CN108753297B - A kind of method inside noble metal nano particles insertion rear-earth-doped luminous material - Google Patents
A kind of method inside noble metal nano particles insertion rear-earth-doped luminous material Download PDFInfo
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- CN108753297B CN108753297B CN201810543518.8A CN201810543518A CN108753297B CN 108753297 B CN108753297 B CN 108753297B CN 201810543518 A CN201810543518 A CN 201810543518A CN 108753297 B CN108753297 B CN 108753297B
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/779—Halogenides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/779—Halogenides
- C09K11/7791—Halogenides with alkali or alkaline earth metals
Abstract
The invention discloses the methods inside a kind of noble metal nano particles insertion rear-earth-doped luminous material, utilize the fuel factor of noble metal nano structure phasmon, using the big small size noble metal nano particles of absorption cross-section as heat source, so that it is generated high heat in a very short period of time by the effect of additional light field, realize noble metal nano particles fast growth and is embedded in inside rear-earth-doped luminous material.The present invention not only considerably increases the effective range of noble metal nano particles surface phasmon, the scattering section of noble metal nano particles is increased simultaneously, phasmon is greatly improved to the regulation efficiency of system fluorescent radiation, realizes the Effective Regulation to material emission performance.Reaction time of the invention is short, required excitation light power density is small, and there is wavelength-dependent behavior, by adjusting the position at noble metal granule plasmon resonance peak, the linear adjustable of excitation wavelength can be achieved, the crystallinity of luminescent material also gets a promotion simultaneously, has advanced optimized its fluorescent emission performance.
Description
Technical field
The invention belongs to rare earth ion doped phosphor preparation technical fields, and in particular to a kind of noble metal is received
Rice grain is embedded in the method inside rear-earth-doped luminous material.
Background technique
There is rare earth ion doped phosphor unique electron configuration and level structure abundant to impart it
The optical characteristics for many brilliances such as spectral line is sharp keen, transmitting band is abundant, background fluorescence is low and fluorescence lifetime is long, is widely used in
The fields such as bio-imaging, medical diagnosis and therapy, solar battery, photocatalysis, LED imaging, biological coding, optical storage.But
Since transition many in rare earth ion belong to the f-f transition of parity forbidden, corresponding absorption cross-section and emission effciency still compare
It is lower, and interfering with each other between the rare earth ion fluorescent radiation band of part often limits wherein a certain special fluorescent radiation band
Effective use.For example, the fluoride nano granule that trivalent ytterbium ion and erbium ion are co-doped with is used for bio-imaging or biology volume
When code, to overcome strong absorption of the biological tissue to fluorescence in visible-range, high contrast, highly sensitive imaging and volume are realized
Code, needs inhibition system Green fluorescent radiation, and improve its red or near-infrared fluorescent emissive porwer (Bai, Z, Lin, H,
Johnson, J, Journal of Materials Chemistry C, 2014,2 (9): 1736-1741.).Therefore, reinforcement
The fluorescent radiation intensity of rare earth ion in being, while regulating and controlling the relative intensity of rare earth ion fluorescent emission band, Lai Shixian rare earth is mixed
The problem of effective application of miscellaneous luminescent material is present material scientific domain urgent need to resolve.
There is noble metal nano structure unique optical property can generate table under the excitation of the outer light field of certain wavelength
Face plasmon resonance.Using noble metal nano body structure surface phasmon, this characteristic be may be implemented to luminescent material fluorescence spy
The Effective Regulation of property.It is to pass through noble metal nano in research of the noble metal nano structure to rear-earth-doped system fluorescence regulation and control
Direct effect between structure and rear-earth-doped luminous material is to realize fluorescence regulation and control.Zeng etc. is in gold nanorods and individually
NaYF4:Yb3+/Er3+/Mn2+In the compound system of nano particle, by adjusting gold nanorods size and draw ratio realize it is glimmering
Photoemissive Effective Regulation, and realize more than ten times of fluorescence enhancement (Yingxian Xue, Chengjie Ding, Heping
Zeng,Small,2017,13(36):1701155.).Schietinger etc. is to exclude interparticle interference, and first observed arrives
The single NaYF of excitation and transmitting enhancing while contribution4:Yb3+,Er3+The up-conversion luminescence of nano particle enhances
(S.Schietinger,T.Aichele,H.Q.Wang,T.Nairn,0.Benson,Nano Lett.,2010,10(1):134-
138.).But due to the EFFECTIVE RANGE very little of noble metal nano particles LSP, usually only more than ten nanometers, this is just significantly
Phasmon is reduced to the regulation efficiency of rare earth luminescent material, this is the problem of the field all the time.Particularly with sub-micro
For meter level or micron-sized rare earth particle, research method general at present is that noble metal nano particles are adhered to rare earth particle
Surface, or rare earth particle is placed in the noble metal substrate surface of self assembly.These methods can only realize phasmon to rare earth
Regulation within the scope of grain surface nanoscale, and effect is had no for most of light emitting ionics inside particle, this allows for table
Face phasmon is very low to the regulation efficiency of system fluorescent radiation.
Summary of the invention
It is an object of the invention to overcome above-mentioned problems of the prior art, a kind of general easy to operate, quick is provided
Noble metal nano particles are embedded in the method inside rear-earth-doped luminous material, to increase having for noble metal nano particles phasmon
Sphere of action is imitated, to greatly promote phasmon to the regulation efficiency of system fluorescent radiation, is realized to rare earth material photism
The Effective Regulation of energy.
For above-mentioned purpose, the technical solution adopted in the present invention is made of following step:
1, noble metal nano particles coat rear-earth-doped luminous material
Rear-earth-doped luminous material is added in deionized water, and reducing agent is added, room temperature ultrasound 5~after twenty minutes, add
Heat adds silane coupling agent to 60~90 DEG C, is continuously heating to 90~100 DEG C, and the expensive gold of 0.01~0.1mol/l is then added
Belong to the aqueous solution of soluble-salt, isothermal reaction 10~30 minutes, natural cooling, centrifugation, washing, drying obtained cladding noble metal
The rear-earth-doped luminous material of nano particle.
2, inside noble metal nano particles insertion rear-earth-doped luminous material
The rear-earth-doped luminous materials of noble metal nano particles will be coated with laser irradiation 2 seconds~20 minutes, optical maser wavelength
It is coupled with the wavelength at noble metal nano particles plasmon resonance peak, laser power density is 1.7 × 103~4.0 × 104W/
cm2, increase noble metal nano particles partial size and be embedded in inside rear-earth-doped luminous material.
Above-mentioned rear-earth-doped luminous material is YF3:RE3+Submicron crystal, LaF3:RE3+Submicron crystal NaYF4:RE3+
Submicron crystal, NaYbF4:RE3+Submicron crystal, NaGdF4:RE3+Submicron crystal, NaLaF4:RE3+Appoint in submicron crystal
It anticipates one kind, wherein RE3+It is any one in lanthanide ion or two.
In above-mentioned steps 1, preferably quality-volume ratio of rear-earth-doped luminous material and deionized water is 1mg:1~3mL,
The molar ratio of rear-earth-doped luminous material and precious metal soluble salt, reducing agent, silane coupling agent is 1:(0.06~0.3): (20
~50): (0.3~1.5).
Above-mentioned precious metal soluble salt is gold chloride, silver chlorate, any one in silver nitrate.
Above-mentioned reducing agent is trisodium citrate, citric acid, ascorbic acid, oxalic acid, sodium borohydride, any one in ethylene glycol
Kind.
Above-mentioned silane coupling agent is 3- aminopropyl trimethoxy siloxane, (methacryloxypropyl) propyl trimethoxy silicon
Any one in alkane, vinyltriethoxysilane.
In above-mentioned steps 2, preferably laser power density is 1.0~2.0 × 104W/cm2, laser irradiation time is 2~10
Second.
Beneficial effects of the present invention are as follows:
1, the present invention utilizes the fuel factor of noble metal nano structure phasmon, with the big small size noble metal of absorption cross-section
Nano particle is heat source, and under the irradiation of laser, noble metal nano particles generate local surface plasmon resonance, by energy office
The quick raising of noble metal nano particles temperature is brought, finally makes noble metal nano particles each other near particle surface in domain
Between merge, recrystallize and be grown to the biggish nano particle of partial size and partial particulate can be embedded in the interior of rear-earth-doped luminous material
Portion.The increase of metallic particles partial size, brings the increase of scattering section Yu absorption cross-section ratio, to be more advantageous to noble metal granule
Enhancing and regulation to rare earth material fluorescent emission.Noble metal nano particles are embedded in inside rear-earth-doped luminous material, are increased expensive
The sphere of action of metallic particles and rare earth luminous ion, to enhance phasmon to the regulation efficiency of fluorescent emission.It crosses herein
Cheng Zhong can make the partial size of rear-earth-doped luminous material reduce, crystallinity is mentioned due to the fuel factor of noble metal nano particles
It rises.
2, the reaction time of the invention is short, it is only necessary to millisecond can be completed, and required excitation light power density is small, and have wavelength according to
Rely characteristic, by adjusting noble metal granule plasmon resonance peak position, it can be achieved that excitation wavelength it is linear adjustable.By
The effect of phasmon fuel factor, the crystallinity of rear-earth-doped luminous material can also get a promotion, and further increase rear-earth-doped
The fluorescent emission performance of luminescent material.
3, the present invention not only considerably increases the effective range of noble metal nano particles surface phasmon, also simultaneously
The scattering section of noble metal nano particles is increased, the crystallinity of luminescent material is improved, to realize phasmon to system
The Effective Regulation of fluorescent radiation regulation efficiency greatly promoted with rare earth particle light-emitting performance.
Detailed description of the invention
Fig. 1 is YF prepared by embodiment 13:Eu3+The SEM of@Au submicron crystal schemes.
Fig. 2 is YF prepared by embodiment 13:Eu3+The TEM and STEM of@Au submicron crystal scheme.
Fig. 3 is YF prepared by embodiment 13:Eu3+SEM figure of the@Au submicron crystal after laser irradiation.
Fig. 4 is YF prepared by embodiment 13:Eu3+TEM figure of the@Au submicron crystal after laser irradiation.
Fig. 5 is YF prepared by embodiment 13:Eu3+TEM of the@Au submicron crystal after laser irradiation marks figure.
Fig. 6 is YF prepared by embodiment 23:Eu3+SEM figure of the@Au submicron crystal after laser irradiation.
Fig. 7 is YF prepared by embodiment 23:Eu3+TEM figure of the@Au submicron crystal after laser irradiation.
Fig. 8 is YF prepared by embodiment 23:Eu3+TEM of the@Au submicron crystal after laser irradiation marks figure.
Fig. 9 is NaYF prepared by embodiment 34:Eu3+The SEM of@Au submicron crystal schemes.
Figure 10 is NaYF prepared by embodiment 34:Eu3+The TEM of@Au submicron crystal schemes.
Figure 11 is NaYF prepared by embodiment 34:Eu3+SEM figure of the@Au submicron crystal after laser irradiation.
Figure 12 is NaYF prepared by embodiment 34:Eu3+TEM figure of the@Au submicron crystal after laser irradiation.
Figure 13 is NaYF prepared by embodiment 34:Eu3+TEM of the@Au submicron crystal after laser irradiation marks figure.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1, Au nano particle coats YF3:Eu3+Submicron crystal
0.95mL 0.5mmol/L Y (NO is added into 60mL deionized water3)3Aqueous solution and 0.05mL 0.5mmol/L
Eu(NO3)3Aqueous solution, 3mL 0.5mmol/L NaF aqueous solution, in 75 DEG C of environment, isothermal reaction 2 hours, natural cooling, successively
With deionized water and dehydrated alcohol centrifuge washing, 60 DEG C drying 10 hours, obtain YF3:Eu3+Submicron crystal.By 0.03g
(0.2mmol)YF3:Eu3+Submicron crystal is added in 40mL deionized water, and 1.4g (7.2mmol) trisodium citrate, room is added
Warm ultrasound after ten minutes, is warming up to 70 DEG C, and 30 μ L (0.167mmol) 3- aminopropyl trimethoxy siloxanes are added, continue to heat up
To 90 DEG C, 3mL 0.01mol/L aqueous solution of chloraurate is then added, isothermal reaction 15 minutes, natural cooling successively used deionization
Water and dehydrated alcohol centrifuge washing, 60 DEG C drying 10 hours, obtain Au nano particle cladding YF3:Eu3+Submicron crystal, i.e.,
YF3:Eu3+@Au submicron crystal.It can be seen from fig. 1 and fig. 2 that the partial size of Au nano particle is about 8~10nm, it is uniform and close
Collection is adhered to YF3:Eu3+Submicron particles surface.
2, Au nano particle is embedded in YF3:Eu3+Inside submicron particles
By YF3:Eu3+@Au submicron crystal with laser irradiation 5 seconds, optical maser wavelength be 532nm (with Au nano particle etc. from
The wavelength at plasmon resonance peak couples), laser power density is 1.5 × 104W/cm2.Gained sample is through scanning electron microscope and transmission electron microscope
Characterization, one of YF3:Eu3+The front and back sides SEM characterization result of@Au submicron particles is shown in that Fig. 3, TEM characterization result are shown in Fig. 4.It will
SEM and TEM characterization result compares, and discovery part Au nano particle is embedded in YF3:Eu3+Inside submicron particles (see figure
Circle marks part in 5), and the partial size of Au nano particle increases to 20~80nm.
Embodiment 2
In the present embodiment, by YF3:Eu3+For@Au submicron crystal with laser irradiation 5 seconds, optical maser wavelength was that 532nm (receives with Au
The wavelength at rice grain plasmon resonance peak couples), laser power density is 2 × 103W/cm2, other steps and 1 phase of embodiment
Together.By Fig. 6~8 as it can be seen that part Au nano particle is embedded in YF3:Eu3+Inside submicron particles, embedded in internal part Au
Nano particle is marked with circle (see Fig. 8), and the partial size of Au nano particle increases to 20~80nm.
Embodiment 3
1, Au nano particle coats NaYF4:Eu3+Submicron crystal
0.95mL 0.5mmol/L Y (NO is added into 60mL deionized water3)3Aqueous solution and 0.05mL 0.5mmol/L
Eu(NO3)3Aqueous solution, 7mL 0.5mmol/L NaF aqueous solution, stir after sixty minutes at room temperature, are warming up to 75 DEG C, isothermal reaction 2
Hour, natural cooling, successively use deionized water and dehydrated alcohol centrifuge washing, 60 DEG C drying 10 hours, obtain NaYF4:Eu3+It is sub-
Micro-crystal.By 0.03g (0.16mmol) NaYF4:Eu3+Submicron crystal is added in 40mL deionized water, and 1.4g is added
(7.28mmol) trisodium citrate, room temperature ultrasound after ten minutes, are warming up to 70 DEG C, 30 μ L (0.167mmol) 3- aminopropyls are added
Trimethoxy siloxane is continuously heating to 90 DEG C, and 3mL 0.01mol/L aqueous solution of chloraurate is then added, and isothermal reaction 15 divides
Clock, natural cooling, successively use deionized water and dehydrated alcohol centrifuge washing, 60 DEG C drying 10 hours, obtain NaYF4:Eu3+@Au
Submicron crystal.As can be seen that the partial size of Au nano particle is about 8~10nm from Fig. 9 and 10, uniform and intensive is adhered to
NaYF4:Eu3+The surface of submicron particles.
2, Au nano particle is embedded in NaYF4:Eu3+Inside submicron particles
By NaYF4:Eu3+For submicron particles with laser irradiation 3 seconds, optical maser wavelength was 532nm (with Au nano particle etc. from swashing
The wavelength of first formant couples), laser power density is 1.5 × 104W/cm2.Gained sample is through scanning electron microscope and transmission electron microscope table
Sign, one of NaYF4:Eu3+The front and back sides SEM characterization result of submicron particles is shown in that Figure 11, TEM characterization result are shown in Figure 12.It will
SEM and TEM characterization result compares, and discovery part Au nano particle is embedded in YF3:Eu3+Inside submicron particles (see figure
Circle marks part in 13), and the partial size of Au nano particle increases to 20~90nm.
Claims (4)
1. a kind of method inside noble metal nano particles insertion rear-earth-doped luminous material, it is characterised in that this method is by following
Step composition:
(1) noble metal nano particles coat rear-earth-doped luminous material
Rear-earth-doped luminous material is added in deionized water, and reducing agent is added, room temperature ultrasound 5~after twenty minutes, it is heated to
60~90 DEG C, silane coupling agent is added, is continuously heating to 90~100 DEG C, 0.01~0.1mol/l noble metal then is added can
The aqueous solution of soluble, isothermal reaction 10~30 minutes, natural cooling, centrifugation, washing, drying obtained cladding noble metal nano
The rear-earth-doped luminous material of particle;
Above-mentioned rear-earth-doped luminous material is YF3:RE3+Submicron crystal, LaF3:RE3+Submicron crystal, NaYF4:RE3+It is sub-
Micro-crystal, NaYbF4:RE3+Submicron crystal, NaGdF4:RE3+Submicron crystal, NaLaF4:RE3+It is any in submicron crystal
One kind, wherein RE3+It is any one in lanthanide ion or two;
Above-mentioned precious metal soluble salt is gold chloride, and reducing agent is trisodium citrate, and silane coupling agent is 3- aminopropyl front three
Oxygroup siloxanes;
(2) inside noble metal nano particles insertion rear-earth-doped luminous material
The rear-earth-doped luminous materials of noble metal nano particles will be coated with laser irradiation 2 seconds~20 minutes, optical maser wavelength is
532nm, laser power density are 1.7 × 103~4.0 × 104W/cm2, increase noble metal nano particles partial size and be embedded in rare earth
Inside doped luminescent material.
2. the method inside noble metal nano particles insertion rear-earth-doped luminous material according to claim 1, feature
Be: in step (1), quality-volume ratio of the rear-earth-doped luminous material and deionized water is 1mg:1~3mL.
3. the method inside noble metal nano particles insertion rear-earth-doped luminous material according to claim 1, feature
It is: in step (1), the molar ratio of the rear-earth-doped luminous material and precious metal soluble salt, reducing agent, silane coupling agent
For 1:(0.06~0.3): (20~50): (0.3~1.5).
4. the method inside noble metal nano particles insertion rear-earth-doped luminous material according to claim 1, feature
Be: in step (2), laser power density is 1.0~2.0 × 104W/cm2, laser irradiation time is 2~10 seconds.
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CN102127444A (en) * | 2010-12-10 | 2011-07-20 | 吉林大学 | Nanogold modified enhanced up-conversion luminescence composite material and preparation method thereof |
CN107298974A (en) * | 2016-09-21 | 2017-10-27 | 华东师范大学 | A kind of quantum dot Core-shell Composite Particles of multilayer parcel and its preparation method and application |
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