CN104371725A - Preparation method of NaYF4:Yb/Er-MoS2 conjugate - Google Patents
Preparation method of NaYF4:Yb/Er-MoS2 conjugate Download PDFInfo
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- CN104371725A CN104371725A CN201410580842.9A CN201410580842A CN104371725A CN 104371725 A CN104371725 A CN 104371725A CN 201410580842 A CN201410580842 A CN 201410580842A CN 104371725 A CN104371725 A CN 104371725A
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Abstract
The invention relates to a preparation method of a NaYF4:Yb/Er-MoS2 conjugate, which comprises the following steps: (1) mixing MoS2 with an organic solvent, sealing, and oscillating to obtain a MoS2-organic solvent suspension solution; (2) sealing the MoS2-organic solvent suspension solution, centrifuging, and taking out the longitudinal middle layer solution to obtain a MoS2 nano/micro fragment solution; and (3) adding NaYF4:Yb/Er into the MoS2 nano/micro fragment solution, sealing, and oscillating to obtain the NaYF4:Yb/Er-MoS2 conjugate suspension solution. The method is simple and easy to implement, low in cost and convenient for mass industrial production. The prepared NaYF4:Yb/Er-MoS2 conjugate has better optical limiting property than MoS2 in the visible waveband, has better optical limiting property than NaYF4:Yb/Er rare-earth nanoparticles in the near-infrared waveband, and can be used for laser protection.
Description
Technical field
The present invention relates to a kind of rare earth and MoS
2the preparation method of binding substances, is specifically related to a kind of NaYF
4: Yb/Er-MoS
2receive the preparation method of micro-fragment binding substances.
Background technology
In present stage, optics uses and extend to near-infrared band, infrared laser technology is ripe and militarily utilization is extensive, as range finder using laser, laser target designator, lidar, laser guidance and blinding laser weapons etc., all can temporarily blinding human eye or interference, destruction equipment photo-sensor, constitute a serious threat.So the material that research and manufacture carry out optical Limiting to near-infrared laser is necessary, the optical limitation of material can be utilized to protect eyes and device from laser hazard.
At infrared band, upper conversion rare earth nano material is as NaYF
4: Yb/Er has very strong linear absorption and non-linear absorption, i.e. optical Limiting, but owing to there is numerous transition patterns in the 4f shell of its ion, if district is excited at infrared light, the visible ray that wavelength is less than exciting light can be launched, so can be restricted in some application, and it is very little in visible waveband linear absorption; At visible waveband, Graphene and MoS
2etc. two-dimensional material, there is good linear absorption and non-linear absorption, i.e. optical Limiting, but absorb very little near infrared low light intensity lower linear.Therefore, a kind of material having good nonlinear optical limiting characteristic at visible and near-infrared band is needed.
At present, the people such as Wei Wei, Tingchao He has successfully prepared graphene oxide and rare earth NaYF
4: Yb/Er nano composite material, its optical limiting property at infrared band is remarkable, but little in visible waveband graphene oxide and its matrix material optical Limiting difference.MoS
2solution wavelength selectivity optical limitation research (Wang Yuanqian, He Jun etc. Acta Physica Sinica, 2014,63 (14): 144204) in describe MoS
2nano micro-material also has optical limiting property, but does not relate to MoS
2the preparation of matrix material, although the MoS of preparation
2nano micro-material has certain light amplification characteristic under little light intensity, but is not suitable in lasing safety.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of in visible waveband and near-infrared band optical limiting property excellence, can be used for the NaYF of lasing safety
4: Yb/Er-MoS
2the preparation method of binding substances.
The technical solution adopted for the present invention to solve the technical problems is as follows: NaYF
4: Yb/Er-MoS
2the preparation method of binding substances, comprises the following steps:
(1) by MoS
2mix with organic solvent, sealing, vibration 1.5 ~ 2.5h, obtains MoS
2-organic solvent aaerosol solution;
(2) by step (1) gained MoS
2-organic solvent aaerosol solution seals, centrifugal, pipettes centrifugal rear longitudinal middle level solution, obtains the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution;
(3) in step (2) gained width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add rare earth NaYF
4: Yb/Er, sealing, vibration 1.5 ~ 2.5h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
Further, in step (1), in often liter of organic solvent, MoS is added
2amount be 2 ~ 3g.
Further, in step (1), described organic solvent is ethanol, tetrahydrofuran (THF), N-Methyl pyrrolidone or DMF.
Further, in step (2), the amount of pipetting of described longitudinal middle level solution is 25 ~ 35% of centrifugal rear suspension liquor capacity.
Further, in step (3), often rise in step (2) gained the MoS that width is 10 ~ 15 μm
2receive in micro-fragment solution and add NaYF
4: the amount of Yb/Er is 2 ~ 3g.
Further, in step (1) and (3), the frequency of described vibration is 36 ~ 40kHz, and the temperature of vibration is 30 ~ 50 DEG C.
Further, in step (2), described centrifugal rotating speed is 1400 ~ 1600r/min, and the centrifugal time is 40 ~ 50min.
Further, by NaYF described in step (3)
4: Yb/Er-MoS
2binding substances aaerosol solution, at 70 ~ 80 DEG C, gets rid of film and dries, obtain NaYF under rotating speed 2500 ~ 3500r/min
4: Yb/Er-MoS
2binding substances film.
The solution prepared by step (1) and (2) is MoS
2receive micro-fragment aaerosol solution, the larger MoS of width can be removed by centrifugal
2fragment, makes the longitudinal middle level solution MoS pipetted
2the width of micro-fragment received is 10 ~ 15 μm, the MoS prepared by this step
2light is anti-reflection, and Limiting effect is best, directly affects NaYF
4: Yb/Er-MoS
2the optical Limiting effect of binding substances; In step (3), organic solvent can disperse MoS
2with rare earth NaYF
4: Yb/Er, forms aaerosol solution, is then made the energy generation transition of two kinds of materials by vibration, thus realizes combining, because 1) vibration can more easily the MoS reunited respectively
2shake scatter with rare earth (rare earth is easy to reunite), and solution fully mixes; 2) when ultra-sonic oscillation, there will be tiny bubble in solution, breaking of bubble can produce High Temperature High Pressure, strengthens aaerosol solution pedesis, makes NaYF
4: Yb/Er and MoS
2more easily react combination.
Preparation method of the present invention has the following advantages:
(1) present approach provides a kind of NaYF
4: Yb/Er-MoS
2the preparation method of binding substances, has filled up the deficiency of this preparation method in prior art, to studying rare earth NaYF further
4: Yb/Er and MoS
2the characteristic that micro-fragment of receiving combines lays the foundation;
(2) according to MoS prepared by the inventive method
2direction is nanoscale to fragment z, can embody nano-meter characteristic, and all the other directions is micro-meter scales, can prevent the damage to human body;
(3) according to NaYF prepared by the inventive method
4: Yb/Er-MoS
2micro-fragment bonding state of receiving is fine, and NaYF
4: Yb/Er-MoS
2receive between micro-fragment and do not reunite, good dispersity;
(4) according to NaYF prepared by the inventive method
4: Yb/Er-MoS
2binding substances, the optical limiting property under 530nm visible light wave range is better than MoS
2, and before light intensity reaches optical Limiting threshold values, do not occur the effect that light is anti-reflection can be used for lasing safety; And optical limiting property is better than NaYF under the near-infrared band of 780nm
4: Yb/Er;
(5) by NaYF that oscillatory reaction obtains
4: Yb/Er-MoS
2binding substances is far superior to the product obtained by natural dissolving method on bonding state and optical Limiting effect.
Accompanying drawing explanation
Fig. 1 is embodiment 1 MoS
2receive micro-fragment microscope figure;
Fig. 2 is embodiment 1 MoS
2atomic force microscope figure;
Fig. 3 is NaYF prepared by embodiment 1 DMF
4: Yb/Er-MoS
2binding substances bonding state SEM schemes;
Fig. 4 is NaYF prepared by embodiment 2 tetrahydrofuran (THF)
4: Yb/Er-MoS
2binding substances bonding state SEM schemes;
Fig. 5 is NaYF prepared by embodiment 3 ethanol
4: Yb/Er-MoS
2binding substances bonding state SEM schemes;
Fig. 6 is NaYF prepared by embodiment 4 N-Methyl pyrrolidone
4: Yb/Er-MoS
2binding substances bonding state SEM schemes;
Fig. 7 is NaYF prepared by reference examples DMF
4: Yb/Er-MoS
2binding substances bonding state SEM schemes;
Fig. 8 is embodiment 1 NaYF
4: Yb/Er-MoS
2binding substances (Che) and MoS
2pump-probe life diagram;
Fig. 9 is embodiment 1 NaYF
4: Yb/Er-MoS
2the NaYF of binding substances (Che), dissolving preparation naturally
4: Yb/Er-MoS
2and NaYF (phy)
4: Yb/Er(RE) fluorescence lifetime figure;
Figure 10 is embodiment 1NaYF
4: Yb/Er-MoS
2the NaYF of binding substances (Che), dissolving preparation naturally
4: Yb/Er-MoS
2and MoS (phy)
2under 530nm visible light wave range, normalized transmittance is with the change curve of light intensity;
Figure 11 is embodiment 1NaYF
4: Yb/Er-MoS
2binding substances (Che) and NaYF
4: Yb/Er(RE) under 780nm near-infrared band normalized transmittance with the change curve of light intensity.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
embodiment 1
(1) by commercially available for 0.1498g MoS
2powder and 60mLN, dinethylformamide mixes, sealing, and in ultrasonic cleaner, frequency 40kHz, under temperature 45 C, vibration 2h, forms homogeneous solution, obtain MoS
2-DMF solution suspension solution; (2) 60mLMoS is got
2-DMF aaerosol solution seal, and under the condition of 1500r/min centrifugal 45min, take out centrifugal rear longitudinal middle level solution 20mL, obtain the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution; (3) at 20mL width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add the commercially available rare earth NaYF of 0.0494g
4: Yb/Er, sealing, in ultrasonic cleaner, frequency 40kHz, under temperature 45 C, vibration 2h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
To the MoS prepared by the present embodiment
2fragment shooting optical microscope photograph (see Fig. 1) and atomic force microscopy (see Fig. 2) can find out MoS
2fragment width is 10 ~ 15 μm, and thickness is 150 ~ 310nm, and the MoS through the discrete preparation of vibration is described
2fragment is a kind of two-dimensional material, and namely only in z direction, dimension is the material of nanoscale.Material to human-body safety on conventional yardstick, may not safety on nanoscale, because the material of nanoscale directly can enter human body cell, and according to MoS prepared by the inventive method
2direction is nanoscale to fragment z, can embody nano-meter characteristic, and all the other directions is micro-meter scales, can prevent again the damage to human body.
Take out 5mLNaYF
4: Yb/Er-MoS
2binding substances aaerosol solution, drips on slide glass, 75 DEG C, gets rid of film and dries, obtain NaYF under 3000r/min rotating speed
4: Yb/Er-MoS
2binding substances film, examines under a microscope rare earth NaYF
4: Yb/Er and MoS
2receive micro-fragment bonding state, see Fig. 3.
As can be seen from Figure 3, roomy bright fragment is single MoS
2receive micro-fragment, being faint in color is NaYF in reunion shape
4: Yb/Er particle, NaYF
4: Yb/Er particle is pasted on MoS
2receive micro-fragment surrounding, can NaYF be found out
4: Yb/Er-MoS
2micro-fragment bonding state of receiving is fine, and NaYF
4: Yb/Er-MoS
2receive between micro-fragment and do not reunite, good dispersity.
From Fig. 8 pump-probe life diagram, NaYF prepared by the present embodiment
4: Yb/Er-MoS
2binding substances is measured the pump-probe life-span t=163fs come and is greater than MoS
2life-span t=105fs, be because NaYF
4: the Yb/Er MoS that had portion of energy to transfer to
2on, illustrate that the phenomenon of energy trasfer has appearred in this nano composite material, demonstrate NaYF
4: Yb/Er-MoS
2combine; From Fig. 9 fluorescence lifetime figure, NaYF prepared by the present embodiment
4: Yb/Er-MoS
2binding substances fluorescence lifetime t=0.740ns is less than NaYF
4: Yb/Er life-span t=0.875ns, due to MoS in the present embodiment
2thickness is 150 ~ 310nm, this thickness MoS
2there is no fluorescence (MoS
2unstressed configuration, the fluorescence lifetime of rare earth is very long, MoS
2itself can not affect the rare earth life-span, only has and to combine when them and to there occurs the shortening that energy trasfer just there will be fluorescence lifetime), so can judge whether the energy of rare earth shifts by test fluorescence, thus prove rare earth and MoS
2combination, there is energy transfer phenomenon in this nano material known accordingly, and the portion of energy of rare earth has transferred to MoS
2cause fluorescence lifetime to shorten, demonstrate NaYF
4: Yb/Er-MoS
2combine.
As shown in Figure 10, the NaYF for preparing of the present embodiment
4: Yb/Er-MoS
2binding substances optical Limiting threshold values (being optical Limiting during normalized transmittance < 100%) under 530nm visible light wave range is 2.89E10 G/cm
2be less than pure MoS
2optical Limiting threshold values 4.43E10 G/cm
2, illustrate that its optical limiting property is better than MoS at 530nm place
2, and before light intensity reaches optical Limiting threshold values, there is not the effect that light is anti-reflection, so can be used for lasing safety.
As shown in Figure 11, the NaYF for preparing of the present embodiment
4: Yb/Er-MoS
2binding substances optical Limiting threshold values under the near-infrared band of 780nm is 2.02E10 G/cm
2be less than NaYF
4: Yb/Er optical Limiting threshold values 2.94E10 G/cm
2, illustrate that optical limiting property is better than NaYF at 780nm place
4: Yb/Er.
embodiment 2
(1) by commercially available for 0.1236g MoS
2powder mixes with 60mL tetrahydrofuran (THF), sealing, and in ultrasonic cleaner, frequency 36kHz, at temperature 30 DEG C, vibration 2.5h, forms homogeneous solution, obtain MoS
2-tetrahydrofuran (THF) aaerosol solution; (2) 60mLMoS is got
2-tetrahydrofuran (THF) aaerosol solution seal, and under the condition of 1400r/min centrifugal 50min, take out centrifugal rear longitudinal middle level solution 15mL, obtain the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution; (3) at 15mL width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add the commercially available rare earth NaYF of 0.0437g
4: Yb/Er, sealing, in ultrasonic cleaner, frequency 36kHz, at temperature 30 DEG C, vibration 1.5h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
Take out 5mLNaYF
4: Yb/Er-MoS
2binding substances aaerosol solution, drips on slide glass, 70 DEG C, gets rid of film and dries, obtain NaYF under 2500r/min rotating speed
4: Yb/Er-MoS
2binding substances film, examines under a microscope rare earth NaYF
4: Yb/Er and MoS
2receive micro-fragment bonding state, see Fig. 4.
As shown in Figure 4, roomy bright fragment is single MoS
2receive micro-fragment, being faint in color is NaYF in reunion shape
4: Yb/Er particle, NaYF
4: Yb/Er particle is pasted on MoS
2receive micro-fragment surrounding, can NaYF be found out
4: Yb/Er-MoS
2micro-fragment bonding state of receiving is fine.
embodiment 3
(1) by commercially available for 0.1652g MoS
2powder mixes with 60mL ethanol, sealing, and in ultrasonic cleaner, frequency 38kHz, at temperature 40 DEG C, vibration 1.5h, forms homogeneous solution, obtain MoS
2-ethanol floats solution; (2) 60mLMoS is got
2-ethanol suspension solution seal, and under the condition of 1600r/min centrifugal 40min, take out centrifugal rear longitudinal middle level solution 21mL, obtain the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution; (3) at 21mL width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add the commercially available rare earth NaYF of 0.0431g
4: Yb/Er, sealing, in ultrasonic cleaner, frequency 38kHz, at temperature 40 DEG C, vibration 2.5h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
Take out 5mLNaYF
4: Yb/Er-MoS
2binding substances aaerosol solution, drips on slide glass, 80 DEG C, gets rid of film and dries, obtain NaYF under 3500r/min rotating speed
4: Yb/Er-MoS
2binding substances film, examines under a microscope rare earth NaYF
4: Yb/Er and MoS
2receive micro-fragment bonding state, see Fig. 5.
As shown in Figure 5, roomy bright fragment is single MoS
2receive micro-fragment, being faint in color is NaYF in reunion shape
4: Yb/Er particle, NaYF
4: Yb/Er particle is pasted on MoS
2receive micro-fragment surrounding, can NaYF be found out
4: Yb/Er-MoS
2micro-fragment bonding state of receiving is fine.
embodiment 4
(1) by commercially available for 0.1781g MoS
2powder mixes with 60mLN-methyl-2-pyrrolidone, sealing, and in ultrasonic cleaner, frequency 39kHz, under temperature 50 C, vibration 2h, forms homogeneous solution, obtain MoS
2-N-Methyl pyrrolidone aaerosol solution; (2) 60mLMoS is got
2-N-Methyl pyrrolidone aaerosol solution seal, and under the condition of 1450r/min centrifugal 48min, take out centrifugal rear longitudinal middle level solution 18mL, obtain the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution; (3) at 18mL width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add the commercially available rare earth NaYF of 0.0534g
4: Yb/Er, sealing, in ultrasonic cleaner, frequency 39kHz, under temperature 50 C, vibration 1.8h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
Take out 5mLNaYF
4: Yb/Er-MoS
2binding substances aaerosol solution, drips on slide glass, 78 DEG C, gets rid of film and dries, obtain NaYF under 2900r/min rotating speed
4: Yb/Er-MoS
2binding substances film, examines under a microscope rare earth NaYF
4: Yb/Er and MoS
2receive micro-fragment bonding state, see Fig. 6.
As shown in Figure 6, roomy bright fragment is single MoS
2receive micro-fragment, being faint in color is NaYF in reunion shape
4: Yb/Er particle.NaYF
4: Yb/Er particle is pasted on MoS
2receive micro-fragment surrounding, can NaYF be found out
4: Yb/Er-MoS
2micro-fragment bonding state of receiving is fine.
reference examples
(1) by 0.1498 commercially available MoS
2powder and 60mLN, dinethylformamide mixes, sealing, and in ultrasonic cleaner, frequency 40kHz, under temperature 45 C, vibration 2h, forms homogeneous solution, obtain MoS
2-DMF aaerosol solution; (2) 60mLMoS is got
2-DMF aaerosol solution seal, and under the condition of 1500r/min centrifugal 45min, take out centrifugal rear longitudinal middle level solution 20mL, obtain the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution; (3) at 20mL width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add the commercially available rare earth NaYF of 0.0494g
4: Yb/Er, allows it naturally dissolve, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
Take out 5mL NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution, drips on slide glass, 75 DEG C, gets rid of film and dries, obtain NaYF under 3000r/min rotating speed
4: Yb/Er-MoS
2binding substances film, examines under a microscope rare earth NaYF
4: Yb/Er and MoS
2receive micro-fragment bonding state, see Fig. 7.
As shown in Figure 7, rare earth NaYF
4: Yb/Er and MoS
2it is not fine that micro-fragment bonding state of receiving dissolves bonding state comparative effectiveness with vibration, although there is rare earth NaYF
4: Yb/Er can be combined in MoS
2receive micro-fragment surrounding, but most rare earth NaYF
4: Yb/Er is difficult to stick to MoS
2on, be free in MoS
2receive micro-fragment periphery or reunite in the solution, be not attached to MoS
2micro-fragment of receiving gets on.
Naturally the NaYF of preparation is dissolved as shown in Figure 9
4: Yb/Er-MoS
2the fluorescence lifetime of binding substances entirety and NaYF
4: Yb/Er fluorescence lifetime basically identical (in figure, curve phy and RE overlaps substantially), in visible fluorescence life test, mainly NaYF
4: Yb/Er plays effect, the MoS of doping
2the rare-earth fluorescent life-span is not affected, proves that its bonding state is very poor or do not combine at all.
As shown in Figure 10, the NaYF of preparation is naturally dissolved
4: Yb/Er-MoS
2binding substances is optical Limiting threshold values 6E10 G/cm under 530nm visible light wave range
2be far longer than pure MoS
2(4.43E10 G/cm
2) or the NaYF for preparing of oscillatory reaction
4: Yb/Er-MoS
2binding substances (2.89E10 G/cm
2), so naturally dissolve the NaYF prepared
4: Yb/Er-MoS
2its optical Limiting poor effect of binding substances.
Claims (8)
1.NaYF
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: comprise the following steps:
(1) by MoS
2mix with organic solvent, sealing, vibration 1.5 ~ 2.5h, obtains MoS
2-organic solvent aaerosol solution;
(2) by step (1) gained MoS
2-organic solvent aaerosol solution seals, centrifugal, pipettes centrifugal rear longitudinal middle level solution, obtains the MoS that width is 10 ~ 15 μm
2receive micro-fragment solution;
(3) in step (2) gained width be the MoS of 10 ~ 15 μm
2receive in micro-fragment solution and add rare earth NaYF
4: Yb/Er, sealing, vibration 1.5 ~ 2.5h, obtains NaYF
4: Yb/Er-MoS
2binding substances aaerosol solution.
2. NaYF according to claim 1
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (1), in often liter of organic solvent, add MoS
2amount be 2 ~ 3g.
3. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (1), and described organic solvent is ethanol, tetrahydrofuran (THF), N-Methyl pyrrolidone or DMF.
4. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (2), and the amount of pipetting of described longitudinal middle level solution is 25 ~ 35% of centrifugal rear suspension liquor capacity.
5. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (3), often rises in step (2) gained the MoS that width is 10 ~ 15 μm
2receive in micro-fragment solution and add NaYF
4: the amount of Yb/Er is 2 ~ 3g.
6. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (1) and (3), the frequency of described vibration is 36 ~ 40kHz, and the temperature of vibration is 30 ~ 50 DEG C.
7. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: in step (2), and described centrifugal rotating speed is 1400 ~ 1600r/min, and the centrifugal time is 40 ~ 50min.
8. NaYF according to claim 1 or 2
4: Yb/Er-MoS
2the preparation method of binding substances, is characterized in that: by NaYF described in step (3)
4: Yb/Er-MoS
2binding substances aaerosol solution, at 70 ~ 80 DEG C, gets rid of film and dries, obtain NaYF under rotating speed 2500 ~ 3500r/min
4: Yb/Er-MoS
2binding substances film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110420652A (en) * | 2019-08-14 | 2019-11-08 | 哈尔滨工业大学 | A kind of NaYF4:Yb/Er@MoS2Core-shell structure micron crystalline substance and preparation method thereof |
| CN110846024A (en) * | 2019-11-19 | 2020-02-28 | 常州工程职业技术学院 | Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007089376A1 (en) * | 2006-01-27 | 2007-08-09 | Coherent, Inc. | Frequency-doubled solid state laser optically pumped by frequency-doubled external-cavity surface-emitting semiconductor laser |
| CN101503560A (en) * | 2009-01-16 | 2009-08-12 | 上海师范大学 | Carbon nano-tube / polymer / metallic sulfide nano composite material and preparation thereof |
-
2014
- 2014-10-27 CN CN201410580842.9A patent/CN104371725B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007089376A1 (en) * | 2006-01-27 | 2007-08-09 | Coherent, Inc. | Frequency-doubled solid state laser optically pumped by frequency-doubled external-cavity surface-emitting semiconductor laser |
| CN101503560A (en) * | 2009-01-16 | 2009-08-12 | 上海师范大学 | Carbon nano-tube / polymer / metallic sulfide nano composite material and preparation thereof |
Non-Patent Citations (3)
| Title |
|---|
| WEI WEI等: "Nanocomposites of Graphene Oxide and Upconversion Rare-Earth Nanocrystals with Superior Optical Limiting Performance", 《SMALL》 * |
| 常梦洁: "有机/无机功能材料二维有序阵列的制备与光学性质研究", 《兰州大学博士学位论文》 * |
| 王沅倩等: "MoS2溶液的波长选择性光限幅效应研究", 《物理学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110420652A (en) * | 2019-08-14 | 2019-11-08 | 哈尔滨工业大学 | A kind of NaYF4:Yb/Er@MoS2Core-shell structure micron crystalline substance and preparation method thereof |
| CN110420652B (en) * | 2019-08-14 | 2022-04-12 | 哈尔滨工业大学 | NaYF4:Yb/Er@MoS2Core-shell structure micron crystal and preparation method thereof |
| CN110846024A (en) * | 2019-11-19 | 2020-02-28 | 常州工程职业技术学院 | Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof |
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