CN107720807B - 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 methods of sulfide nanocrystalline material, it is characterized in that, the preparation method includes the following steps: for lead compound, dimethylamino dithiocarbonic acid sodium to be added in pure water, ultrasound 30-40min after stirring filters, washs, drying and to obtain lead source presoma；Lead source presoma is added in organic solvent, is sufficiently stirred and mixes, ultrasonic cleaning 20-30min obtains forerunner's reaction solution；Under the ultrasonic agitation power of 100-400W, by forerunner's reaction solution gradient microwave heating, wherein gradient microwave heating is to be heated to 110-120 DEG C to obtain the first reaction solution, and warming temperature gradient is 35-40 DEG C/min；It is heated to 130-180 DEG C of heat preservation 4-6min and obtains the second reaction solution, warming temperature gradient is 2-30 DEG C/min；S4: it by the second reaction solution cooled to room temperature, is centrifuged and washing of precipitate is obtained into sulfide nanocrystalline material.
Description
Invention field
The present invention relates to a kind of preparation methods of nanocrystalline material, and in particular to a kind of preparation of sulfide nanocrystalline material
Method belongs to nanocrystalline material field.
Background technique
Nano material is an important development direction of modern material science.It has four big effects, i.e. quantum size is imitated
It answers, small-size effect, skin effect, macro quanta tunnel effect, to show the optics different from traditional material, electricity, magnetic
, calorifics, mechanics, chemistry and diffusion and sintering characteristic.
The different sizes of extensive concern of the semiconductor nano material by numerous scientists, material open exploration with structure
New opportunities of its chemical property with physical property.Vulcanized lead (PbS) has narrow band gap (0.41eV) with biggish bohr half
Diameter, while the attention as a kind of important and typical direct band-gap semicondictor by scientific circles, vulcanize lead base micro-nano structure function
Energy material has extensive in optics, sensor, laser, solar battery, near-infrared probe, the fields 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 faces such as material and nanotechnology.
Currently, physical-chemical process studies relative maturity, the method for preparing Nano lead sulfide mainly has hydro-thermal method, solvent heat
Method, microwave method, sonochemical method, Electron-beam irradiation, phase transfer method, reduction method etc..
Liao et al. is with microwave method by suitable PbAc2·3H2O is added in formaldehyde, then adds suitable thio second
Mixed solution is placed in microwave return-flow system and heats 20min by phthalein amine, is cooled to room temperature and obtains PbS nano cubic 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.
In this regard, 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 dispersing agent polyethylene glycol in solution
The amount of 2000 (PEG 2000) 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 during the preparation process, in practical application
Still it is extremely restricted.
Summary of the invention
The present invention in view of the above-mentioned problems existing in the prior art, proposes a kind of simple, quick, preparation cost-effective and environmentally friendly
Method, meanwhile, the Novel vulcanization lead nanocrystalline material that the preparation method obtains is regular, morphology controllable.
Above-mentioned purpose of the invention can be realized by the following technical scheme: a kind of preparation side of sulfide nanocrystalline material
Method, the preparation method include the following steps:
S1: lead compound, dimethylamino dithiocarbonic acid sodium being added in pure water, ultrasound 30-40min after stirring, filter,
It washs, dry to obtain lead source presoma；
S2: lead source presoma being added in organic solvent, is sufficiently stirred and mixes, and ultrasonic cleaning 20-30min obtains forerunner
Reaction solution；
S3: under the ultrasonic agitation power of 100-400W, by forerunner's reaction solution gradient microwave heating, 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 heat preservation
4-6min obtains the second reaction solution, and warming temperature gradient is 2-30 DEG C/min；
S4: it by the second reaction solution cooled to room temperature, is centrifuged and washing of precipitate is obtained into sulfide nanocrystalline material.
The present invention obtains the sulfide nanocrystalline material of the different-shape by controlling different temperature values, wherein In
Temperature is maintained at 130-140 DEG C and obtains rodlike sulfide nanocrystalline material in S3 step, and temperature is maintained at 170-180 DEG C and obtains six
Flat column sulfide nanocrystalline body.But when change certain technological parameters such as raw material dosage ratio, microwave power, thermostat temperature therein
Deng being then unable to get the nano material that such 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 one of lead or a variety of, most preferably plumbi nitras.
In a kind of above-mentioned preparation method of sulfide nanocrystalline material, the lead compound and the thio first of dimethylamino two
The molar 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 step 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 step
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- diformazan
Any one in base formamide (DMF), dimethyl sulfoxide (DMSO) or N- methyl pyrrolidone (NMP), most preferably second two
Alcohol.
The vulcanized lead synthesized under different temperatures makes rodlike vulcanized lead have excellent table due to its structure and morphology feature
Face enhances Ramam effect (SERS), so as to be applied to Raman detection, has a good application prospect.
A kind of measurement method of surface-enhanced Raman effects, the measurement method utilize sulfide nanocrystalline as described above
Material.The measurement method includes the following steps: 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, laser is made to pass through filter plate,
It is impinged upon on sample under 100 times of object lens, wherein sample is made on a silicon substrate by being dissolved in put after ethyl alcohol.
In order to further study the Raman trait of the sulfide nanocrystalline material, in the case where taking anaerobic, with not
It is synthermal to measure, to explore the temperature characterisitic of material.
Compared with prior art, the present invention has the advantage that
1, the present invention is by the sulfide nanocrystalline material of differential responses temperature control synthesis different-shape, method is simple,
Quickly, cost-effective and environmentally friendly；
2, 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.
Detailed description of the invention
Fig. 1 is under low power scanning electron microscope, and vulcanized lead is by 130 DEG C of low temperature rodlike to 180 DEG C of high temperature of six dendritic vulcanized lead
Pattern variation.
Fig. 2 is under transmission electron microscope picture, and six dendritic vulcanized lead are observed from high resolution transmission electron microscopy (HRTEM)
There are the width of 0.212nm lattice fringe.
Fig. 3 is power spectrum (EDX) test of vulcanized lead nano material: being shown containing tetra- kinds of elements of Pb, S, C, N.
Fig. 4 is X-ray diffractogram (XRD), with (Pb (DMDC)2) sulphur lead source obtains in the XRD diffraction pattern of sample, band side
The diffraction maximum of piece asterisk note is Pb (DMDC)2Diffraction maximum, remaining mainly corresponds to the diffraction maximum of PbS.
Fig. 5 is x-ray photoelectron spectroscopy (XPS), with sulphur lead source (Pb (DMDC)2) sample is obtained in conjunction with other characterization sides
It can be seen that Pb exists in the form of PbS in material likes:.
Fig. 6 is PbS and Pb (DMDC)2The thermal gravimetric analysis curve of/PbS
Fig. 7 is PbS and Pb (DMDC)2/ PbS infrared analysis spectrogram determines the chemical bond state in wherein lead source.
Fig. 8 be different exposure time Raman figure (a be time for exposure 30s；B is 10s) A be 5 DEG C/min rodlike sample
Product；B is 10 DEG C/min；C is 30 DEG C/min.
Fig. 9 is the Raman shift comparison of different material: a Au；B is sample；C is PbS QDs；D is power.
Specific implementation method
The following is specific embodiments of the present invention, and in conjunction with attached drawing, technical scheme of the present invention will be further described, but
Invention is not limited to these embodiments.
Embodiment 1
S1: respectively by 0.1mol plumbi nitras, the dimethylamino dithiocarbonic acid sodium (Sodium Dimethyldithiocarbamate) of 0.2mol, it is put into 200ml
Beaker in, be added 100ml high purity water, stirring, then ultrasound 30min, allows it to react completely, then filters, wash, 120
2h is dried under degree Celsius, is obtained white chunks product, is ground into a powder in mortar, installed in vial, is placed in drying
It is stand-by in case.
S2: weighing out the presoma dimethylamino dithiocarbonic acid lead of 0.05mmol, measures 50ml ethylene glycol, is put into 50ml
In long-neck twoport round-bottomed flask.Ultrasound 20min in supersonic cleaning machine is placed it in, while being aided with and being 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 by room temperature microwave heating extremely
120 DEG C, warming temperature gradient is 35-40 DEG C/min, obtains the first reaction solution；First reaction solution is continued into microwave heating 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: by the second reaction solution cooled to room temperature, and with the centrifugal speed of 9000rpm centrifugation 5 minutes, by institute
It must precipitate and successively respectively be washed 3 times with dehydrated alcohol and deionized water, then save and obtain 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 details are not described herein again, 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 details are not described herein again, 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, microwave heating outlet temperature is respectively 150 DEG C, 170 in embodiment 8-10
DEG C, 190 DEG C, other are same as Example 1, and details are not described herein again, and obtained sulfide nanocrystalline material is respectively designated as PbS-
8, 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 details are not described herein again, 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 details are not described herein again, and obtained sulfide nanocrystalline material is respectively designated as
PbS-14 and PbS-15.
Six dendritic vulcanized lead nano material resulting to above-described embodiment has carried out the microscopic sdIBM-2+2q.p.approach of a variety of means of different, knot
Fruit is as follows:
1, discovery is characterized to the SEM of PbS-5-PbS-7, the form of PbS-5-PbS-7 is six dendritic similar structures, but shape
Looks systematicness is less than PbS-1 (180 DEG C).
2, discovery characterized to the SEM of PbS-8-PbS-10, PbS-8 and PbS-9 not yet generate six dendritic appearance structures and
There are bulk presoma assembly, the form of PbS-10 is six dendritic, and the morphological rules of PbS-9 is poor, illustrates temperature to pattern
Control station leading position.
3, the SEM of PbS-11-PbS-13 is characterized and is found, there are bulk presoma assembly in PbS-11, shown as anti-
Should not completely, PbS-12 and PbS-13 and PbS-1 pattern are almost the same, but short are preferred with the reaction time.
4, discovery characterized to the SEM of PbS-14-PbS-15, there are bulk presoma assembly in PbS-14, and pattern with
Sea urchin shape has gap, PbS-14 and PbS-15 and PbS-1 pattern almost the same, but short is preferred with the reaction time.
Embodiment 16:
The resulting rodlike sulfide nanocrystalline material of embodiment 1 is used for Raman test, specific processing method are as follows:
Sulfide nanocrystalline self assembly macroscopic body and the synthesis of vulcanized lead nano material synthesized by different heating rates are stand-by；
The preparation method of vulcanized lead quantum dot is from document report in recent years, at room temperature, by the lead chloride of 1mmol and 5mL oil
Ammonia (OLA) is added in three neck round bottom, and magnetic agitation oil bath is warming up to 100 degrees Celsius of formation chlorinations under vacuum state
Lead oil ammonia mixture, i.e., whole to clarify, heating time is one hour, and nitrogen is led under 100 degrees Celsius, continues heating 5 minutes,
At the same time, 0.67mmol sulphur powder is added inside another round-bottomed flask to mix with the oily ammonia of 205ml, and heats under vacuum
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 finally washs centrifugation with hexamethylene, is stored among hexamethylene, for use.
Embodiment 17
The clean silicon wafer of 1cm*1cm is taken, sample is taken out 200 microlitres with liquid rifle, uniformly drop is dried on silicon wafer with infrared lamp
It is dry, it places it on Raman spectrometer, dynamic scan, 100~3000 wave numbers of scanning range, the time for exposure 10 seconds, exposure time
Number 3 times, laser power 5mw.
Embodiment 18
Under conditions of anaerobic argon gas, test PbS/Pb (DMDC)2Self assembly macroscopic body in 3K, 20K, 40K, 60K, 80K,
The Raman of 100K, 150K, 300K different temperatures is corresponding.
Embodiment 19
Using 4- mercaptopyridine as probe molecule, its solid powder is taken to measure as a comparison, then matches it with water
At 10-3Alternative sample is weighed 0.002g and is put into wherein by the solution of mol/L, and magneton stirs 24 hours for use；In order to reach pair
The effect of ratio, we equally stir the magneton that the vulcanized lead quantum dot prepared is put into progress same time under same concentration
It mixes, three samples is placed on silicon on-chip testing.
In conclusion the preparation method of the invention it can be seen from above-mentioned all embodiments passes through specific technique
The synergistic combination and coordinative role of step and technological parameter etc., to obtain the rodlike sulfide nanocrystalline with unique morphology
Material, and there is good Raman performance and SERS effect.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit protection model of the invention
It encloses.In addition, it should also be understood that, after reading the technical contents of the present invention, those skilled in the art can make the present invention each
Kind change, modification and/or variation, all these equivalent forms are equally fallen within defined by the application the appended claims
Within protection scope.
Claims (8)
1. a kind of preparation method of sulfide nanocrystalline material, which is characterized in that the preparation method includes the following steps:
S1: lead compound, dimethylamino dithiocarbonic acid sodium are added in pure water, ultrasound 30-40min, filters, washes after stirring
It washs, dry to obtain lead source presoma；
S2: lead source presoma being added in organic solvent, is sufficiently stirred and mixes, and ultrasonic cleaning 20-30min obtains forerunner's reaction
Liquid；
S3: under the ultrasonic agitation power of 100-400W, by forerunner's reaction solution gradient microwave heating, wherein gradient microwave heating is
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 heat preservation 4-
6min obtains the second reaction solution, and warming temperature gradient is 2-30 DEG C/min；
S4: it by the second reaction solution cooled to room temperature, is centrifuged and washing of precipitate is obtained into sulfide nanocrystalline material.
2. a kind of preparation method of sulfide nanocrystalline material according to claim 1, which is characterized in that the leaded is closed
Object is one of lead sulfate, plumbi nitras, lead chloride or a variety of.
3. a kind of preparation method of sulfide nanocrystalline material according to claim 1, which is characterized in that the leaded is closed
The molar ratio of object and dimethylamino dithiocarbonic acid sodium is 1:2-3.
4. a kind of preparation method of sulfide nanocrystalline material according to claim 1, which is characterized in that the S1 step
The temperature of middle ultrasonic agitation is 50-60 DEG C.
5. a kind of preparation method of sulfide nanocrystalline material according to claim 1, which is characterized in that the S2 step
It is aided with heated at constant temperature when middle ultrasonic cleaning, temperature is 50-60 DEG C.
6. a kind of preparation method of sulfide nanocrystalline material according to claim 1, which is characterized in that described organic molten
Agent is appointing in ethylene glycol, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) or N-Methyl pyrrolidone (NMP)
It anticipates one kind.
7. a kind of measurement method of surface-enhanced Raman effects, which is characterized in that the measurement method is utilized such as claim 1 institute
State the sulfide nanocrystalline material of method preparation.
8. a kind of measurement method of surface-enhanced Raman effects according to claim 7, which is characterized in that the measurement side
Method includes the following steps: for sulfide nanocrystalline material prepared by method as described in claim 1 to be placed at room temperature, with identical function
The laser light source of the 633nm wavelength of rate is tested with Raman spectrometer, and by the identical time for exposure, laser is made to pass through filtering
Piece impinges upon on sample under 100 times of object lens, wherein sample is made on a silicon substrate by being dissolved in put after ethyl alcohol.
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