CN107720807A - A kind of preparation method of sulfide nanocrystalline material - Google Patents
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Abstract
The invention discloses the present invention relates to a kind of preparation method of sulfide nanocrystalline material, it is characterised in that the preparation method comprises the following steps：Lead compound, dimethylamino dithiocarbonic acid sodium are added in pure water, 30 40min of ultrasound after stirring, filter, wash, drying and to obtain lead source presoma；Lead source presoma is added in organic solvent, is sufficiently stirred and mixes, is cleaned by ultrasonic 20 30min and obtains forerunner's reaction solution；Under 100 400W ultrasonic agitation power, by forerunner's reaction solution gradient microwave heat, wherein gradient microwave be heated to be heated to 110 120 DEG C the first reaction solution, warming temperature gradient is 35 40 DEG C/min；It is heated to 130 180 DEG C of 4 6min of insulation and obtains the second reaction solution, warming temperature gradient is 2 30 DEG C/min；S4：Second reaction solution is naturally cooled into room temperature, centrifuges and washing of precipitate is obtained into sulfide nanocrystalline material.
Description
Invention field
The present invention relates to a kind of preparation method of nanocrystalline material, and in particular to a kind of preparation of sulfide nanocrystalline material
Method, belong to nanocrystalline material field.
Background technology
Nano material is an important development direction of modern material science.It has four big effects, i.e. quantum size is imitated
Answer, small-size effect, skin effect, macro quanta tunnel effect, so as to show the optics different from traditional material, electricity, magnetic
, calorifics, mechanics, chemistry and diffusion and sintering characteristic.
For semiconductor nano material by the extensive concern of numerous scientists, the different sizes of material open exploration with structure
New opportunities of its chemical property with physical property.Vulcanized lead (PbS) has narrow band gap (0.41eV) with larger bohr half
Footpath, while paid attention to as a kind of important and typical direct band-gap semicondictor by scientific circles, vulcanize lead base micro-nano structure work(
Energy material has extensive in optics, sensor, laser, solar cell, near-infrared probe, the field such as microelectronics and thermoelectricity
Purposes, however, how to tie up, be grown with shaping looks surely, being assembled and self assembly vulcanization lead base micro-nano structure material, be still current material
One of key challenge of field face such as material and nanometer technology.
At present, physical-chemical process research relative maturity, the method for preparing Nano lead sulfide mainly have hydro-thermal method, solvent heat
Method, microwave method, sonochemical method, Electron-beam irradiation, phase transfer method, reducing process etc..
Liao et al. is with microwave method by appropriate PbAc2·3H2O is added in formaldehyde, then adds appropriate thio second
Phthalein amine, mixed solution is placed in microwave return-flow system and heats 20min, be cooled to room temperature and obtain PbS nano cubics crystalline substance
Body.
Liao Xuehong, Chen Yu etc. use microwave method, with Pb (NO3)2, thioacetamide (TAA) be raw material, pass through change 16
It is nanocrystalline that the dosage of alkyl trimethyl ammonium bromide (CTAB) has synthesized square PbS.
On the other hand, patent document (publication number：CN105253911A) disclose it is a kind of using sulfate reducing bacteria (SRB,
Clostridiaceae sp.) method for preparing vulcanized lead nano material, and by adjusting dispersant polyethylene glycol in solution
2000 (PEG 2000) amount is prepared for the cubic system vulcanized lead nano material of three kinds of different-shapes.
But above-mentioned preparation process is complicated, needs to consider multiple key process parameters in preparation process, in practical application
Still it is extremely restricted.
The content of the invention
The present invention is in view of the above-mentioned problems existing in the prior art, it is proposed that a kind of simple, quick, preparation cost-effective and environmentally friendly
Method, meanwhile, Novel vulcanization lead nanocrystalline material that the preparation method obtains is regular, morphology controllable.
The above-mentioned purpose of the present invention can be realized by following technical proposal：A kind of preparation side of sulfide nanocrystalline material
Method, the preparation method comprise the following steps：
S1：Lead compound, dimethylamino dithiocarbonic acid sodium are added in pure water, ultrasonic 30-40min after stirring, filter,
Wash, dry to obtain lead source presoma；
S2：Lead source presoma is added in organic solvent, is sufficiently stirred and mixes, is cleaned by ultrasonic 20-30min and obtains forerunner
Reaction solution；
S3：Under 100-400W ultrasonic agitation power, forerunner's reaction solution gradient microwave is heated, wherein gradient microwave adds
Heat obtains the first reaction solution to be heated to 110-120 DEG C, and warming temperature gradient is 35-40 DEG C/min；It is heated to 130-180 DEG C of insulation
4-6min obtains the second reaction solution, and warming temperature gradient is 2-30 DEG C/min；
S4：Second reaction solution is naturally cooled into room temperature, centrifuges and washing of precipitate is obtained into sulfide nanocrystalline material.
The present invention by controlling different temperature to be worth to the sulfide nanocrystalline material of the different-shape, wherein,
Temperature is maintained at 130-140 DEG C and obtains bar-shaped sulfide nanocrystalline material in S3 steps, and temperature is maintained at 170-180 DEG C and obtains six
Flat column sulfide nanocrystalline body.But when change some technological parameters such as raw material dosage ratio, microwave power, thermostat temperature therein
Deng can not then obtain the nano material that such a form can vary with temperature.
In a kind of above-mentioned preparation method of sulfide nanocrystalline material, the lead compound is lead sulfate, plumbi nitras, chlorine
Change the one or more in lead, most preferably plumbi nitras.
In a kind of above-mentioned preparation method of sulfide nanocrystalline material, the lead compound and two thio first of dimethylamino
The mol ratio of sour sodium is 1: 2-3, most preferably 1: 2.
In the preparation method of sulfide nanocrystalline material of the present invention, the temperature being stirred by ultrasonic in the S1 steps is 50-
60℃。
In a kind of above-mentioned preparation method of sulfide nanocrystalline material, it is aided with constant temperature when being cleaned by ultrasonic in the S2 steps
Heating, temperature are 50-60 DEG C.
In a kind of above-mentioned preparation method of sulfide nanocrystalline material, the organic solvent is ethylene glycol, N, N- diformazans
Any one in base formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO) or N- methyl pyrrolidones (NMP), most preferably second two
Alcohol.
The vulcanized lead synthesized under different temperatures causes bar-shaped vulcanized lead to have excellent table due to its structure and morphology feature
Face enhancing Ramam effect (SERS), so as to applied to Raman detection, have a good application prospect.
A kind of measuring method of surface-enhanced Raman effects, the measuring method utilize sulfide nanocrystalline as described above
Material.The measuring method comprises the following steps：By the sulfide nanocrystalline material at room temperature, with equal-wattage
The LASER Light Source of 633nm wavelength is tested with Raman spectrometer, and by the identical time for exposure, makes laser by filter plate,
Impinged upon under 100 times of object lens on sample, wherein, sample is made on a silicon substrate by being dissolved in put after ethanol.
In order to further study the Raman trait of described sulfide nanocrystalline material, in the case of taking anaerobic, with not
It is synthermal to measure, to explore the temperature characterisitic of material.
Compared with prior art, the invention has the advantages that：
1st, the present invention synthesizes the sulfide nanocrystalline material of different-shape by differential responses temperature control, method is simple,
Quickly, cost-effective and environmentally friendly；
2nd, the sulfide nanocrystalline material of different structure shape characteristic produced by the present invention, can be used for Raman detection, examine
The fields such as survey, sensing have huge potential using value.
Brief description of the drawings
Fig. 1 is under low power ESEM, and vulcanized lead is by the bar-shaped six dendritic vulcanized lead to 180 DEG C of high temperature of 130 DEG C of low temperature
Pattern change.
Fig. 2 is under transmission electron microscope picture, and six dendritic vulcanized lead are observed from high resolution transmission electron microscopy (HRTEM)
The width of 0.212nm lattice fringes be present.
Fig. 3 is power spectrum (EDX) test of vulcanized lead nano material：Show containing tetra- kinds of elements of Pb, S, C, N.
Fig. 4 is X-ray diffractogram (XRD), with (Pb (DMDC)2) sulphur lead source obtained in the XRD diffraction patterns of sample, band side
The diffraction maximum of piece asterisk note is Pb (DMDC)2Diffraction maximum, remaining mainly corresponds to PbS diffraction maximum.
Fig. 5 is x-ray photoelectron power spectrum (XPS), with sulphur lead source (Pb (DMDC)2) obtain sample and combine other sign sides
Formula：It can be seen that Pb exists in the form of PbS in material.
Fig. 6 is PbS and Pb (DMDC)2/ PbS thermal gravimetric analysis curve
Fig. 7 is PbS and Pb (DMDC)2/ PbS infrared analysis spectrograms, it is determined that the wherein chemical bond state in lead source.
Fig. 8 is that (a is time for exposure 30s for the Raman figure of different exposure time；B is 10s) A be 5 DEG C/min bar-shaped sample
Product；B is 10 DEG C/min；C is 30 DEG C/min.
Fig. 9 is the Raman shift contrast of different material：A is Au；B is sample；C is PbS QDs；D is power.
Specific implementation method
It is the specific embodiment of the present invention below, technical scheme is further described with reference to accompanying drawing, but
The present invention is not limited to these embodiments.
Embodiment 1
S1：Respectively by 0.1mol plumbi nitras, 0.2mol dimethylamino dithiocarbonic acid sodium (Sodium Dimethyldithiocarbamate), 200ml is put into
Beaker in, add 100ml high purity waters, stirring, then ultrasonic 30min, allows it to react completely, then filters, washing, 120
2h is dried under degree Celsius, white chunks product is obtained, is smashed in mortar, installed in vial, be placed in drying
It is stand-by in case.
S2：0.05mmol presoma dimethylamino dithiocarbonic acid lead is weighed out, 50ml ethylene glycol is measured, is put into 50ml
In long-neck twoport round-bottomed flask.Ultrasonic 20min in supersonic cleaning machine is placed on, while is aided with and is heated to 50 DEG C.
S3：In the case where power 200W is stirred by ultrasonic, forerunner's reaction solution that step S2 is obtained is heated to by room temperature microwave
120 DEG C, warming temperature gradient is 35-40 DEG C/min, obtains the first reaction solution；First reaction solution continuation microwave is heated to 180
DEG C and 130 DEG C (140 DEG C, 160 DEG C, 180 DEG C), and at such a temperature keep 5 minutes, obtain the second reaction solution；
S4：Second reaction solution is naturally cooled into room temperature, and centrifuged 5 minutes with 9000rpm centrifugal speed, by institute
Respectively washing 3 times of priority absolute ethyl alcohol and deionized water must be precipitated, then preserves and obtains sulfide nanocrystalline material in ethanol
It is named as PbS-1.
Embodiment 2-4
With being different only in that for embodiment 1, the amount of the weighing difference of lead dimethyl dithiocarbamate in embodiment 2-4
For 0.01mol, 0.03mol and 0.06mol, other are same as Example 1, and here is omitted, obtained sulfide nanocrystalline
Material is respectively designated as PbS-2, PbS-3 and PbS-4.
Embodiment 5-7
With being different only in that for embodiment 1, the power being stirred by ultrasonic in embodiment 5-7 be respectively 100W, 300W and
400W, other are same as Example 1, and here is omitted, obtained sulfide nanocrystalline material be respectively designated as PbS-5,
PbS-5 and PbS-7.
Embodiment 8-10
With being different only in that for embodiment 1, in the embodiment 8-10 microwave end-point temperature be respectively 150 DEG C, 170
DEG C, 190 DEG C, other are same as Example 1, and here is omitted, and obtained sulfide nanocrystalline material is respectively designated as PbS-
8th, PbS-9 and PbS-10.
Embodiment 11-13
With being different only in that for embodiment 1, in the embodiment 11-13 microwave heating thermal-insulation time be respectively 0min,
10min, 20min, other are same as Example 1, and here is omitted, and obtained sulfide nanocrystalline material is respectively designated as
PbS-11, PbS-12 and PbS-13.
Embodiment 14-15
With being different only in that for embodiment 1, second of warming temperature gradient is respectively 5 DEG C/min in embodiment 14-15
With 15 DEG C/min, other are same as Example 1, and here is omitted, and obtained sulfide nanocrystalline material is respectively designated as
PbS-14 and PbS-15.
Six dendritic vulcanized lead nano materials obtained by above-described embodiment have been carried out with the microscopic sdIBM-2+2q.p.approach of a variety of means of different, has been tied
Fruit is as follows：
1st, discovery is characterized to PbS-5-PbS-7 SEM, PbS-5-PbS-7 form is six dendritic similar structures, but shape
Looks systematicness is less than PbS-1 (180 DEG C).
2nd, PbS-8-PbS-10 SEM is characterized and found, PbS-8 and PbS-9 not yet generate six dendritic appearance structures and
Bulk presoma assembly be present, PbS-10 form is dendritic for six, and PbS-9 pattern rule is poor, illustrates temperature to pattern
Control station leading position.
3rd, discovery is characterized to PbS-11-PbS-13 SEM, bulk presoma assembly is present in PbS-11, shown as anti-
Should not completely, PbS-12 and PbS-13 and PbS-1 patterns are basically identical, but short are preferred with the reaction time.
4th, PbS-14-PbS-15 SEM is characterized and found, bulk presoma assembly in PbS-14 be present, and pattern with
Sea urchin shape has that gap, PbS-14 and PbS-15 and PbS-1 patterns are basically identical, but short is preferred with the reaction time.
Embodiment 16:
The bar-shaped sulfide nanocrystalline material of the gained of embodiment 1 is tested for Raman, specific processing method is：
Sulfide nanocrystalline self assembly macroscopic body and the vulcanized lead nano material synthesis synthesized by different heating rates are stand-by；
The preparation method of vulcanized lead quantum dot comes from document report in recent years, at room temperature, by 1mmol lead chloride and 5mL oil
Ammonia (OLA) is added in three neck round bottom, under vacuum state magnetic agitation oil bath be warming up to 100 degrees Celsius formation chlorinations
Lead oil ammonia mixture, i.e., overall to clarify, the heat time is one hour, and nitrogen is led under 100 degrees Celsius, continues heating 5 minutes,
At the same time, 0.67mmol sulphur powders are added inside another round-bottomed flask to mix with 205ml oily ammonia, and heat under vacuo
To 80 degrees Celsius of 30min, taking-up is rapidly injected in vulcanization lead oil ammonia mixed system, is warming up to 210 degrees Celsius, is kept in this temperature
5min, centrifugation finally is washed with hexamethylene, is stored among hexamethylene, it is stand-by.
Embodiment 17
The clean silicon chips of 1cm*1cm are taken, sample is taken out 200 microlitres with liquid rifle, uniformly drops on silicon chip, is dried with infrared lamp
It is dry, place it on Raman spectrometer, dynamic scan, 100~3000 wave numbers of scanning range, 10 seconds time for exposure, exposure time
Number 3 times, laser power 5mw.
Embodiment 18
Under conditions of anaerobic argon gas, PbS/Pb (DMDC) is tested2Self assembly macroscopic body in 3K, 20K, 40K, 60K, 80K,
The Raman of 100K, 150K, 300K different temperatures is corresponding.
Embodiment 19
Using 4- mercaptopyridines as probe molecule, take its solid powder to measure as a comparison, then match somebody with somebody it with water
Into 10-3Mol/L solution, alternative sample is weighed into 0.002g and is put into wherein, magneton stir 24 hours it is stand-by；In order to reach pair
The effect of ratio, the magneton that the vulcanized lead quantum dot prepared is equally put into progress same time under same concentration by we stir
Mix, three samples are placed on silicon on-chip testing.
In summary, the preparation method of the present invention passes through specific technique it can be seen from above-mentioned all embodiments
The synergistic combination and coordinative role of step and technological parameter etc., so as to obtain the bar-shaped sulfide nanocrystalline with unique morphology
Material, and there is good Raman performance and SERS effects.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to the protection model of the limitation present invention
Enclose.In addition, it should also be understood that, after the technology contents of the present invention have been read, those skilled in the art can make each to the present invention
Kind change, modification and/or variation, all these equivalent form of values equally fall within what the application appended claims were limited
Within protection domain.
Claims (8)
1. a kind of preparation method of sulfide nanocrystalline material, it is characterised in that the preparation method comprises the following steps：
S1：Lead compound, dimethylamino dithiocarbonic acid sodium are added in pure water, ultrasonic 30-40min after stirring, filters, wash
Wash, dry to obtain lead source presoma；
S2：Lead source presoma is added in organic solvent, is sufficiently stirred and mixes, is cleaned by ultrasonic 20-30min and obtains forerunner's reaction
Liquid；
S3：Under 100-400W ultrasonic agitation power, forerunner's reaction solution gradient microwave is heated, wherein gradient microwave is heated to be
It is heated to 110-120 DEG C and obtains the first reaction solution, warming temperature gradient is 35-40 DEG C/min；It is heated to 130-180 DEG C of insulation 4-
6min obtains the second reaction solution, and warming temperature gradient is 2-30 DEG C/min；
S4：Second reaction solution is naturally cooled into room temperature, centrifuges and washing of precipitate is obtained into sulfide nanocrystalline material.
2. the preparation method of a kind of sulfide nanocrystalline material according to claim 1, it is characterised in that the leaded is closed
Thing is the one or more in lead sulfate, plumbi nitras, lead chloride.
3. the preparation method of a kind of sulfide nanocrystalline material according to claim 1, it is characterised in that the leaded is closed
The mol ratio of thing and dimethylamino dithiocarbonic acid sodium is 1:2-3.
A kind of 4. preparation method of sulfide nanocrystalline material according to claim 1, it is characterised in that the S1 steps
The temperature of middle ultrasonic agitation is 50-60 DEG C.
A kind of 5. preparation method of sulfide nanocrystalline material according to claim 1, it is characterised in that the S2 steps
It is aided with heated at constant temperature during middle ultrasonic cleaning, temperature is 50-60 DEG C.
6. the preparation method of a kind of sulfide nanocrystalline material according to claim 1, it is characterised in that described organic molten
Agent is appointing in ethylene glycol, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) (DMSO) or 1-METHYLPYRROLIDONE (NMP)
Meaning is a kind of.
7. a kind of measuring method of surface-enhanced Raman effects, it is characterised in that the measuring method is utilized such as claim 1 institute
State the sulfide nanocrystalline material of method preparation.
A kind of 8. measuring method of surface-enhanced Raman effects according to claim 7, it is characterised in that the measurement side
Method comprises the following steps：Sulfide nanocrystalline material prepared by method as claimed in claim 1 is placed at room temperature, with identical work(
The LASER Light Source of the 633nm wavelength of rate is tested with Raman spectrometer, and by the identical time for exposure, laser is passed through filtering
Piece, impinged upon under 100 times of object lens on sample, wherein, sample is made on a silicon substrate by being dissolved in put after ethanol.
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| CN109467061A (en) * | 2018-10-23 | 2019-03-15 | 温州大学新材料与产业技术研究院 | A kind of PbS-Te nano particle of carried noble metal and preparation method thereof |
| CN112678864A (en) * | 2020-12-25 | 2021-04-20 | 电子科技大学 | Preparation method of lead sulfide sol |
| WO2024171842A1 (en) * | 2023-02-16 | 2024-08-22 | 富士フイルム株式会社 | PbS QUANTUM DOT LIQUID DISPERSION, METHOD FOR PRODUCING SEMICONDUCTOR FILM, METHOD FOR PRODUCING LIGHT DETECTION ELEMENT, METHOD FOR PRODUCING IMAGE SENSOR, AND METHOD FOR PRODUCING PbS QUANTUM DOT LIQUID DISPERSION |
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