CN106867532B - Lanthanide rare ytterbium adulterates silver sulfide quantum dot and its preparation method and application - Google Patents
Lanthanide rare ytterbium adulterates silver sulfide quantum dot and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of lanthanide rare ytterbium doping silver sulfide quantum dots and its preparation method and application；It is to adulterate Yb using silver sulfide quantum dot as matrix3+For active ions, heterogeneous sulphur layer is grown in silver sulfide quantum dot surface and is obtained, chemical formula are as follows: Ag2S:Yb3+.Preparation method is comprising steps of 1) three hydration sodium oiethyl dithiocarbamates and silver nitrate are reacted to obtain presoma；2) presoma is dissolved in lauryl mercaptan, and heating reaction obtains silver sulfide quantum dot；3) acetic acid ytterbium and olaquindox are mixed to get ytterbium ion solution；4) sulphur powder and octadecylene are mixed to get sulphur solution, 5) silver sulfide quantum dot, octadecylene and olaquindox are added into reaction vessel, it stirs evenly, under the conditions of argon gas, ytterbium solution reaction is added into reaction vessel, it is then injected into sulphur solution reaction, obtains lanthanide rare ytterbium doping silver sulfide quantum dot.Lanthanide rare ytterbium doping silver sulfide quantum dot not only has excellent photochemical properties, but also its small toxicity.
Description
Technical field
The present invention relates to technical field of quantum dot preparation, adulterate silver sulfide more specifically to a kind of lanthanide rare ytterbium
Quantum dot and its preparation method and application.
Background technique
In recent years, Molecular imaging techniques are increasingly developed, and application can make the diagnostic level of disease be promoted to molecule abnormality rank
Section, detects the lesion of molecular level, can directly observe a series of processes such as cause, generation, development of disease in vivo,
And observe the gene of disease, molecular level anomalous variation and feature.As the key technology of molecular imaging, near-infrared fluorescence imaging
Easy to operate, reagent consumes less, is higher to the sensing sensitivity of target molecules, is good biomolecule functional imaging method.
And it is a kind of three-dimensional cluster that relied on fluorescence probe-near-infrared quantum dots (QDs), which are imaged, in near-infrared (NIR), by finite population
Atom composition, three of them dimension in nanometer scale, it be it is a kind of conduction band electron, valence band hole and exciton three
The semiconductor nano material held on a direction in space.The luminosity of quantum dot be by electronics, hole and they around
Caused by the interaction of environment, when excitation level is more than band gap, quantum dot, which is absorbed by photon, makes electronics jump from valence band
Conduction band is adjourned, the electronics on conduction band transition can also return valence band and emit photon and then generate fluorescent effect again.
The quantum dot reported at present is mainly the uniform or core shell being made of II-VI group (such as CdS, CdSe, CdTe) element
The nano particle of structure (such as CdS/HgS/CdS), CdHgTe/ZnS, CdTe/CdSe, ZnTe/CdSe, CdTeSe, CdHgTe etc.
Various near-infrared quantum dots materials have been successfully synthesized.However, majority quantum is all heavy metal sulfide selenides quantum at present
Point makes it be difficult to be widely applied due to containing the toxic ion of heavy metal.Therefore, there is an urgent need to produce a kind of near-infrared quantum dots,
Existing excellent photochemical properties realize penetration into tissue；And low toxicity or nontoxic, to mark and be imaged neck in living body biological
It is applied in the fields such as domain, photoelectron material.
Summary of the invention
The purpose of the present invention is to provide a kind of lanthanide rare ytterbiums to adulterate silver sulfide quantum dot and its preparation method and application,
Lanthanide rare ytterbium doping silver sulfide quantum dot not only has excellent photochemical properties, but also its small toxicity, can be used as glimmering
Signal material is applied in living body biological imaging body.
The technical solution adopted by the present invention to solve the technical problems is:
Lanthanide rare ytterbium adulterates silver sulfide quantum dot, it is to adulterate Yb using silver sulfide quantum dot as matrix3+For activation from
Son grows heterogeneous sulphur layer in silver sulfide quantum dot surface and obtains；The chemical formula of the lanthanide rare ytterbium doping silver sulfide quantum dot
Are as follows: Ag2S:Yb3+。
According to the above scheme, the partial size of the lanthanide rare ytterbium doping silver sulfide quantum dot is 10~20nm.
The preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, comprising the following steps:
1) preparation of presoma silver diethyldithiocarbamate: by three hydration sodium oiethyl dithiocarbamates and nitric acid
Silver is dissolved in deionized water, and magnetic agitation is reacted, and after completion of the reaction, is successively filtered, washed, is dried, before obtaining
Drive body silver diethyldithiocarbamate；
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate is dissolved in lauryl mercaptan
In, heating stirring is uniformly mixed and obtains clear solution under protective gas atmosphere, and hot defecation solution is reacted under the conditions of argon gas,
Successively pass through centrifugal filtration, washing, drying after completion of the reaction, obtains near-infrared silver sulfide quantum dot；
3) preparation of ytterbium solution: under vacuum conditions after mixing evenly by acetic acid ytterbium and olaquindox, heat preservation is uniformly mixed
To ytterbium solution；
4) preparation of sulphur solution: under vacuum conditions after mixing evenly by sulphur powder and octadecylene, heat preservation obtains after mixing
To sulphur solution；
5) preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: near-infrared is added first into reaction vessel and vulcanizes silver content
Sub- point, octadecylene and olaquindox, stir evenly under vacuum conditions, and under the conditions of argon gas, ytterbium solution is injected into reaction vessel,
Insulation reaction injects sulphur solution into reaction vessel again after completion of the reaction and carries out growth sulphur shell reaction certainly, reacts from sulphur shell is grown
It washs, be centrifuged afterwards, gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping silver sulfide quantum dot.
According to the above scheme, the step 1), three hydration sodium oiethyl dithiocarbamates are 20~25mmol, silver nitrate is
20~25mmol, deionized water are 40~50mL, and the magnetic agitation under dark condition, the reaction time is 2~3h, end of reaction
Afterwards, reaction solution is obtained into product through centrifugal filtration, is distinguished washed product 4~6 times with water and dehydrated alcohol, washes clean is placed on
Presoma silver diethyldithiocarbamate is dried to obtain in baking oven.
According to the above scheme, the step 2), presoma silver diethyldithiocarbamate are 0.2~0.4mmol, 12 sulphur
Alcohol is 10~25mL, and mixing time is 10~20min；Reaction temperature is 200~220 DEG C, and the reaction time is 2~3h.
According to the above scheme, the step 3), acetic acid ytterbium are 0.4~1g, and olaquindox is 2~4mL；Whipping temp be 60~
120 DEG C, mixing time is 20~30min；Heat preservation mixing condition is, under the conditions of argon gas, holding temperature is 120~180 DEG C, protects
The warm time is 30~60min.
According to the above scheme, the step 4) is firstly added 0.2~0.32g of sulphur powder, 10~20mL of octadecylene, whipping temp
It is 60~120 DEG C, mixing time is 20~30min, and holding temperature is 120~180 DEG C, and soaking time is 30~60min.
According to the above scheme, the step 5), 0.1~0.2mmol of near-infrared silver sulfide quantum dot, 10~20mL of octadecylene with
And 2~5mL of olaquindox, whipping temp are 60~120 DEG C, mixing time is 20~30min；The rate of ytterbium solution injection is 0.2
~0.4mL/min, reaction temperature are 200~220 DEG C, and the reaction time is 30~60min；Finally with the speed of 0.2~0.4mL/min
Rate injects sulphur solution to reaction vessel, and reaction temperature is 200~220 DEG C, and the reaction time is 30~60min.
Lanthanide rare ytterbium adulterates silver sulfide quantum dot in the application as fluorescence labeling material.Especially as fluorescent marker
Application of the material in living body biological imaging imaging.
The synthesis process of lanthanide rare ytterbium doping silver sulfide quantum dot of the present invention is as shown in Figure 1, the present invention is with silver nitrate
Silver-colored source synthesizes near-infrared silver sulfide quantum dot as sulphur source using lauryl mercaptan first, then using acetic acid ytterbium as ytterbium source, heat injection ytterbium from
Son obtains lanthanide rare ytterbium doping silver sulfide quantum dot finally by injection sulphur solution from one layer of sulphur shell is grown.Lanthanum of the present invention
Be rare earth ytterbium doping silver sulfide quantum dot nucleocapsid construction mechanism it is as shown in Figure 2.
The present invention compared with the existing technology, has the advantages that
1, silver sulfide quantum dot is dissolved in complexing agent olaquindox solvent by the present invention, using octadecylene as surfactant into
Row solvent thermal reaction；200~220 DEG C at a temperature of, the heat that ytterbium ion and sulphur solution are successively injected using given pace is injected
Method makes rare earth ytterbium ion be grown in silver sulfide quantum dot nano crystalline substance surface, from one layer of sulphur shell of growth.Using solvent-thermal method and
Lanthanide rare ytterbium doping silver sulfide quantum dot is prepared in hot injection method, and preparation process is simple, at low cost, and in preparation process
It is environmentally protective without using toxic raw materials.
2, by multiple stirring, the operation such as raw material is added in heating and thermal insulation, and substep, is made each raw material high degree of dispersion, is obtained
The lanthanide rare ytterbium doping silver sulfide quantum dot arrived is uniform in size, and size controlling is in 10~20nm.
3, silver sulfide quantum dot has low toxicity, and biocompatibility is preferable, synthesis condition is mild, emission wavelength is with cluster size
The advantages that adjustable, but the defects of its fluorescence intensity is weaker relatively narrow with fluorescence bands, ytterbium ion has Multi-stage electronic structure, this hair
It is bright by lanthanide rare ytterbium ion in conjunction with silver sulfide quantum dot, fluorescence intensity is greatly improved, and widens quantum dot
Fluorescence bands.
Detailed description of the invention
Fig. 1 is the synthesis process figure that lanthanide rare ytterbium of the present invention adulterates silver sulfide quantum dot；
Fig. 2 is the nucleocapsid construction mechanism figure that lanthanide rare ytterbium of the present invention adulterates silver sulfide quantum dot；
Fig. 3 is the TEM transmission plot that 1 step 2) of the embodiment of the present invention obtains silver sulfide quantum dot；
Fig. 4 is the TEM transmission plot that the embodiment of the present invention 1 obtains lanthanide rare ytterbium doping silver sulfide quantum dot；
Fig. 5 is that the embodiment of the present invention 1 obtains lanthanide rare ytterbium doping silver sulfide quantum dot, and the TEM that scale is 2nm is transmitted
Figure；
Fig. 6 is that 1 step 2) of the embodiment of the present invention obtains the abosrption spectrogram of silver sulfide quantum dot；
Fig. 7 is the abosrption spectrogram that the embodiment of the present invention 1 obtains lanthanide rare ytterbium doping silver sulfide quantum dot.
Specific embodiment
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now control attached drawing is described in detail
A specific embodiment of the invention.
Embodiment 1
The preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, comprising the following steps:
1) preparation of presoma silver diethyldithiocarbamate: sodium oiethyl dithiocarbamate 20mmol is hydrated by three
It is dissolved in 40ml deionized water with silver nitrate 20mmol, the magnetic agitation under dark condition, reacts 2h, it after completion of the reaction, will
Reaction solution obtains product through centrifugal filtration, is distinguished washed product 4 times with water and dehydrated alcohol, washes clean is placed on 70 DEG C of baking ovens
In be dried to obtain presoma silver diethyldithiocarbamate.
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate 0.2mmol is dissolved in
In 12mL lauryl mercaptan, 20min is stirred, is uniformly mixed and obtains clear solution, hot defecation solution carries out anti-under the conditions of argon gas
It answers, reaction temperature is 220 DEG C, reaction time 2h, successively passes through centrifugal filtration, washing, drying after completion of the reaction, is obtained close red
Outer silver sulfide quantum dot.
3) preparation of ytterbium solution: acetic acid ytterbium 0.9g and olaquindox 4mL are stirred under vacuum conditions, whipping temp 60
DEG C, mixing time 20min, heat preservation, which is uniformly mixed, obtains ytterbium solution, and holding temperature is 150 DEG C, soaking time 30min.
4) preparation of sulphur solution: sulphur powder 0.32g and octadecylene 20mL are stirred under vacuum conditions, whipping temp 60
DEG C, mixing time 20min, heating and thermal insulation, holding temperature are 120 DEG C after mixing, soaking time 30min；After heat preservation
Obtain sulphur solution；
5) preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: near-infrared is added first into reaction vessel and vulcanizes silver content
Sub- point 0.1mmol, octadecylene 10mL and olaquindox 2mL, are stirred under vacuum conditions, and whipping temp is 60 DEG C, and mixing time is
20min uniformly under the conditions of argon gas, injects ytterbium solution 1ml into reaction vessel with the rate of 0.3mL/min, insulation reaction,
Reaction temperature is 220 DEG C, reaction time 30min, is injected again into reaction vessel with the rate of 0.3mL/min after completion of the reaction
Sulphur solution 1ml is carried out from growth sulphur shell reaction, and reaction temperature is 220 DEG C, reaction time 30min, from after growing the reaction of sulphur shell
With being centrifuged after acetone washing 5 times, gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping vulcanization silver content
Sub- point.
Comparison diagram 3 and Fig. 4, lanthanide rare ytterbium adulterate silver sulfide quantum dot compared to silver sulfide quantum dot, and size is more
Uniformly.And as shown in connection with fig. 5, the partial size of lanthanide rare ytterbium doping silver sulfide quantum dot is 2.8nm.As shown in fig. 6, silver sulfide
Quantum dot has absorption peak at 1080nm, as shown in fig. 7, lanthanide rare ytterbium, which adulterates silver sulfide quantum dot, has Yb in 920nm3+Ion
Absorption peak generate, it was demonstrated that Yb3+Effectively adulterated.
Embodiment 2
The preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, comprising the following steps:
1) preparation of presoma silver diethyldithiocarbamate: sodium oiethyl dithiocarbamate 25mmol is hydrated by three
It is dissolved in 50ml deionized water with silver nitrate 25mmol, the magnetic agitation under dark condition, reacts 3h, it after completion of the reaction, will
Reaction solution obtains product through centrifugal filtration, is distinguished washed product 6 times with water and dehydrated alcohol, washes clean is placed on 65 DEG C of baking ovens
In be dried to obtain presoma silver diethyldithiocarbamate.
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate 0.4mmol is dissolved in
In 25mL lauryl mercaptan, 10min is stirred, is uniformly mixed and obtains clear solution, hot defecation solution carries out anti-under the conditions of argon gas
It answers, reaction temperature is 200 DEG C, reaction time 2h, successively passes through centrifugal filtration, washing, drying after completion of the reaction, is obtained close red
Outer silver sulfide quantum dot.
3) preparation of ytterbium solution: acetic acid ytterbium 0.5g and olaquindox 2mL are stirred under vacuum conditions, whipping temp 100
DEG C, mixing time 20min, heat preservation, which is uniformly mixed, obtains ytterbium solution, and holding temperature is 120 DEG C, soaking time 30min.
4) preparation of sulphur solution: sulphur powder 0.2g and octadecylene 14mL are stirred under vacuum conditions, and whipping temp is 80 DEG C,
Mixing time is 20min, after mixing heating and thermal insulation, and holding temperature is 150 DEG C, soaking time 30min；It is obtained after heat preservation
Sulphur solution；
5) preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: near-infrared is added first into reaction vessel and vulcanizes silver content
Sub- point 0.2mmol, octadecylene 20mL and olaquindox 5mL, are stirred under vacuum conditions, and whipping temp is 80 DEG C, and mixing time is
20min under the conditions of argon gas, injects ytterbium solution 1ml, heat preservation into reaction vessel after mixing with the rate of 0.2mL/min
Reaction, reaction temperature is 220 DEG C, reaction time 30min, after completion of the reaction again into reaction vessel with the speed of 0.2mL/min
Rate injects sulphur solution 1ml and carries out growth sulphur shell reaction certainly, and reaction temperature is 220 DEG C, reaction time 30min, from growth sulphur shell
With being centrifuged after acetone washing 6 times after reaction, gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping sulphur
Change silver-colored quantum dot.
Embodiment 3
The preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, comprising the following steps:
1) preparation of presoma silver diethyldithiocarbamate: sodium oiethyl dithiocarbamate 25mmol is hydrated by three
It is dissolved in 40ml deionized water with silver nitrate 25mmol, the magnetic agitation under dark condition, reacts 3h, it after completion of the reaction, will
Reaction solution obtains product through centrifugal filtration, is distinguished washed product 5 times with water and dehydrated alcohol, washes clean is placed on 60 DEG C of baking ovens
In be dried to obtain presoma silver diethyldithiocarbamate.
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate 0.2mmol is dissolved in
In 20mL lauryl mercaptan, 10min is stirred, is uniformly mixed and obtains clear solution, hot defecation solution carries out anti-under the conditions of argon gas
It answers, reaction temperature is 200 DEG C, reaction time 2h, successively passes through centrifugal filtration, washing, drying after completion of the reaction, is obtained close red
Outer silver sulfide quantum dot.
3) preparation of ytterbium solution: acetic acid ytterbium 0.4g and olaquindox 1.8mL are stirred under vacuum conditions, and whipping temp is
100 DEG C, mixing time 30min, heat preservation, which is uniformly mixed, obtains ytterbium solution, and holding temperature is 150 DEG C, soaking time 30min.
4) preparation of sulphur solution: sulphur powder 0.30g and octadecylene 20mL are stirred under vacuum conditions, whipping temp 80
DEG C, mixing time 20min, heating and thermal insulation, holding temperature are 150 DEG C after mixing, soaking time 30min；After heat preservation
Obtain sulphur solution；
5) preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: near-infrared is added first into reaction vessel and vulcanizes silver content
Sub- point 0.2mmol, octadecylene 18mL and olaquindox 4mL, are stirred under vacuum conditions, and whipping temp is 100 DEG C, and mixing time is
20min under the conditions of argon gas, injects ytterbium solution 1ml, heat preservation into reaction vessel after mixing with the rate of 0.3mL/min
Reaction, reaction temperature is 220 DEG C, reaction time 30min, after completion of the reaction again into reaction vessel with the speed of 0.3mL/min
Rate injects sulphur solution 1ml and carries out growth sulphur shell reaction certainly, and reaction temperature is 220 DEG C, reaction time 30min, from growth sulphur shell
With being centrifuged after acetone washing 4 times after reaction, gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping sulphur
Change silver-colored quantum dot.
Embodiment 4
The preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, comprising the following steps:
1) preparation of presoma silver diethyldithiocarbamate: sodium oiethyl dithiocarbamate 23mmol is hydrated by three
It is dissolved in 45 deionized waters with silver nitrate 23mmol, the magnetic agitation under dark condition, reaction 3h after completion of the reaction will be anti-
It answers liquid to obtain product through centrifugal filtration, is distinguished washed product 5 times with water and dehydrated alcohol, washes clean is placed in 70 DEG C of baking ovens
It is dried to obtain presoma silver diethyldithiocarbamate.
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate 0.3mmol is dissolved in
In 10mL lauryl mercaptan, 10min is stirred, is uniformly mixed and obtains clear solution, hot defecation solution carries out anti-under the conditions of argon gas
It answers, reaction temperature is 210 DEG C, reaction time 3h, successively passes through centrifugal filtration, washing, drying after completion of the reaction, is obtained close red
Outer silver sulfide quantum dot.
3) preparation of ytterbium solution: acetic acid ytterbium 1g and olaquindox 3.6mL are stirred under vacuum conditions, whipping temp 120
DEG C, mixing time 20min, heat preservation, which is uniformly mixed, obtains ytterbium solution, and holding temperature is 180 DEG C, reaction time 60min.
4) preparation of sulphur solution: sulphur powder 0.32g and octadecylene 20mL are stirred under vacuum conditions, whipping temp 120
DEG C, mixing time 30min, heating and thermal insulation, holding temperature are 180 DEG C after mixing, soaking time 60min；After heat preservation
Obtain sulphur solution；
5) preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: near-infrared is added first into reaction vessel and vulcanizes silver content
Sub- point 0.1mmol, octadecylene 20mL and olaquindox 3mL, are stirred under vacuum conditions, and whipping temp is 120 DEG C, and mixing time is
30min under the conditions of argon gas, injects ytterbium solution 1ml, heat preservation into reaction vessel after mixing with the rate of 0.4mL/min
Reaction, reaction temperature is 200 DEG C, reaction time 60min, after completion of the reaction again into reaction vessel with the speed of 0.4mL/min
Rate injects sulphur solution 1ml and carries out growth sulphur shell reaction certainly, and reaction temperature is 200 DEG C, reaction time 60min, from growth sulphur shell
With being centrifuged after acetone washing 5 times after reaction, gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping sulphur
Change silver-colored quantum dot.
The embodiment of the present invention is described with above attached drawing, but the invention is not limited to above-mentioned specific
Embodiment, the above mentioned embodiment is only schematical, rather than restrictive, those skilled in the art
Under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, it can also make very much
Form, all of these belong to the protection of the present invention.
Claims (9)
1. a kind of preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot, the lanthanide rare ytterbium adulterate silver sulfide quantum dot
It is to adulterate Yb using silver sulfide quantum dot as matrix3+For active ions, heterogeneous sulphur layer is grown in silver sulfide quantum dot surface and is obtained；
The chemical formula of the lanthanide rare ytterbium doping silver sulfide quantum dot are as follows: Ag2S:Yb3+, which comprises the following steps:
1) preparation of presoma silver diethyldithiocarbamate: three hydration sodium oiethyl dithiocarbamates and silver nitrate are molten
Solution in deionized water, reacted by magnetic agitation, after completion of the reaction, is successively filtered, washed, is dried, obtain presoma
Silver diethyldithiocarbamate；
2) preparation of near-infrared silver sulfide quantum dot: presoma silver diethyldithiocarbamate is dissolved in lauryl mercaptan, is protected
Shield atmosphere enclose lower heating stirring be uniformly mixed obtain clear solution, hot defecation solution is reacted under the conditions of argon gas, reaction
After successively pass through centrifugal filtration, washing, drying, obtain near-infrared silver sulfide quantum dot；
3) preparation of ytterbium solution: under vacuum conditions after mixing evenly by acetic acid ytterbium and olaquindox, heat preservation is uniformly mixed and obtains ytterbium
Solution；
4) preparation of sulphur solution: under vacuum conditions after mixing evenly by sulphur powder and octadecylene, heat preservation obtains sulphur after mixing
Solution；
5) near-infrared silver sulfide quantum the preparation of lanthanide rare ytterbium doping silver sulfide quantum dot: is added first into reaction vessel
Point, octadecylene and olaquindox, stir evenly under vacuum conditions, and under the conditions of argon gas, ytterbium solution is injected into reaction vessel, is protected
Temperature reaction is injected sulphur solution into reaction vessel again after completion of the reaction and is carried out from growth sulphur shell reaction, from after growing the reaction of sulphur shell
Gained centrifugation product is dispersed in aniline solution and obtains lanthanide rare ytterbium doping silver sulfide quantum dot by washing, centrifugation.
2. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
Step 1), three hydration sodium oiethyl dithiocarbamates are 20~25mmol, silver nitrate is 20~25mmol, deionized water 40
~50mL, the magnetic agitation under dark condition, reaction time are that 2~3h after completion of the reaction obtains reaction solution through centrifugal filtration
Product is distinguished washed product 4~6 times with water and dehydrated alcohol, and washes clean, which is placed in baking oven, is dried to obtain presoma diethyl
Base thiocarbamic acid silver.
3. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
Step 2), presoma silver diethyldithiocarbamate are 0.2~0.4mmol, and lauryl mercaptan is 10~25mL, and mixing time is
10~20min；Reaction temperature is 200~220 DEG C, and the reaction time is 2~3h.
4. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
Step 3), acetic acid ytterbium are 0.4~1g, and olaquindox is 2~4mL；Whipping temp be 60~120 DEG C, mixing time be 20~
30min；Heat preservation mixing condition is, under the conditions of argon gas, holding temperature is 120~180 DEG C, and soaking time is 30~60min.
5. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
Step 4), 0.2~0.32g of sulphur powder, 10~20mL of octadecylene, whipping temp are 60~120 DEG C, and mixing time is 20~30min,
Holding temperature is 120~180 DEG C, and soaking time is 30~60min.
6. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
Step 5), 0.1~0.2mmol of near-infrared silver sulfide quantum dot, 2~5mL of 10~20mL of octadecylene and olaquindox, whipping temp
It is 60~120 DEG C, mixing time is 20~30min；The rate of ytterbium solution injection is 0.2~0.4mL/min, and reaction temperature is
200~220 DEG C, the reaction time is 30~60min；It is finally molten to reaction vessel injection sulphur with the rate of 0.2~0.4mL/min
Liquid, reaction temperature are 200~220 DEG C, and the reaction time is 30~60min.
7. the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 1, which is characterized in that described
The partial size that lanthanide rare ytterbium adulterates silver sulfide quantum dot is 10~20nm.
8. a kind of group of the lanthanides that the preparation method of lanthanide rare ytterbium doping silver sulfide quantum dot as described in claim 1 is prepared
Rare earth ytterbium adulterates silver sulfide quantum dot in the application as fluorescence labeling material.
9. lanthanide rare ytterbium doping silver sulfide quantum dot according to claim 8 is as fluorescence labeling material in living body biological
Application in imaging.
Priority Applications (1)
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