03 | 2019-04-09 | 山东建筑大学 | A kind of method that chemical liquid phase reaction prepares lead telluride thin film |
| CN109592651A (en) * | 2018-12-03 | 2019-04-09 | 山东建筑大学 | A kind of lead telluride thin film |
| CN113755174B (en) * | 2021-09-26 | 2023-10-20 | 杭州师范大学 | Lead telluride quantum dot and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
| CN1915803A (en) * | 2006-09-08 | 2007-02-21 | 华中科技大学 | Method for preparing polycrystalline Nano film of zinc selenide |
| CN101225548A (en) * | 2007-10-23 | 2008-07-23 | 南京航空航天大学 | Method for preparing lead telluride nano-wire |
-
2009
- 2009-07-07 CN CN200910054457XA patent/CN101602496B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1384048A (en) * | 2002-06-21 | 2002-12-11 | 清华大学 | Nano level metal telluride preparing process |
| CN1915803A (en) * | 2006-09-08 | 2007-02-21 | 华中科技大学 | Method for preparing polycrystalline Nano film of zinc selenide |
| CN101225548A (en) * | 2007-10-23 | 2008-07-23 | 南京航空航天大学 | Method for preparing lead telluride nano-wire |
Non-Patent Citations (2)
| Title |
|---|
| JP特开2008-81393A 2008.04.10 |
| T.J.Zhu et al..Synthesis of PbTe thermoelectric materials by alkaline reducing chemical routes.《Materials Research Bulletin》.2008,第43卷第2850-2854页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101602496A (en) | 2009-12-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101602496B (en) | Synchronic preparation method of lead telluride thin film and nano powder | |
| Hossain et al. | Understanding the shrinkage of optical absorption edges of nanostructured Cd-Zn sulphide films for photothermal applications | |
| CN101765649A (en) | nanoparticles | |
| EP2475618B1 (en) | Solid material in divided state, method for manufacturing such a material and use of such a material in a photovoltaic cell | |
| Zhang et al. | A simple method for systematically controlling ZnO crystal size and growth orientation | |
| CN101214932A (en) | Method for preparing nanometer tin selenide | |
| CN101214990B (en) | Normal temperature synthesis method for nanometer zinc oxide | |
| CN100545081C (en) | Dendritic silver selenide nano crystal thin film material and preparation method | |
| Seo et al. | Effect of sulfur and copper amounts in sol–gel precursor solution on the growth, crystal properties, and optical properties of Cu 2 ZnSnS 4 films | |
| CN103774232A (en) | Preparation method of Ag2E nano wire | |
| CN101792116B (en) | Method for preparing carboxylic acid-chemically modified metal oxide nanoparticles | |
| CN103496744A (en) | Preparation method of as-reduced ammonium tungsten bronze nanoparticles | |
| CN104651939A (en) | Method for preparing antimony sulphoioide single crystal and similar compound single crystal | |
| Arsad et al. | Effect of chemical bath deposition variables on the properties of zinc sulfide thin films: a review | |
| CN100534907C (en) | Zinc oxide synthesizing process | |
| CN100515953C (en) | Method for preparing zinc oxide thin film | |
| Pîslaru-Dănescu et al. | Synthesis and characterization of antireflective ZnO nanoparticles coatings used for energy improving efficiency of silicone solar cells | |
| JP6143047B2 (en) | Wavelength conversion device and manufacturing method thereof | |
| CN102910616A (en) | One-step method for preparing graphene/lead telluride nano composite by means of coreduction | |
| CN109850932B (en) | Monodisperse Cu with adjustable particle size2O single crystal solid sphere and preparation method thereof | |
| CN102765744B (en) | One-step preparation method of zinc oxide quantum dots | |
| Martins et al. | Thin film of ZnAl2O4: Eu3+ synthesized by a non-alkoxide precursor sol-gel method | |
| CN102585588B (en) | Preparation method of copper-zinc-tin-sulfur ink | |
| Salavati‐Niasari et al. | Synthesis of bismuth sulfide nanostructures by using bismuth (III) monosalicylate precursor and fabrication of bismuth sulfide based p–n junction solar cells | |
| CN102659084A (en) | Preparation method of zinc selenide nanometer powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110525 Termination date: 20140707 |
|
| EXPY | Termination of patent right or utility model |