CN107699229A - A kind of preparation method for adulterating oil-soluble silver sulfide nano luminescent material - Google Patents
A kind of preparation method for adulterating oil-soluble silver sulfide nano luminescent material Download PDFInfo
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- CN107699229A CN107699229A CN201710860018.2A CN201710860018A CN107699229A CN 107699229 A CN107699229 A CN 107699229A CN 201710860018 A CN201710860018 A CN 201710860018A CN 107699229 A CN107699229 A CN 107699229A
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Abstract
The present invention relates to a kind of preparation method for adulterating oil-soluble silver sulfide nano luminescent material, includes the synthesis of mixing presoma, the synthesis of vulcanized sodium presoma, adulterates the synthesis of oil-soluble silver sulfide nano luminescent material；Ag can be prepared2S:Mn nano luminescent materials, Ag2S:Eu nano luminescent materials and Ag2S:Y nano luminescent materials.The method of the present invention is simple, and easily operated, reaction condition is gentle, and cost is low, good operability；The Ag being prepared2S:Mn nano luminescent materials, Ag2S:Eu nano luminescent materials and Ag2S:Y nano luminescent material good crystallinities, be uniformly dispersed stabilization, and fluorescence intensity is high, is had a good application prospect in solar cell, laser, drug test etc..
Description
Technical field
The invention belongs to field of nanometer material technology, more particularly to a kind of preparation for adulterating oil-soluble silver sulfide nano luminescent material
Method.
Background technology
Nano luminescent material has small-size effect, skin effect, quantum size effect and macro quanta tunnel effect, exhibition
Shown with the visibly different optical property of body phase material, be widely used in sensor, solar cell, laser, nanometer
The making of laser material, the degraded of organic pollution, in addition in sides such as drug test, bioprotein mark, DNA quantitative analyses
Face, show good application prospect.
Doping property nano material refers to mix transition metal ions in Conventional nano material【Wei Chen et
al.J.Appl.Phys.2000,88,5188】Or rare metal ion【Huang Yang et al.Mater.Lett,2004,
58,1173】, so as to strengthen the luminescent properties of Conventional nano material.
The quantum dot reported at present is mostly the cadmium based semiconductor quantum dot such as cadmium selenide, cadmium telluride, the bio-toxicity of cadmium element
Greatly limit the application of cadmium system quantum dot with environmental pollution, thus develop the red light quantum point without cadmium system have it is particularly significant
Meaning.
Common doping silver sulfide preparation method mainly has coprecipitation, sol-gel process, microemulsion method etc..Co-precipitation
Method is readily incorporated impurity.Sol-gel process cost of material height and organic solvent insalubrity, are unfavorable for large-scale industry metaplasia
Production.Microemulsion method has that production process is complicated, and cost is high, the problem of low yield.Oil-water interfaces method refers to the raw material difference of reactant
In oil phase and aqueous phase, the preferable lipophile particle of the smaller uniformity of particle diameter is formed in oil-water interface under lower temperature, then
Particle is automatically transferred in oil phase after being wrapped up by surfactant, and good dispersion and can be kept steadily in the long term in oil phase.Oil
Water termination method has the oil solubility nanometer that simple to operate, reaction condition is gentle, cost is low, well-crystallized can be obtained without roasting
The advantages of particle.Zhou Xingping in 2008 etc. uses oil-water interfaces method【Zhou Xingping etc., Donghua University's journal；Natural science edition,
2008.35(4):441-445】Successfully synthesize CdS quantum dot, the quantum dot quantum efficiency high prepared, particle diameter distribution is narrow, single
Good dispersion, synthetic method is simple, and temperature requirement is low, can largely produce, cost is smaller.Zhou Xingping in 2010 etc. uses profit again
Interface method【Zhou Xingping etc., nanosecond science and technology；2010,12:Vo17,No.6】, ZnS quantum dot is successfully synthesized, and it is dilute to adulterate some
There is metal, fluorescence property is good, is a kind of good semi-conducting material.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation for adulterating oil-soluble silver sulfide nano luminescent material
Method, this method is simple, easily operated, and reaction condition is gentle, the doping oil-soluble silver sulfide nano luminescent material being prepared
Fluorescence intensity is high.
A kind of preparation method of doping oil-soluble silver sulfide nano luminescent material of the present invention, including：
(1) one kind in manganese stearate, stearic acid europium, yttrium stearate is mixed to get mixture with silver stearate, will be mixed
Compound dissolving forms solution in a solvent, adds surfactant, stirring, obtains mixing presoma, wherein silver stearate solution
Concentration be 0.01~0.1M, the ratio of silver stearate and surfactant is 1g:3ml~2g:3ml；
(2) vulcanized sodium dissolving is formed into sodium sulfide solution in a solvent, stirs, vulcanized sodium presoma is obtained, wherein vulcanizing
The concentration of sodium solution is 0.03~0.3M；
(3) the vulcanized sodium presoma in step (2) is added in the mixing presoma in step (1), stirs, be transferred to
React, separating, washing, dry in reactor, obtain adulterating oil-soluble silver sulfide nano luminescent material, wherein vulcanized sodium presoma
Volume ratio with mixing presoma is 1:1~1:3.
Manganese stearate and silver stearate are using mol ratio as 1 in the step (1):100~5:100 mixing；Or stearic acid europium
With silver stearate using mol ratio as 0.79:100~12:100 mixing；Or yttrium stearate and silver stearate are using mol ratio as 1:100
~25:100 mixing.
Manganese stearate and silver stearate are using mol ratio as 1 in the step (1):100 mixing；Or stearic acid europium and stearic acid
Silver is using mol ratio as 0.79:100 mixing；Or yttrium stearate and silver stearate are using mol ratio as 10:100.
Manganese stearate mixes with silver stearate in the step (1), and Ag is prepared2S:Mn nano luminescent materials；It is or hard
Resin acid europium mixes with silver stearate, and Ag is prepared2S:Eu nano luminescent materials；Or yttrium stearate mixes with silver stearate, system
It is standby to obtain Ag2S:Y nano luminescent materials.
Solution temperature is 80 DEG C in the step (1)；Solvent is hexamethylene；Surfactant is oleic acid.
Solvent is deionized water in the step (2).
Reaction temperature is 180 DEG C in the step (3), reaction time 2h.
Separating, washing concretely comprises the following steps in the step (3)：Absolute ethyl alcohol is added, layering, it is molten to isolate upper oil phase
Liquid, remove lower floor's aqueous phase, then be washed with deionized, isolate upper oil phase solution, 10min is centrifuged under 10000rmp, use
Washes of absolute alcohol 2 times, then centrifuge 10min under 10000rmp.
Drying temperature is 65~70 DEG C in the step (3), and drying time is 2~4h.
The preparation method of a kind of doping oil-soluble silver sulfide nano luminescent material of the present invention, with deionized water and hexamethylene
For solvent, using silver stearate as silver-colored source, using manganese stearate as manganese source, using stearic acid europium as europium source, using yttrium stearate as yttrium source, with
Vulcanized sodium is sulphur source, using oleic acid as surfactant, is reacted with oil-water interfaces method, obtains Ag2S:Mn nano luminescent materials,
Ag2S:Eu nano luminescent materials and Ag2S:Y nano luminescent materials.The present invention is stearic at oil-water interfaces by oil-water interfaces method
It is doping oil-soluble with surfactant transitions under manganese source, europium source or yttrium source existence condition under sour silver and vulcanized sodium existence condition
Silver sulfide nano luminescent material.
Beneficial effect
(1) method of the invention is simple, and easily operated, reaction condition is gentle, and cost is low, good operability；
(2) Ag that the present invention obtains2S:Mn nano luminescent materials, Ag2S:Eu nano luminescent materials and Ag2S:Y nano luminescents
Material crystalline is good, and be uniformly dispersed stabilization, and fluorescence intensity is high, has in solar cell, laser, drug test etc. good
Good application prospect.
Brief description of the drawings
Fig. 1 is the process chart of the present invention；
Fig. 2 is the Ag that embodiment 1 obtains2S:The Ag that Mn nano luminescent materials, embodiment 2 obtain2S:Eu nano luminescent materials
The XRD of the oil-soluble vulcanization silver nano material obtained with comparative example 1；
Fig. 3 is the TEM figures that the oil-soluble that comparative example 1 obtains vulcanizes silver nano material；
Fig. 4 is the Ag that embodiment 1 obtains2S:The UV absorption figure of Mn nano luminescent materials；
Fig. 5 is the Ag that embodiment 1 obtains2S:Fluorescent emission figure of the Mn nano luminescent materials when excitation wavelength is 380nm；
Fig. 6 is the Ag that embodiment 2 obtains2S:Fluorescent emission figure of the Eu nano luminescent materials when excitation wavelength is 384nm；
Fig. 7 is the Ag that embodiment 3 obtains2S:Fluorescent emission figure of the Y nano luminescent materials when excitation wavelength is 362nm.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
(1) 1.24g (0.003mol) silver stearate is mixed with 0.025g, 0.075g, 0.125g manganese stearate respectively, made
The mol ratio of manganese stearate and silver stearate is respectively 1:100、3:100、5:100,30ml hexamethylenes are dissolved completely at 80 DEG C
In alkane, 3ml oleic acid is added, magnetic agitation is transparent to solution, obtains adulterating silver stearate and manganese stearate cyclohexane solution.
(2) 2.16g (0.009mol) vulcanized sodium is weighed, is dissolved completely at normal temperatures in 30ml deionized waters, stirring is equal
It is even, obtain sodium sulfide solution.
(3) the doping silver stearate and stearic acid being slowly added into the sodium sulfide solution in step (2) in step (1)
In manganese cyclohexane solution, both volume ratios are 1:1, stir and be transferred in ptfe autoclave, it is anti-at 180 DEG C
2h is answered, reacted solution adds 100ml absolute ethyl alcohols, layering, caused silver sulfide nanometer particles is uniformly dispersed in upper strata oil
Xiang Zhong, lower floor's aqueous phase is removed, then washed with 100ml deionized waters, isolate upper oil phase solution.Take out 1ml oil-phase solutions point
It is dispersed in 25ml hexamethylenes, ultrasound, does fluorometric investigation.Remaining oil phase is centrifuging 10min under 10000rmp, clear with absolute ethyl alcohol
Wash product 2 times, then 10min is centrifuged under 10000rmp, finally obtain deposit in 65 DEG C of dry 2h of vacuum drying chamber
Ag2S:Mn nano luminescent materials.
Fig. 4 shows：The silver sulfide nanometer particles for showing to adulterate different content manganese ion have ultraviolet absorption peak.
Fig. 5 shows：When excitation wavelength is 380nm, the mol ratio of manganese stearate and silver stearate is 1:100 obtain
Ag2S:Mn nano luminescent materials fluoresce maximum intensity.
Embodiment 2
(1) it is 1.24g (0.003mol) silver stearate is stearic with 0.016g, 0.04g, 0.06g, 0.12g, 0.24g respectively
Sour europium mixing, it is respectively 0.79 to make the mol ratio of stearic acid europium and silver stearate:100、2:100、3:100、6:100、12:100,
It is dissolved completely at 80 DEG C in 30ml hexamethylenes, adds 3ml oleic acid, magnetic agitation is transparent to solution, obtains adulterating stearic acid
Silver and stearic acid europium cyclohexane solution.
(2) 2.16g (0.009mol) vulcanized sodium is weighed, is dissolved completely at normal temperatures in 30ml deionized waters, stirring is equal
It is even, obtain sodium sulfide solution.
(3) the doping silver stearate and stearic acid being slowly added into the sodium sulfide solution in step (2) in step (1)
In europium cyclohexane solution, both volume ratios are 1:1, stir and be transferred in ptfe autoclave, it is anti-at 180 DEG C
2h is answered, reacted solution adds 100ml absolute ethyl alcohols, layering, caused silver sulfide nanometer particles is uniformly dispersed in upper strata oil
Xiang Zhong, lower floor's aqueous phase is removed, then washed with 100ml deionized waters, isolate upper oil phase solution.Take out 1ml oil-phase solutions point
It is dispersed in 25ml hexamethylenes, ultrasound, does fluorometric investigation.Remaining oil phase is centrifuging 10min under 10000rmp, clear with absolute ethyl alcohol
Wash product 2 times, then 10min is centrifuged under 10000rmp, finally obtain deposit in 65 DEG C of dry 2h of vacuum drying chamber
Ag2S:Eu nano luminescent materials.
Fig. 6 shows：When excitation wavelength is 384nm, the mol ratio of stearic acid europium and silver stearate is 0.79:100 obtain
Ag2S:Eu nano luminescent materials fluoresce maximum intensity.
Embodiment 3
(1) it is 1.24g (0.003mol) silver stearate is stearic with 0.0285g, 0.1425g, 0.285g, 0.4275g respectively
Sour yttrium mixing, it is respectively 1 to make the mol ratio of yttrium stearate and silver stearate:100、5:100、10:100、15:100, at 80 DEG C
It is dissolved completely in 30ml hexamethylenes, adds 3ml oleic acid, magnetic agitation is transparent to solution, obtains adulterating silver stearate and tristearin
Sour yttrium cyclohexane solution.
(2) 2.16g (0.009mol) vulcanized sodium is weighed, is dissolved completely at normal temperatures in 30ml deionized waters, stirring is equal
It is even, obtain sodium sulfide solution.
(3) the doping silver stearate and stearic acid being slowly added into the sodium sulfide solution in step (2) in step (1)
In yttrium cyclohexane solution, both volume ratios are 1:1, stir and be transferred in ptfe autoclave, it is anti-at 180 DEG C
2h is answered, reacted solution adds 100ml absolute ethyl alcohols, layering, caused silver sulfide nanometer particles is uniformly dispersed in upper strata oil
Xiang Zhong, lower floor's aqueous phase is removed, then washed with 100ml deionized waters, isolate upper oil phase solution.Take out 1ml oil-phase solutions point
It is dispersed in 25ml hexamethylenes, ultrasound, does fluorometric investigation.Remaining oil phase is centrifuging 10min under 10000rmp, clear with absolute ethyl alcohol
Wash product 2 times, then 10min is centrifuged under 10000rmp, finally obtain deposit in 65 DEG C of dry 2h of vacuum drying chamber
Ag2S:Y nano luminescent materials.
Fig. 7 shows：When excitation wavelength is 362nm, the mol ratio of yttrium stearate and silver stearate is 10:100 obtain
Ag2S:Y nano luminescent materials fluoresce maximum intensity.
Comparative example 1
(1) 1.24g (0.003mol) silver stearates are dissolved completely in 30ml hexamethylenes at 80 DEG C, add 3ml oil
Acid, magnetic agitation is transparent to solution, obtains silver stearate cyclohexane solution.
(2) 2.16g (0.009mol) vulcanized sodium is weighed, is dissolved completely at normal temperatures in 30ml deionized waters, stirring is equal
It is even, obtain sodium sulfide solution.
(3) sodium sulfide solution in step (2) is slowly added into the silver stearate cyclohexane solution in step (1)
In, both volume ratios are 1:1, stir and be transferred in ptfe autoclave, 2h is reacted at 180 DEG C, after reaction
Solution add 100ml absolute ethyl alcohols, layering, make caused by silver sulfide nanometer particles be uniformly dispersed in upper oil phase, under removal
Layer aqueous phase, then washed with 100ml deionized waters, isolate upper oil phase solution.Take out 1ml oil-phase solutions and be dispersed in 25ml hexamethylenes
In alkane, ultrasound, TEM tests are done.Remaining oil phase is centrifuging 10min under 10000rmp, with washes of absolute alcohol product 2 times, then
10min is centrifuged under 10000rmp, finally deposit is obtained oil-soluble silver sulfide and received in 65 DEG C of dry 2h of vacuum drying chamber
Rice material.
Fig. 2 shows：After adulterating manganese ion or europium ion, the crystal formation of silver sulfide does not change, or α-Ag2S crystal.
Fig. 3 shows：Obtained oil-soluble vulcanization silver nano material average grain diameter is 20~25nm, is disperseed more uniform.
Claims (9)
1. a kind of preparation method for adulterating oil-soluble silver sulfide nano luminescent material, including：
(1) one kind in manganese stearate, stearic acid europium, yttrium stearate is mixed to get mixture with silver stearate, by mixture
Dissolving forms solution in a solvent, adds surfactant, stirring, obtains mixing presoma, wherein silver stearate solution is dense
Spend for 0.01~0.1M, the ratio of silver stearate and surfactant is 1g:3ml~2g:3ml；
(2) vulcanized sodium dissolving is formed into sodium sulfide solution in a solvent, stirs, obtain vulcanized sodium presoma, wherein vulcanized sodium is molten
The concentration of liquid is 0.03~0.3M；
(3) the vulcanized sodium presoma in step (2) is added in the mixing presoma in step (1), stirs, be transferred to reaction
React, separating, washing, dry in kettle, obtain adulterating oil-soluble silver sulfide nano luminescent material, wherein vulcanized sodium presoma and mixed
The volume ratio for closing presoma is 1:1~1:3.
2. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In manganese stearate and silver stearate are using mol ratio as 1 in the step (1):100~5:100 mixing；Or stearic acid europium and tristearin
Sour silver is using mol ratio as 0.79:100~12:100 mixing；Or yttrium stearate and silver stearate are using mol ratio as 1:100~25:
100 mixing.
3. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In manganese stearate and silver stearate are using mol ratio as 1 in the step (1):100 mixing；Or stearic acid europium and silver stearate with
Mol ratio is 0.79:100 mixing；Or yttrium stearate and silver stearate are using mol ratio as 10:100.
4. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In manganese stearate mixes with silver stearate in the step (1), and Ag is prepared2S:Mn nano luminescent materials；Or stearic acid europium
Mixed with silver stearate, Ag is prepared2S:Eu nano luminescent materials；Or yttrium stearate mixes with silver stearate, it is prepared
Ag2S:Y nano luminescent materials.
5. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In solution temperature is 80 DEG C in the step (1)；Solvent is hexamethylene；Surfactant is oleic acid.
6. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In solvent is deionized water in the step (2).
7. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In reaction temperature is 180 DEG C in the step (3), reaction time 2h.
8. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In separating, washing concretely comprises the following steps in the step (3)：Absolute ethyl alcohol is added, layering, upper oil phase solution is isolated, goes
A layer aqueous phase is fallen down, then is washed with deionized, isolates upper oil phase solution, 10min is centrifuged under 10000rmp, with anhydrous second
Alcohol cleans 2 times, then centrifuges 10min under 10000rmp.
9. according to a kind of preparation method of doping oil-soluble silver sulfide nano luminescent material described in claim 1, its feature exists
In drying temperature is 65~70 DEG C in the step (3), and drying time is 2~4h.
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| CN114316988A (en) * | 2021-12-29 | 2022-04-12 | 武汉大学 | Preparation method and application of near-infrared IIb region metal ion (M = Zn, Mn) doped silver telluride quantum dot |
| CN114540009A (en) * | 2022-02-16 | 2022-05-27 | 西湖大学 | Stable dispersed near-infrared Ag2X nanocrystalline colloidal solution synthesis method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114316988A (en) * | 2021-12-29 | 2022-04-12 | 武汉大学 | Preparation method and application of near-infrared IIb region metal ion (M = Zn, Mn) doped silver telluride quantum dot |
| CN114316988B (en) * | 2021-12-29 | 2023-03-10 | 武汉大学 | Preparation method and application of near-infrared IIb region metal ion (M = Zn, mn) doped silver telluride quantum dot |
| CN114540009A (en) * | 2022-02-16 | 2022-05-27 | 西湖大学 | Stable dispersed near-infrared Ag2X nanocrystalline colloidal solution synthesis method |
| CN114540009B (en) * | 2022-02-16 | 2023-11-28 | 西湖大学 | Stably dispersed near infrared Ag 2 Method for synthesizing X nano-crystal colloid solution |
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