CN108998019A - A kind of broadband emission near-infrared fluorescent powder and preparation method thereof - Google Patents
A kind of broadband emission near-infrared fluorescent powder and preparation method thereof Download PDFInfo
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- CN108998019A CN108998019A CN201810891883.8A CN201810891883A CN108998019A CN 108998019 A CN108998019 A CN 108998019A CN 201810891883 A CN201810891883 A CN 201810891883A CN 108998019 A CN108998019 A CN 108998019A
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- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
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Abstract
The invention discloses a kind of broadband emission near-infrared fluorescent powder and preparation method, chemical formula M3Ga2‑xGeO8:xCr3+, wherein M is one or both of Mg, Ca, Sr, Zn element, 0.01≤x≤0.2.Fluorescent powder of the present invention can be excited by the light in 200~700nm wave-length coverage, launch the near-infrared fluorescent powder of 650~1200nm range, excitation and launch wavelength range are wide, and luminous intensity is high, stability is high, the high temperature solid-state the preparation method simple process of use, easily operated control, favorable repeatability, it is highly-safe, preparation time is short, high production efficiency, is suitable for industrialization large-scale production and popularization and application.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of broadband emission near-infrared fluorescent powder and its preparation side
Method.
Background technique
It is near-infrared luminous to have the characteristics that big penetration depth, high sensitivity, background are small, in terms of bioanalysis
There is important application prospect.Infrared fluorescent material has been widely used for science and technology, industry, agricultural and daily life
In.With the development of science and technology, in recent years luminescent material again be applied in some new devices, however these illumination and
Display fluorescent material shines mainly in the visible light wave range of human eye sensitivity.And our interested fluorescent materials, mainly
It shines in the insensitive dark red and near infrared band of human eye.Dark red and near-infrared fluorescent material, absorb visible light, transmitting it is dark red and
Near infrared light.It, can be in infrared tracking instrument, infrared radiation source survey meter, organs of living beings detection, deep tissues according to this fluorescent characteristic
Detection, food inspection, plant illumination etc. have potential application prospect, and directly apply to dark red and near-infrared fluorescent material
Research it is actually rare, application important bottleneck be that its near infrared luminous intensity is weaker and transmitting band is relatively narrow.
With the continuous improvement of people's living standards, food quality assurance and quality control are increasingly by the weight of people
Depending on.Perfect quality assurance and quality control system are established in enterprises, can not only be reduced production cost, be guaranteed product matter
Amount, and the sustainable development that can be economized on resources, reduce environmental pollution, protecting environment, realizing enterprise.NIR technology
Appearance so that fine new page has been opened in process analysis procedure analysis.Near infrared spectrum belongs to the frequency multiplication of molecular vibration spectrum and sum of fundamental frequencies absorbs
Spectrum, mainly to the absorption of hydric group, wherein containing the composition and molecular structure of most of type organic compounds
Information.Different groups and same group have significant difference to the absorbing wavelength of near infrared light in different chemical environments, and
Absorption coefficient is small, and fever is few, therefore near infrared spectrum can be used as a kind of effective carrier for obtaining information.In the 1960s,
The Norris etc. in the U.S. is first begin to research using moisture, the protein, fat in near-infrared spectral analysis technology measurement cereal
Equal size, and it is dedicated to the research of other quality of agricultural product.
Since near infrared light has very strong penetration capacity, in test sample, it is not necessary to any pre-treatment is carried out,
Any chemical reagents are not needed.It compares with conventional method of analysis, neither can cause environmental pollution, and a large amount of reagent can be saved
Expense, and minute is short, no destructiveness, is a kind of fast and accurately analysis method applied to many agricultural product.Cause
This, develops efficient, sensitive broadband emission near-infrared fluorescent powder and has become an extremely urgent job, and at present main
Developing direction.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of broadband emission near-infrared fluorescent powder and preparation method thereof is provided, this
The near-infrared fluorescent powder provided is invented with Cr3+As Doped ions, luminous intensity is relatively strong and transmitting band is broadband, is mainly used in
Field of food detection.
The chemical general formula for solving fluorescent powder used by above-mentioned technical problem is M3Ga2-xGeO8:xCr3+, wherein M is represented
Any one in Mg, Ca, Sr, Zn or two kinds, 0.01≤x≤0.2, emission wavelength is located at 650~1200nm, and emission peak is located at
800~915nm.
In the chemical general formula of above-mentioned fluorescent powder, preferably M represents Mg, 0.04≤x≤0.06.
Broadband emission near-infrared fluorescent powder of the present invention the preparation method comprises the following steps: according to M3Ga2-xGeO8:xCr3+Stoichiometry
Than accurately weighing raw material MO or MCO3、Ga2O3、GeO2、Cr2O3, ground and mixed is uniform, and 3~6 are sintered at 1300~1500 DEG C
Hour, it is cooled to room temperature, is fully ground, obtain broadband emission near-infrared fluorescent powder.
In above-mentioned preparation method, it is sintered 4~5 hours preferably at 1400 DEG C.
In above-mentioned preparation method, the heating rate being further preferably sintered is 5~10 DEG C/min.
The present invention passes through in M3Ga2GeO8Middle doping Cr3+, to obtain wave-length coverage in the high-intensitive of 650~1200nm
Near-infrared fluorescent powder, excitation and launch wavelength range are wide, and luminous intensity is high, and stability is high, the high temperature solid-state the preparation method of use
Simple process, easily operated control, favorable repeatability is highly-safe, and preparation time is short, high production efficiency, is suitable for industrialization
Large-scale production and popularization and application.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the near-infrared fluorescent powder of Examples 1 to 4 preparation.
Fig. 2 is the excitation and emission spectra figure of near-infrared fluorescent powder prepared by embodiment 2.
Fig. 3 is the launching light spectrogram of the near-infrared fluorescent powder of Examples 1 to 4 preparation.
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
According to Mg3Ga1.99GeO8:0.01Cr3+Stoichiometric ratio, weigh MgO 0.3627g, Ga2O3 0.5595g、GeO2
0.3249g、Cr2O30.0023g, and dehydrated alcohol is added and grinds 30 minutes in the agate mortar after mixing, after grinding
Powder be put into corundum crucible, then corundum crucible is put into high temperature box furnace, is heated up with the heating rate of 10 DEG C/min
To 1400 DEG C, Isothermal sinter 5 hours, it is down to room temperature to temperature, is fully ground, obtains near-infrared fluorescent powder Mg3Ga1.99GeO8:
0.01Cr3+。
Embodiment 2
In the present embodiment, according to Mg3Ga1.97GeO8:0.03Cr3+Stoichiometric ratio, weigh MgO 0.3627g, Ga2O3
0.5539g、GeO2 0.3249g、Cr2O30.0068g, other steps are same as Example 1, obtain near-infrared fluorescent powder
Mg3Ga1.97GeO8:0.03Cr3+。
Embodiment 3
In the present embodiment, according to Mg3Ga1.95GeO8:0.05Cr3+Stoichiometric ratio, weigh MgO 0.3627g, Ga2O3
0.5483g、GeO2 0.3249g、Cr2O30.0114g, other steps are same as Example 1, obtain near-infrared fluorescent powder
Mg3Ga1.95GeO8:0.05Cr3+。
Embodiment 4
In the present embodiment, according to Mg3Ga1.93GeO8:0.07Cr3+Stoichiometric ratio, weigh MgO 0.3627g, Ga2O3
0.5427g、GeO2 0.3249g、Cr2O30.0160g, other steps are same as Example 1, obtain near-infrared fluorescent powder
Mg3Ga1.93GeO8:0.07Cr3+。
Near-infrared fluorescent powder obtained by Examples 1 to 4 is subjected to XRD analysis, as shown in Figure 1.XRD shows that obtained material is
Single-phase and all diffraction maximum matches with standard card, illustrates that the fluorescent powder of preparation is pure phase and is keeping crystal structure not
Cr in the case where change3+Successfully enter in parent lattice.
Excitation and emission spectra test is carried out to fluorescent powder prepared by embodiment 3, as a result sees Fig. 2.Excitation spectrum shows it
Excitation peak is made of three excitation peaks of 265nm, 420nm, 600nm or so, is respectively derived from Cr3+'s4A2→4T1(4P)、4A2
→4T1(4F) and4A2→4T2(4F) transition, the fluorescent powder can be by near ultraviolet LED chip (380~420nm) and blue-light LED chips
(420~480nm) is effectively excited；Emission spectrum has a weak spike in 700nm or so, belongs to Cr3+'s2E→4A2Spin is prohibited
Transition is hindered, broadband emission belongs to Cr within the scope of 650~1200nm3+'s4T2→4A2Spin allowed transition, shows the fluorescent powder
The near-infrared fluorescent of 650~1200nm can be emitted under the excitation of external light source, peak value is located at 915nm.
Claims (5)
1. a kind of broadband emission near-infrared fluorescent powder, it is characterised in that: the chemical general formula of the fluorescent powder is M3Ga2-xGeO8:xCr3+,
Wherein M represents any one in Mg, Ca, Sr, Zn or two kinds, 0.01≤x≤0.2, and emission wavelength is located at 650~1200nm,
Emission peak is located at 800~915nm.
2. broadband emission near-infrared fluorescent powder according to claim 1, it is characterised in that: the M represents Mg, 0.04≤x
≤0.06。
3. a kind of preparation method of broadband emission near-infrared fluorescent powder described in claim 1, it is characterised in that: according to M3Ga2- xGeO8:xCr3+Stoichiometric ratio, accurately weigh raw material MO or MCO3、Ga2O3、GeO2、Cr2O3, ground and mixed is uniform,
It is sintered 3~6 hours at 1300~1500 DEG C, is cooled to room temperature, is fully ground, obtain broadband emission near-infrared fluorescent powder.
4. the preparation method of broadband emission near-infrared fluorescent powder according to claim 3, it is characterised in that: at 1400 DEG C
Sintering 4~5 hours.
5. the preparation method of broadband emission near-infrared fluorescent powder according to claim 3 or 4, it is characterised in that: sintering
Heating rate is 5~10 DEG C/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093155A (en) * | 2019-06-17 | 2019-08-06 | 陕西师范大学 | A kind of two area's broad band emitting phosphor of near-infrared and preparation method thereof |
| CN111647404A (en) * | 2020-07-25 | 2020-09-11 | 陕西师范大学 | Cr (chromium)3+Activated broadband near-infrared fluorescent powder and preparation method thereof |
| WO2022163269A1 (en) * | 2021-01-29 | 2022-08-04 | パナソニックＩｐマネジメント株式会社 | Fluorescent material, light-emitting device, sensing system light source, and sensing system illumination system |
| CN116143498A (en) * | 2022-11-21 | 2023-05-23 | 河北光兴半导体技术有限公司 | Near infrared fluorescent ceramic material, preparation method thereof and near infrared light-emitting device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105255478A (en) * | 2015-10-15 | 2016-01-20 | 广东工业大学 | Reversible photochromic material with near-infrared long afterglow luminescence and preparing method thereof |
| CN108231979A (en) * | 2017-01-24 | 2018-06-29 | 江苏博睿光电有限公司 | Infrared L ED light source |
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2018
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Patent Citations (2)
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| CN105255478A (en) * | 2015-10-15 | 2016-01-20 | 广东工业大学 | Reversible photochromic material with near-infrared long afterglow luminescence and preparing method thereof |
| CN108231979A (en) * | 2017-01-24 | 2018-06-29 | 江苏博睿光电有限公司 | Infrared L ED light source |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110093155A (en) * | 2019-06-17 | 2019-08-06 | 陕西师范大学 | A kind of two area's broad band emitting phosphor of near-infrared and preparation method thereof |
| CN111647404A (en) * | 2020-07-25 | 2020-09-11 | 陕西师范大学 | Cr (chromium)3+Activated broadband near-infrared fluorescent powder and preparation method thereof |
| WO2022163269A1 (en) * | 2021-01-29 | 2022-08-04 | パナソニックＩｐマネジメント株式会社 | Fluorescent material, light-emitting device, sensing system light source, and sensing system illumination system |
| CN116143498A (en) * | 2022-11-21 | 2023-05-23 | 河北光兴半导体技术有限公司 | Near infrared fluorescent ceramic material, preparation method thereof and near infrared light-emitting device |
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Application publication date: 20181214 |