CN102952547A - Graphene and rare earth up-conversion fluorescent composite material and preparation method thereof - Google Patents
Graphene and rare earth up-conversion fluorescent composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene and rare earth up-conversion fluorescent composite material and a preparation method thereof. The method comprises the steps of: using a graphite powder as a raw material to prepare graphite oxide by a Hummer method; conducting ultrasonic dispersion on 5-85mg of graphite oxide into 24-60mL of water; then adding Y (NO3), Yb (NO3) and Er (NO3) in a total molar weight of 0.05-1mmol by a stoichiometric ration of 78:20:2 into the graphite oxide dispersion; adding 0.02-0.5g of NaF and stirring for 5-10min; transferring the mixture to a 100mL reactor; reacting for 4-24h at 200-240 DEG C; naturally cooling to room temperature; centrifuging for separation and washing the reaction product with deionized water twice to obtain a graphene and yttrium fluoride up-conversion fluorescent powder composite material, which comprises a mixture of two or three selected from the followings: graphene-YF3:Yb, Er; graphene-(alpha) NaYF4:Yb, Er; and graphene-(beta) NaYF4:Yb, Er. The method provided by the invention is simple, employs non-toxic raw materials, and can change type of the earth up-conversion fluorescent material and up-conversion fluorescence properties of a final composite material by simply adjusting conditions of a hydrothermal reaction.
Description
Technical field
What the present invention relates to is a kind of Graphene and rare earth up-conversion fluorescence matrix material.The present invention also relates to a kind of Graphene and rare earth up-conversion fluorescence composite manufacture method.
Background technology
Graphene has sp
2Therefore the monolayer carbon atomic structure of hydridization has advanced machinery, light and electrical properties.Found it is the study hotspot of material and biological technical field so far from 2004 always, especially exploring Graphene aspect the using value of physics, chemistry and biological field.At present, Graphene has been obtained impressive progress in the research of the aspects such as nanoelectronics, nano-sensor and nano-complex.Yet, how further to optimize Graphene and remain the problem of high care of researchist to satisfy it in the application of wide field more.
Optimize the quick and the most practical method of Graphene and be exactly the graphene-based matrix material that Graphene and the compound preparation of other materials is more advanced.This matrix material possesses the excellent properties of bi-material simultaneously, and is functional stronger, so range of application is wider, such as in fields such as sensor, solar cell, transistor and biochips.Yet the hydrophobicity of Graphene self has limited its application in the aqueous solution on the one hand, has also improved on the other hand the difficulty of compound other functional materialss.The simplest solution utilizes its oxidation of precursor graphite as matrix exactly.Graphite oxide not only possesses the monolayer carbon atomic sheet structure of Graphene, and has a large amount of hydroxyls and epoxy group(ing) on its surface, is easy to compound other functional materialss.Therefore, present graphene-based matrix material is as substrate material mostly with graphite oxide.
At present, the graphene-based matrix material of having reported has Graphene-metal composite, Graphene-magnetic oxide matrix material and Graphene-fluorescent material matrix material etc., wherein, Graphene-fluorescent material based composites is because its broad prospect of application in photochemical catalysis and optics amplitude limit field has caused our concern.The rare earth upconverting fluorescent material is with its large Stokes shift, narrow emmission spectrum, long fluorescence lifetime, high chemistry/photochemical stability, hypotoxicity and infraredly show one's talent in numerous fluorescent materials to unique advantages such as excited by visible light, becomes the first-selection of fluorescent material.Though this respect research is arranged at present, and the photoluminescent property of the matrix material that regrettably obtains is all very poor.
To sum up, the research of the Graphene of the rare earth upconverting fluorescent material that the systematic study functionalization is different classes of-fluorescent material matrix material was not also reported, scheme or the route that in addition, can prepare Graphene with good up-conversion fluorescence character-rare earth up-conversion fluorescence matrix material were not reported yet.
Summary of the invention
The object of the present invention is to provide a kind of have good up-conversion fluorescence character Graphene and rare earth up-conversion fluorescence matrix material.The present invention also aims to provide that a kind of process is simple, Graphene and the rare earth up-conversion fluorescence composite manufacture method of advantages of nontoxic raw materials.
The object of the present invention is achieved like this:
Formation and the chemical expression of Graphene of the present invention and rare earth up-conversion fluorescence matrix material are: Graphene-YF
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er or Graphene-(β)
4: Yb, Er, "-" presentation function wherein, ": " expression is mixed, " α " expression α phase, " β " expression β phase.
Graphene of the present invention and rare earth up-conversion fluorescence composite manufacture method are:
(1) adopts the standby graphite oxide of Hummer legal system take Graphite Powder 99 as raw material;
(2) with 5～85mg graphite oxide ultra-sonic dispersion in 24～60mL water, be the Y (NO of 0.05～1mmol again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.02～0.5g NaF, after stirring 5～10min, transfer in the 100mL reactor, 200～240 ° of C reaction 4-24h naturally cool to room temperature, and centrifugation is also used the deionized water washed twice, then obtain the matrix material of the fluorochemical up-conversion phosphor of Graphene and yttrium, comprise Graphene-YF
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er, Graphene-(β)
4: Yb, the mixture of one or both among the Er or three kinds, "-" presentation function wherein, ": " expression is mixed, " α " expression α phase, " β " expression β phase.
In 24mL water, be the Y (NO of 1mmol with 65～85mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.76～1.0g Trisodium Citrate, after stirring 5min, add 24mL ethanol, drip volume ratio that 24mL is dissolved with the water of 0.3～0.5gNaF and ethanol under the intense agitation and be 1 solution, regulate pH value to 3, transfer in the 100mL reactor, 240 ° of C reaction 4h obtain mutually NaYF of Graphene and β
4: Yb, the matrix material of Er fluorescent material is expressed as the NaYF of Graphene-(β)
4: Yb, Er.
In 60mL water, be the Y (NO of 0.05mmol with 5～7mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.02～0.2g NaF, after stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h naturally cool to room temperature, and centrifugation is also used the deionized water washed twice, then obtain the matrix material of the fluorochemical up-conversion phosphor of Graphene and yttrium, comprise Graphene-YF
3: Yb, the NaYF of Er and Graphene-(α)
4: Yb, Er.
The present invention adopts hydrothermal method to prepare three kinds of Graphenes-rare earth up-conversion fluorescence matrix material, comprises Graphene-YF
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er and Graphene-(β)
4: Yb, Er.This method has following features, the one, in the hydrothermal reaction process, when graphite oxide is reduced to Graphene, with different classes of rare earth up-conversion fluorescence particle functionalization to grapheme material; The 2nd, this hydrothermal method process is simple, advantages of nontoxic raw materials, can be by the simple hydrothermal reaction condition of adjusting respectively with YF
3: Yb, Er, α phase NaYF
4: Yb, Er and β be NaYF mutually
4: Yb, three kinds of different rare earth up-conversion fluorescence particles of Er evenly are compound on the grapheme material; The 3rd, can by changing the classification of rare earth upconverting fluorescent material, adjust the up-conversion fluorescence character of final matrix material.The method and design route than other method have stable reaction conditions, convenient, composite particles is uniformly dispersed and purity is high and the characteristics such as environmental protection, the most important thing is, final optimization pass obtains the NaYF of Graphene-(β)
4: Yb, Er in the Er matrix material
3+Upper up-conversion emission intensity the highest in similar Graphene-fluorescent material matrix material at present.Its specific solution, optimum result and theoretical versatility still belong to blank at home and abroad.Matrix material of the present invention sends strong up-conversion fluorescence (comparing with light functionalization graphene matrix material) under the 980nm exciting light, have a extensive future in photochemical catalysis and optics amplitude limit field.
Description of drawings
Fig. 1 (a) is the XRD figure of graphite oxide, and Fig. 1 (b) is the SEM photo of graphite oxide.
Fig. 2 is that embodiment () utilizes the graphite oxide hydro-thermal to prepare Graphene-YF
3: Yb, the process schematic diagram of Er matrix material.
Curve among Fig. 3 (a), (b) and (c) be respectively product Graphene-YF of embodiment () (two) and (three)
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er and Graphene-(β)
4: Yb, the XRD figure of Er; JCPDS 32-1431 and JCPDS16-0334 are respectively YF
3With β NaYF mutually
4: Yb, the standard card of Er.
Fig. 4 (a)-Fig. 4 (b), Fig. 4 (c)-Fig. 4 (d) and Fig. 4 (e)-Fig. 4 (f) is respectively product Graphene-YF of embodiment () (two) and (three)
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er and Graphene-(β)
4: Yb, the SEM of Er and TEM photo; Wherein Fig. 4 (f) is for being compound in the β phase NaYF on the Graphene
4: Yb, the high resolution TEM photo of Er.
Fig. 5 (a) is embodiment (two) and (threes') the NaYF of product Graphene-(α)
4: Yb, the NaYF of Er and Graphene-(β)
4: Yb, the upper inversion spectrum figure of Er matrix material; Fig. 5 (b) is NaYF
4: Yb, the upper switching mechanism figure of Er.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention and effect are further described.But employed concrete grammar, prescription and explanation are not limitation of the present invention.
Embodiment (one):
Graphite oxide adopts the Hummer legal system standby take Graphite Powder 99 as raw material, as compound raw material of lower step, and material as a comparison.In 60mL water, be the Y (NO of 0.05mmol with 5.9mg graphite oxide ultra-sonic dispersion with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add 0.025g NaF, behind the stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h.Naturally cool to room temperature, centrifugation is also used the deionized water washed twice, then obtains Graphene and fluorescent material YF
3: Yb, the matrix material of Tm is expressed as Graphene-YF
3: Yb, Er, "-" presentation function wherein, ": " expression is mixed wherein, " α " expression α phase.
Embodiment (two):
In 60mL water, be the Y (NO of 0.05mmol with 5.9mg graphite oxide ultra-sonic dispersion with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add 0.108g NaF, behind the stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h.Naturally cool to room temperature, centrifugation and use the deionized water washed twice then obtains mutually NaYF of Graphene and fluorescent material α
4: Yb, the matrix material of Er is expressed as the NaYF of Graphene-(α)
4: Yb, Er.
Embodiment (three):
In 24mL water, be the Y (NO of 1mmol with 75mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add the 0.8823g Trisodium Citrate, behind the stirring 5min, add 24mL ethanol, drip water and ethanol (volume ratio the is 1) solution that 24mL is dissolved with 0.42gNaF under the intense agitation.Regulate pH value to 3, transfer in the 100mL reactor, 240 ° of C reaction 4h.Obtain mutually NaYF of Graphene and β
4: Yb, the matrix material of Er fluorescent material is expressed as the NaYF of Graphene-(β)
4: Yb, Er.
Embodiment (four):
In 60mL water, be the Y (NO of 0.05mmol with 5mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add 0.02g NaF, behind the stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h.Naturally cool to room temperature, centrifugation is also used the deionized water washed twice, then obtains the fluorochemical up-conversion fluorescence powder composite material of Graphene and yttrium.
Embodiment (five):
In 60mL water, be the Y (NO of 0.05mmol with 7mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add 0.2g NaF, behind the stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h.Naturally cool to room temperature, centrifugation is also used the deionized water washed twice, then obtains the fluorochemical up-conversion fluorescence powder composite material of Graphene and yttrium.
Embodiment (six):
In 24mL water, be the Y (NO of 1mmol with 65mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add the 0.76g Trisodium Citrate, behind the stirring 5min, add 24mL ethanol, drip water and ethanol (volume ratio the is 1) solution that 24mL is dissolved with 0.3gNaF under the intense agitation.Regulate pH value to 3, transfer in the 100mL reactor, 240 ° of C reaction 4h.Obtain the fluorochemical up-conversion fluorescence powder composite material of Graphene and yttrium.
Embodiment (seven):
In 24mL water, be the Y (NO of 1mmol with 85mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the above-mentioned graphite oxide dispersion with stoichiometric ratio 78:20:2.Add the 1.0g Trisodium Citrate, behind the stirring 5min, add 24mL ethanol, drip water and ethanol (volume ratio the is 1) solution that 24mL is dissolved with 0.5gNaF under the intense agitation.Regulate pH value to 3, transfer in the 100mL reactor, 240 ° of C reaction 4h.Obtain the fluorochemical up-conversion fluorescence powder composite material of Graphene and yttrium.
Claims (4)
1. a Graphene and rare earth up-conversion fluorescence matrix material is characterized in that: be Graphene-YF
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er or Graphene-(β)
4: Yb, a kind of or its mixture among the Er, "-" presentation function wherein, ": " expression is mixed, " α " expression α phase, " β " expression β phase.
2. a Graphene and rare earth up-conversion fluorescence composite manufacture method is characterized in that:
(1) adopts the standby graphite oxide of Hummer legal system take Graphite Powder 99 as raw material;
(2) with 5～85mg graphite oxide ultra-sonic dispersion in 24～60mL water, be the Y (NO of 0.05～1mmol again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.02～0.5g NaF, after stirring 5～10min, transfer in the 100mL reactor, 200～240 ° of C reaction 4-24h naturally cool to room temperature, and centrifugation is also used the deionized water washed twice, then obtain the matrix material of the fluorochemical up-conversion phosphor of Graphene and yttrium, comprise Graphene-YF
3: Yb, the NaYF of Er, Graphene-(α)
4: Yb, the NaYF of Er, Graphene-(β)
4: Yb, the mixture of one or both among the Er or three kinds, "-" presentation function wherein, ": " expression is mixed, " α " expression α phase, " β " expression β phase.
3. Graphene according to claim 2 and rare earth up-conversion fluorescence composite manufacture method is characterized in that: in 24mL water, be the Y (NO of 1mmol with 65～85mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.76～1.0g Trisodium Citrate, after stirring 5min, add 24mL ethanol, drip volume ratio that 24mL is dissolved with the water of 0.3～0.5g NaF and ethanol under the intense agitation and be 1 solution, regulate pH value to 3, transfer in the 100mL reactor, 240 ° of C reaction 4h obtain mutually NaYF of Graphene and β
4: Yb, the matrix material of Er fluorescent material is expressed as the NaYF of Graphene-(β)
4: Yb, Er.
4. Graphene according to claim 2 and rare earth up-conversion fluorescence composite manufacture method is characterized in that: in 60mL water, be the Y (NO of 0.05mmol with 5～7mg graphite oxide ultra-sonic dispersion again with integral molar quantity
3), Yb (NO
3) and Er (NO
3) add in the graphite oxide dispersion with stoichiometric ratio 78:20:2, add 0.02～0.2g NaF, after stirring 10min, transfer in the 100mL reactor, 200 ° of C reaction 24h naturally cool to room temperature, and centrifugation is also used the deionized water washed twice, then obtain the matrix material of the fluorochemical up-conversion phosphor of Graphene and yttrium, comprise Graphene-YF
3: Yb, the NaYF of Er and Graphene-(α)
4: Yb, Er.
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