CN102795605A - Method for preparing nanometer material lead selenide by aqueous phase method - Google Patents
Method for preparing nanometer material lead selenide by aqueous phase method Download PDFInfo
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- CN102795605A CN102795605A CN201210276273XA CN201210276273A CN102795605A CN 102795605 A CN102795605 A CN 102795605A CN 201210276273X A CN201210276273X A CN 201210276273XA CN 201210276273 A CN201210276273 A CN 201210276273A CN 102795605 A CN102795605 A CN 102795605A
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Abstract
The invention provides a method for preparing nanometer material lead selenide by an aqueous phase method. The method is technically characterized by comprising the following steps of: adding selenide powder, sodium borohydride and distilled water in a container; carrying out ice-bath reaction under the argon shield, thereby obtaining a selenide precursor solution; then adding lead acetate, mercapto propionic acid and distilled water into another container, adjusting the pH value of a system to 6.0-10.0 by utilizing a sodium hydroxide solution; introducing argon into the solution system; adding the selenide precursor solution under the argon protection; and heating to 80 DEG C-120 DEG C, refluxing for 0-2.0 hours, then stopping the reaction, naturally cooling to room temperature, washing with acetone, centrifuging and vacuum-drying to prepare the back powdery PbSe nanometer crystal material. The preparation technology of the method is simple in flow, does not require severe conditions of high temperature and high pressure, and moreover, is suitable for continuous production; and compared with the prior other technologies, the method for preparing nanometer material lead selenide by the aqueous phase method provided by the invention is more environment-friendly, does not generate excessive pollution, and also can control the form of the product through controlling the technology process.
Description
Technical field
The present invention relates to a kind of method of utilizing the water legal system to be equipped with the nano material lead selenide, method is simple for this, and asepsis environment-protecting has universality, can in the laboratory, prepare fast and effectively, belongs to the inorganic nano material preparing technical field.
Background technology
Nano material just becomes a kind of material the most dynamic in the novel material after coming to light.Nano material is owing to have small-size effect, surface effects, quantum size effect and macro quanta tunnel effect etc.; It is showed from the distinct performance of traditional macrocrystal material in many aspects; Be widely used in numerous researchs and Application Areas, the progress that promotes development and national economy and Future Society has been had irreplaceable effect.
Lead selenide is as a kind of important semiconductor nano material, and it is typical IV ~ VI family, the direct band-gap semicondictor with cube sodium chloride type structure, and energy gap is very little, and spectral absorption is arranged in infrared to visible region, has significant infrared electric conductivity matter.Because energy gap is narrow, lead selenide can be used for producing many devices such as light detector, photoresistor, optical transmitting set, owing to the size adjustable of lead selenide nano particle, can effectively control its energy gap, thereby better meet the demand of various devices again.At present, lead selenide nano material has been widely used in fields such as photoelectronics, biophysics, fluorescence microscopy and has had important application prospects.
The present method for preparing the nano material lead selenide has a variety of, comprises hydrothermal method, microwave method; Sonochemical method, photochemical method, chemical radiation etc.; But the above method preparation condition is strict, complex operation, and time remaining is long; Cost is high, and environmental pollution is serious, prepares result and unsatisfactory sometimes.
Summary of the invention
The technical problem that solves
For fear of the weak point of prior art, the present invention proposes the method that a kind of water legal system is equipped with the nano material lead selenide, and method is simple for this, and asepsis environment-protecting can prepare in the laboratory fast and effectively, and can carry out suitability for industrialized production.
Technical scheme
A kind of water legal system is equipped with the method for nano material lead selenide, it is characterized in that step is following:
Step 1: is that 1.04:1 puts into container with selenium powder and Peng Qinghuana according to mass ratio, adds zero(ppm) water, in container, charge into argon gas again with the expeling dissolved oxygen, and ice bath reacts to colorless cleared solution under the protection of argon gas, generates needed sodium hydrogen selenide solution;
Step 2: plumbic acetate is put into container, add zero(ppm) water it is dissolved fully, adding volume again is the thin basic propionic acid of 0.5%-2%, and with pH value to 6.0 ~ 10.0 of sodium hydroxide solution regulator solution; Feed argon gas again to remove dissolved oxygen wherein, under argon shield, stir and add the sodium hydrogen selenide solution of step 1 preparation, be heated to 80 ° of C ~ 120 ° C, stopped reaction behind the 0 ~ 2.0h that refluxes; The mass ratio of said plumbic acetate and selenium powder is 4.8:1;
Step 3: after treating that solution naturally cools to room temperature, adopt the nano material lead selenide material that makes the black powder shape after washing with acetone, centrifugal, the vacuum-drying.
Beneficial effect
The present invention provides a kind of water legal system to be equipped with the method for nano material lead selenide, and preparation technology's flow process is simple, does not need severe condition such as HTHP; And suitable continuous production; Compare with the technology that has other now, the present invention is environmental protection more, does not produce too much pollution; Can also pass through the CONTROL PROCESS process, thus the form of control product.
Description of drawings
Fig. 1 is the nanocrystalline X-ray powder diffraction figure of embodiment one prepared PbSe.
Fig. 2 is the nanocrystalline X-ray powder diffraction figure of embodiment two prepared PbSe.
Fig. 3 is the nanocrystalline X-ray powder diffraction figure of embodiment three prepared PbSe.
Fig. 4 is the nanocrystalline X-ray powder diffraction figure of embodiment four prepared PbSe.
Fig. 5 is the nanocrystalline X-ray powder diffraction figure of embodiment five prepared PbSe.
Fig. 6 is the nanocrystalline X-ray powder diffraction figure of embodiment six prepared PbSe.
Fig. 7 is the nanocrystalline X-ray powder diffraction figure of embodiment seven prepared PbSe.
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
Step 1: selenium powder and Peng Qinghuana are put into container, add zero(ppm) water, in container, charge into argon gas again and driven away dissolved oxygen, and ice bath reacts to colorless cleared solution under the protection of argon gas, generate needed sodium hydrogen selenide solution, reaction principle is following:
4NaBH
4+2Se+7H
2O=2NaHSe+Na
2B
4O
7+14H
2
Step 2: plumbic acetate is put into container, add zero(ppm) water it is dissolved fully, add again and dredge basic propionic acid, and with pH value to 6.0 ~ 10.0 of sodium hydroxide solution regulator solution.Solution system is fed argon gas to remove dissolved oxygen wherein; Under argon shield, stir fast and add freshly prepd sodium hydrogen selenide solution; Heating, backflow, back stopped reaction; After treating that solution naturally cools to room temperature, with making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying.When temperature reaches the predetermined temperature of experiment, do not reflux and stopped reaction, also can obtain nano material PbSe, be the size that different return times influences nano particle.
Dredge basic propionic acid in experiment as coating, be used for encapsulated nanoparticles, prevent the reunion between the nano particle, unnecessary thin basic propionic acid has been vapored away when the heating of step 2.
Embodiment one
The concrete preparation process of present embodiment is following:
Take by weighing the 0.399g selenium powder earlier in three-necked bottle, add 0.384g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 1.921g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 1.0mL, and with the pH value to 6.0 of 1mol/L NaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 100 ° of C, stopped reaction behind the backflow 0.5h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 15.11nm.
Embodiment two
The concrete preparation process of present embodiment is following:
Take by weighing the 0.399g selenium powder earlier in three-necked bottle, add 0.384g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 1.921g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 1.50mL, and with the pH value to 7.0 of 1mol/LNaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 120 ° of C, stopped reaction behind the backflow 0.5h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 8.04nm.
Embodiment three
The concrete preparation process of present embodiment is following:
Take by weighing the 0.416g selenium powder earlier in three-necked bottle, add 0.40g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 2.0g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 2.00mL, and with the pH value to 8.0 of 1mol/L NaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 100 ° of C, stopped reaction behind the backflow 0.5h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 9.08nm.
Embodiment four
The concrete preparation process of present embodiment is following:
Take by weighing the 0.399g selenium powder earlier in three-necked bottle, add 0.384g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 1.921g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 1.50mL, and with the pH value to 8.0 of 1mol/LNaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 100 ° of C, stopped reaction behind the backflow 0h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 11.85nm.
Embodiment five
The concrete preparation process of present embodiment is following:
Take by weighing the 0.52g selenium powder earlier in three-necked bottle, add 0.50g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 2.50g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 2.00mL, and with the pH value to 8.0 of 1mol/L NaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 100 ° of C, stopped reaction behind the backflow 1.0h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 11.06nm.
Embodiment six
The concrete preparation process of present embodiment is following:
Take by weighing the 0.399g selenium powder earlier in three-necked bottle, add 0.384g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 1.921g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 1.50mL, and with the pH value to 8.0 of 1mol/LNaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 80 ° of C, stopped reaction behind the backflow 0.5h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 6.58nm.
Embodiment seven
The concrete preparation process of present embodiment is following:
Take by weighing the 0.399g selenium powder earlier in three-necked bottle, add 0.384g Peng Qinghuana and 50mL zero(ppm) water, ice bath reacts to achromaticity and clarification under argon shield, generates required sodium hydrogen selenide solution; Take by weighing the 1.921g plumbic acetate again in three-necked bottle, add 100mL zero(ppm) water and the thin basic propionic acid of 1.50mL, and with the pH value to 10.0 of 1mol/LNaOH solution regulator solution.Solution system is led to argon gas to remove dissolved oxygen; Under argon shield, stir the freshly prepd sodium hydrogen selenide solution of adding fast, be heated to 100 ° of C, stopped reaction behind the backflow 0.5h; After treating that solution naturally cools to room temperature; With making black powder shape PbSe nanocrystalline material after washing with acetone, centrifugal, the vacuum-drying, pattern is a nano particle, and mean diameter is 8.05nm.
Claims (1)
1. a water legal system is equipped with the method for nano material lead selenide, and its characterization step is following:
Step 1: is that 1.04:1 puts into container with selenium powder and Peng Qinghuana according to mass ratio, adds zero(ppm) water, in container, charge into argon gas again with the expeling dissolved oxygen, and ice bath reacts to colorless cleared solution under the protection of argon gas, generates needed sodium hydrogen selenide solution;
Step 2: plumbic acetate is put into container, add zero(ppm) water it is dissolved fully, adding volume again is the thin basic propionic acid of 0.5%-2%, and with pH value to 6.0 ~ 10.0 of sodium hydroxide solution regulator solution; Feed argon gas again to remove dissolved oxygen wherein, under argon shield, stir and add the sodium hydrogen selenide solution of step 1 preparation, be heated to 80 ° of C ~ 120 ° C, stopped reaction behind the 0 ~ 2.0h that refluxes; The mass ratio of said plumbic acetate and selenium powder is 4.8:1;
Step 3: after treating that solution naturally cools to room temperature, adopt the nano material lead selenide material that makes the black powder shape after washing with acetone, centrifugal, the vacuum-drying.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172039A (en) * | 2013-03-05 | 2013-06-26 | 西北工业大学 | Method for preparing nano-material lead selenide through organic phase method |
| CN107311121A (en) * | 2017-07-21 | 2017-11-03 | 华北理工大学 | A kind of system for preparing nano lead-selenide |
| CN108584890A (en) * | 2018-06-26 | 2018-09-28 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of selenizing thin film lead |
| CN110240148A (en) * | 2019-06-10 | 2019-09-17 | 陕西科技大学 | Two tungsten selenides of metal structure/redox graphene composite structure and preparation method thereof |
| CN112331668A (en) * | 2020-10-27 | 2021-02-05 | 复旦大学 | Visible-infrared band two-dimensional charge trapping memory and preparation method thereof |
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| CN1569619A (en) * | 2004-04-29 | 2005-01-26 | 上海交通大学 | Aqueous phase synthesis for high quality cadmium selenide quantum dots in temperature controlled microwave reactor |
| CN1792773A (en) * | 2005-12-28 | 2006-06-28 | 中国科学院长春应用化学研究所 | Process for preparing aqueous phase lead selenide nano material |
| CN101012054A (en) * | 2007-01-04 | 2007-08-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick and use thereof |
| CN101913600A (en) * | 2010-08-27 | 2010-12-15 | 上海交通大学 | Method for preparing graphene/semiconductor quantum dot composite material |
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| CN1569619A (en) * | 2004-04-29 | 2005-01-26 | 上海交通大学 | Aqueous phase synthesis for high quality cadmium selenide quantum dots in temperature controlled microwave reactor |
| CN1792773A (en) * | 2005-12-28 | 2006-06-28 | 中国科学院长春应用化学研究所 | Process for preparing aqueous phase lead selenide nano material |
| CN101012054A (en) * | 2007-01-04 | 2007-08-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick and use thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172039A (en) * | 2013-03-05 | 2013-06-26 | 西北工业大学 | Method for preparing nano-material lead selenide through organic phase method |
| CN107311121A (en) * | 2017-07-21 | 2017-11-03 | 华北理工大学 | A kind of system for preparing nano lead-selenide |
| CN108584890A (en) * | 2018-06-26 | 2018-09-28 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of selenizing thin film lead |
| CN110240148A (en) * | 2019-06-10 | 2019-09-17 | 陕西科技大学 | Two tungsten selenides of metal structure/redox graphene composite structure and preparation method thereof |
| CN110240148B (en) * | 2019-06-10 | 2020-12-01 | 陕西科技大学 | Tungsten diselenide/redox graphene composite structure with metal structure and preparation method thereof |
| CN112331668A (en) * | 2020-10-27 | 2021-02-05 | 复旦大学 | Visible-infrared band two-dimensional charge trapping memory and preparation method thereof |
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Application publication date: 20121128 |