CN109266334A - A kind of preparation method of near-infrared long-persistence nano crystalline substance - Google Patents
A kind of preparation method of near-infrared long-persistence nano crystalline substance Download PDFInfo
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- CN109266334A CN109266334A CN201811091014.3A CN201811091014A CN109266334A CN 109266334 A CN109266334 A CN 109266334A CN 201811091014 A CN201811091014 A CN 201811091014A CN 109266334 A CN109266334 A CN 109266334A
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- ethyl orthosilicate
- znga
- nanocrystalline
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K11/7708—Vanadates; Chromates; Molybdates; Tungstates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
- C09K11/682—Chalcogenides with zinc or cadmium
Abstract
The invention discloses a kind of Cr3+Adulterate ZnGa2O4The preparation method of near-infrared long-persistence nano crystalline substance, the nanocrystalline size is at 5~30 nanometers.The nanocrystalline preparation method is the following steps are included: ethyl orthosilicate is dissolved in dehydrated alcohol by (1), the volume ratio 1: 5~1: 10 of ethyl orthosilicate and dehydrated alcohol.Nitric acid is added, the molar ratio 10: 1~20: 1 of ethyl orthosilicate and nitric acid is uniformly mixed.(2) claim zinc nitrate, gallium nitrate, rare earth nitrades and chromic nitrate to be dissolved in 1~5ml water, the resulting solution of step 1 is then added；(3) the resulting solution of step 2 is continued into stirring 0.5~5 hour, is aged 3~7 days, then obtains xerogel within dry 5~24 hours at 30~80 DEG C.Gained xerogel is put into Muffle furnace, keeps the temperature 1~6 hour at 600~1100 DEG C, naturally cools to room temperature, obtain glass ceramics.(4) obtained glass ceramics is put into 0.5~4mol%NaOH solution, is put into water heating kettle, in 60~200 DEG C, kept the temperature 5~24 hours, obtain Cr3+Adulterate ZnGa2O4It is nanocrystalline.
Description
Technical field
The present invention relates to the preparation methods of a kind of red long-persistence nano crystalline substance material for being applied to illumination field.
Background technique
Long afterglow refers to that luminescent material material after excitation light source (usually ultraviolet-visible light) stops irradiation still being able to hold
The phenomenon of supervention light.Therefore long after glow luminous material is otherwise known as light-storing material.As fluorescence labeling material, long-afterglow material is only
It needs using excitation light source irradiation a period of time before label, and in detection and labeling process, excitation light source can be removed, this
Sample can be avoided effectively due to the tissue fever and the interference of organism autofluorescence that light source irradiates and generates.Due to biological group
Knit to it is near-infrared luminous absorb it is low, near infrared band is also referred to as " optical window " of biological tissue, be it is optimal biology mark
Remember optical region.Recent years, near-infrared is long-persistence luminous to be started to show up prominently in biomarker field.At present more than near-infrared length
The research of brightness material is still in infancy, and only realizes that near-infrared is long-persistence luminous in a limited number of a system, mainly has:
Cr3+Adulterate gallate, such as ZnGa2O4、Zn3Ga2Ge2O10、LiGa5O8、Ga2O3、Gd3Ga5O12、Zn3Ga2SnO8Deng；And Mn2 +Doping system such as CaMgSi2O6: Mn2+, Eu2+, Dy3+、Ca0.2Zn0.9Mg0.9Si2O6: Eu2+, Ln3+(Ln=Dy, Pr, Ce, Nd),
Zn2P2O7: Mn2+, Tm3+、MAlO3: Mn4+, Ge4+(M=La, Gd) etc..Wherein ZnGa2O4: Cr3+It is that found near-infrared is sent out at present
The best long after glow luminous material of light efficiency.
Traditional long after glow luminous material generally uses high temperature solid-state method to synthesize, and during the sintering process, particle can be serious
Reunite, the particle size because obtained from is all very big (between 1-100 microns), this is obviously not suitable as biological labled material.
Currently, obtaining the most common method of nanometer long after glow luminous material is exactly ball-milling method, i.e., more than the bulky grain length obtained solid phase method
Then brightness luminescent material ball mill grinding is screened by partial size, to obtain nanoscale long-afterglow material.But pass through this
The nano material luminous intensity obtained after kind ball milling can sharply weaken, particle size is also uneven, it is not easy to it is surface modified,
To strongly limit its application in biomarker field.In addition, people also attempt using various wet chemical methods come
Prepare long-persistence nano-luminescent materials.As the Liu Yingliang group of Agricultural University Of South China is prepared for Y (OH) first with solvent-thermal method3It receives
Then mitron is prepared for the Y for having red long-afterglow luminous using subsequent heat treatment and vulcanizing treatment2O2S:Eu3+, Mg2+,
Ti4+Nanocrystalline (Mater.Chem.Phys., 119,52 (2010)).The Xu Min rosy clouds group of University Of Tianjin utilizes microwave legal system for the first time
For Sr3Al2O6: Eu2+, Dy3+Red long-afterglow luminescence nanocrystalline (Mater.Sci.Eng.B, 136,159 (2007)).Nankai
The Yan Xiuping seminar of university is prepared for the long-persistence luminous Cr of 49nm or so near-infrared by sol-gel method3+/Pr3+Doping
Zn2.94Ga1.96Ge2O10Nanocrystalline (J.Am.Chem.Soc., 135,14125 (2013)).Massachusetts, USA University Medical College
Gang Han seminar is prepared for 10nm ZnGa below by hydro-thermal method2O4: Cr3+It is nanocrystalline, after 750 DEG C of heat treatment,
The nanocrystalline long afterglow performance (J.Mater.Chem., 22,24713 (2012)) done well.Yuan Quan seminar of Wuhan University uses
Hydro-thermal method has synthesized that Zn1+xGa2-2xGexO4:Cr is nanocrystalline, utilizes the nanocrystalline tumour fluorescence label for realizing mouse
(ACS Nano, 11,8010 (2017)).In order to improve ZnGa2O4: Cr3+Luminous intensity, Rui Zou etc. uses SiO2Shell is as guarantor
Sheath, again SiO after high-temperature calcination2Erosion removal, ZnGa2O4: Cr3+, Sn4+Luminous intensity improves 13.5 times of (Nano
Research, 10,2070 (2017)).Generally speaking, the process route of long-persistence nano crystalline substance is prepared not enough using chemical method
Perfect, the nanocrystalline crystallization degree prepared is relatively low, and overall luminous is also weaker, and the luminous intensity that improve material is usual
The heat treatment process by high temperature is also needed, so as to cause the reunion of nano particle, influences application of the material in biomarker.
How to prepare that luminous efficiency height, particle size small (5-100nm), particle diameter distribution be uniform, good water solubility long-persistence nano material
Material is still that this kind of material is widely used in biomarker field problem urgently to be resolved.
Summary of the invention
In order to solve the deficiencies in the prior art, Cr is prepared the present invention provides a kind of3+Adulterate ZnGa2O4Long-persistence nano is brilliant
New method.This method uses the approach of glass ceramics, and the high ZnGa of crystallization degree is precipitated by the high-temperature heat treatment of glass2O4
It is nanocrystalline, glass matrix is then removed by alkali corrosion and obtains long-persistence nano crystalline substance.The nanocrystalline of this method preparation has ruler
The advantages that very little uniform, crystallization degree is high, luminous efficiency is high.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of Cr3+Adulterate ZnGa2O4It is nanocrystalline, the chemical formula of the material are as follows: ZnGa2-2xO4: x mol%Cr3+, y
Mol%Ln3+, wherein 0≤x≤50, it is preferable that 0≤x≤10；0≤y≤50, it is preferable that 0≤y≤10；Ln takes La, Ce, Pr,
One or more of Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
As illustratively, the rear-earth-doped gallic acid zinc nanocrystalline can be ZnGa1.94O4: 1mol%Cr3+, 2mol%
Dy3+。
According to the present invention, the ZnGa2-2xO4: x mol%Cr3+Material is nanostructure, and partial size is 5-100 nanometers,
It is preferred that 5~50 nanometers, more preferably 10~30 nanometers.
The present invention provides above-mentioned Cr3+Adulterate ZnGa2O4Nanocrystalline preparation method, described method includes following steps:
Ethyl orthosilicate is dissolved in dehydrated alcohol by step 1, the volume ratio 1: 5~1 of ethyl orthosilicate and dehydrated alcohol:
Between 10.Nitric acid acid as catalyst is added to be uniformly mixed between ethyl orthosilicate and the molar ratio 1: 1~10: 1 of nitric acid.
Step 2 claims zinc nitrate, gallium nitrate, rare earth nitrades and chromic nitrate to be dissolved in 1~5ml water, ethyl orthosilicate and nitre
Between the molar ratio 9: 1~1: 1 of sour zinc, between the molar ratio 9: 2~1: 2 of ethyl orthosilicate and gallium nitrate, step 1 is then added
In resulting solution；
The resulting solution of step 2 is continued stirring 0.5~5 hour by step 3, is aged 3~7 days, then dry at 30~80 DEG C
Obtain xerogel within dry 5~24 hours.Resulting xerogel is put into Muffle furnace, and heating rate control is per minute at 1~10 DEG C, most
Finishing temperature is controlled at 600~1100 DEG C, soaking time 1~6 hour, is then naturally cooled to room temperature, is obtained glass ceramics.
Obtained glass ceramics is put into 0.5~4mol%NaOH solution by step 4, is put into water heating kettle, in 60~
200 DEG C, 5~24 hours are kept the temperature, removes SiO2Substrate obtains Cr3+Adulterate ZnGa2O4It is nanocrystalline.
Gain effect of the invention is as follows:
1, a kind of Cr of the present invention3+Adulterate ZnGa2O4Nanocrystalline preparation method is different from hydro-thermal method and high temperature solid-state method etc.
Method, this method simple process, the ZnGa being prepared2O4Nanocrystalline luminous intensity be higher than wet chemistry method preparation it is nanocrystalline, its
The dispersibility of particle is better than the long after glow luminous material of high temperature solid-state method preparation.
2, a kind of Cr of the present invention3+Adulterate ZnGa2O4Nanocrystalline preparation method can pass through the essence of glass heat treatment process
The really partial size of adjustment nano particle.
3, a kind of Cr of the present invention3+Adulterate ZnGa2O4The nanocrystal surface that nanocrystalline preparation method obtains contains largely
Hydroxyl can be evenly dispersed in water, in dehydrated alcohol, be conducive to the further functionalization and bio-modification of nano grain surface,
Promote it in the application of life science.
Detailed description of the invention
Fig. 1 is the process flow chart that glass ceramics approach prepares water-soluble long-persistence nano crystalline substance
Fig. 2 is Cr after 600,900,1000 DEG C of heat treatment 3h3+Adulterate SiO2-ZnGa2O4XRD spectra, it is vertical linear in figure
Spectrogram is standard ZnGa2O4Powder diffraction spectrum (JCPDS NO.38-1240)
Fig. 3 is Cr after 1000 DEG C of heat treatment 3h3+, Dy3+Codope SiO2-ZnGa2O4(a) excitation spectrum (inspection of glass ceramics
Survey launch wavelength is 708nm) and emission spectra (excitation wavelength 277nm), (b) Cr3+Fluorescence lifetime curve (the excitation wave of 2E energy level
A length of 277nm, Detection wavelength 708nm)
Fig. 4 removes SiO2The Cr obtained after matrix3+, Dy3+Codope ZnGa2O4Nanocrystalline transmission electron microscope photo.
Specific embodiment
The present invention prepares long-persistence nano crystalline substance using glass ceramics approach, and specific embodiment is as shown in Figure 1.
The present invention is further detailed below with reference to example.But skilled in the art realises that following embodiments
It is not limiting the scope of the invention, any improvements and changes made on the basis of the present invention are all protected in the present invention
In range.
Embodiment 1, ZnGa2O4: Cr3+1mol%, Dy3+2mol% nanocrystalline preparation
5mL ethyl orthosilicate is dissolved in 20mL dehydrated alcohol, is uniformly mixed.1mL concentrated nitric acid is added in the solution
Make catalyst, continues stirring 10 minutes.Weigh 0.853g zinc nitrate, 1.423g gallium nitrate, 0.014g chromic nitrate and 0.052g six
Nitric hydrate dysprosium is dissolved in 5mL water, is then added dropwise in above-mentioned resulting solution, and resulting solution continues stirring 2 hours, is poured into
It in culture dish, is aged 7 days at room temperature, obtained gel continues 10 hours dry at 50 DEG C.Resulting xerogel is put into Muffle
In furnace, it is heated to 900-1000 DEG C with the heating rate of 2 DEG C/min, soaking time 2 hours, room temperature is then naturally cooled to, obtains
To SiO2-ZnGa2O4: Cr3+Glass ceramics.Obtained glass ceramics is put into 4mol/LNaOH solution, 120 DEG C of hydro-thermal process
12 hours, remove SiO2Substrate obtains Cr3+, Dy3+Adulterate ZnGa2O4It is nanocrystalline.
As shown in Fig. 2, sample is so amorphous state in 600 DEG C in air heat treatment 3h successors；900 DEG C in air of sample
It is heat-treated 3h, spinel-type ZnGa can be grown from glass matrix2O4It is nanocrystalline, it can be evaluated whether using Scherrer formula
Size nanocrystalline at this time is in 5nm or so out.And with the increase of heat treatment temperature, ZnGa2O4Diffraction maximum it is gradually sharp,
Show nanocrystalline growing up.When heat treatment temperature is increased to 1000 DEG C, ZnGa is obtained2O4Crystallite dimension is 18nm or so.
As shown in figure 3, under the excitation of 277nm ultraviolet light, sample is in 600- in air after 1000 DEG C of heat treatment 3h
Generated between 800nm it is stronger shine, it is wherein luminous 695nm to belong to Cr3+Ion2E→4A2The R- line of transition is sent out
It penetrates, other emission peaks belong to adjoint2E→4A2The Stokes and anti-Stokes phonon sideband of transition emit.It is monitoring
In the excitation spectrum to shine at 708nm, occurs wide excitation peak near 277 and 406nm, these belong to Cr3+Ion4A2→4T1(4P)
The transition of spin license.In monitoring Cr3+'s2In the fluorescence decay curve of E energy level, we can observe Cr3+The long fluorescence longevity
Life.
Fig. 4 is Cr after 1000 DEG C of heat treatment 3h3+, Dy3+Codope SiO2-ZnGa2O4NaOH of the glass ceramics in 0.5M is molten
In liquid, the transmission electron microscope photo of powder sample is obtained after 120 DEG C of hydro-thermal process 6h.It can be seen from the figure that by NaOH solution
Hydro-thermal process, most of ZnGa2O4It can be stripped out from glass ceramics.
Embodiment 2, ZnGa2O4: Cr3+1mol% nanocrystalline preparation
5mL ethyl orthosilicate is dissolved in 20mL dehydrated alcohol, is uniformly mixed.1mL concentrated nitric acid is added in the solution
Make catalyst, continues stirring 10 minutes.It weighs 0.853g zinc nitrate, 1.452g gallium nitrate and 0.014g chromic nitrate and is dissolved in 5mL water
In, it is then added dropwise in above-mentioned resulting solution, resulting solution continues stirring 2 hours, pours into culture dish, old at room temperature
Change 7 days, obtained gel continues 10 hours dry at 50 DEG C.Resulting xerogel is put into Muffle furnace, with the heating of 2 DEG C/min
Rate is heated to 1000 DEG C, soaking time 2 hours, then naturally cools to room temperature, obtains SiO2-ZnGa2O4: Cr3+Glass pottery
Porcelain.Obtained glass ceramics is put into 4mol/L NaOH solution, 180 DEG C hydro-thermal process 8 hours, remove SiO2Substrate obtains
Cr3+Adulterate ZnGa2O4It is nanocrystalline.
Embodiment 3, ZnGa2O4: Cr3+1mol%, Tm3+Nanocrystalline preparation
5mL ethyl orthosilicate is dissolved in 20mL dehydrated alcohol, is uniformly mixed.1mL concentrated nitric acid is added in the solution
Make catalyst, continues stirring 10 minutes.Weigh 0.853g zinc nitrate, 1.423g gallium nitrate, 0.014g chromic nitrate and 0.053g six
Nitric hydrate thulium is dissolved in 5mL water, is then added dropwise in above-mentioned resulting solution, and resulting solution continues stirring 2 hours, is poured into
It in culture dish, is aged 7 days at room temperature, obtained gel continues 10 hours dry at 50 DEG C.Resulting xerogel is put into Muffle
In furnace, 900~1000 DEG C are heated to the heating rate of 2 DEG C/min, soaking time 2 hours, room temperature is then naturally cooled to, obtains
To SiO2-ZnGa2O4: Cr3+Glass ceramics.Obtained glass ceramics is put into 4mol/L NaOH solution, 120 DEG C of hydro-thermal process
12 hours, remove SiO2Substrate obtains Cr3+, Tm3+Adulterate ZnGa2O4It is nanocrystalline.
Claims (1)
1. a kind of preparation method of near-infrared long-persistence nano crystalline substance, it is characterised in that the steps included are as follows for this method:
Ethyl orthosilicate is dissolved in dehydrated alcohol by step 1, the volume ratio 1: 5~1: 10 of ethyl orthosilicate and dehydrated alcohol it
Between.Nitric acid acid as catalyst is added to be uniformly mixed between ethyl orthosilicate and the molar ratio 1: 1~10: 1 of nitric acid；
Step 2 weighs zinc nitrate, gallium nitrate, rare earth nitrades and chromic nitrate and is dissolved in 1~5ml water, ethyl orthosilicate and nitric acid
Between the molar ratio 9: 1~1: 1 of zinc, between the molar ratio 9: 2~1: 2 of ethyl orthosilicate and gallium nitrate, step 1 institute is then added
In the solution obtained；
The resulting solution of step 2 is continued stirring 0.5~5 hour by step 3, is aged 3~7 days, then in 30~80 DEG C of dry 5-
Obtain xerogel within 24 hours.Resulting xerogel is put into Muffle furnace, and heating rate control is per minute at 1~10 DEG C, most final temperature
Degree control soaking time 1~6 hour, then naturally cools to room temperature, obtains glass ceramics at 600~1100 DEG C；
Obtained glass ceramics is put into 0.5~4mol%NaOH solution by step 4, is put into water heating kettle, in 60~200 DEG C,
Heat preservation 5~24 hours removes SiO2Substrate obtains rare earth and Cr3+Adulterate ZnGa2O4It is nanocrystalline.
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Citations (3)
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|---|---|---|---|---|
| US20140371575A1 (en) * | 2012-01-30 | 2014-12-18 | Centre National De La Recherche Scientifique (Cnrs | Persistent Luminescence Nanoparticles Excitable in situ for in vivo Optical Imaging, in vivo Multimodal Optical-MRI Imaging, and Theranostics |
| CN106590656A (en) * | 2016-12-06 | 2017-04-26 | 喀什大学 | Preparation method of near-infrared long afterglow luminescent nanometer particle |
| CN108191213A (en) * | 2017-12-06 | 2018-06-22 | 常州市丰瑞电子有限公司 | A kind of preparation method of composite fluorescence cloche |
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2018
- 2018-09-10 CN CN201811091014.3A patent/CN109266334A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140371575A1 (en) * | 2012-01-30 | 2014-12-18 | Centre National De La Recherche Scientifique (Cnrs | Persistent Luminescence Nanoparticles Excitable in situ for in vivo Optical Imaging, in vivo Multimodal Optical-MRI Imaging, and Theranostics |
| CN106590656A (en) * | 2016-12-06 | 2017-04-26 | 喀什大学 | Preparation method of near-infrared long afterglow luminescent nanometer particle |
| CN108191213A (en) * | 2017-12-06 | 2018-06-22 | 常州市丰瑞电子有限公司 | A kind of preparation method of composite fluorescence cloche |
Non-Patent Citations (1)
| Title |
|---|
| LI, ZHANJUN;等: "In Vivo Repeatedly Charging Near-Infrared-Emitting Mesoporous SiO2/ZnGa2O4:Cr3+ Persistent Luminescence Nanocomposites", 《ADVANCED SCIENCE 》 * |
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