CN108531167A - A kind of near-infrared shortwave fluorescent powder and preparation method thereof - Google Patents
A kind of near-infrared shortwave fluorescent powder and preparation method thereof Download PDFInfo
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- CN108531167A CN108531167A CN201810604872.7A CN201810604872A CN108531167A CN 108531167 A CN108531167 A CN 108531167A CN 201810604872 A CN201810604872 A CN 201810604872A CN 108531167 A CN108531167 A CN 108531167A
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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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
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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
- C09K11/7792—Aluminates
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Abstract
The invention discloses a kind of near-infrared shortwave fluorescent powders and preparation method thereof.The fluorescent powder can be excited by the light of 250 ~ 500nm, launch the near infrared light of 900 ~ 1100nm.The chemical formula of the fluorescent powder is：MAl5O8:Ln3+ x,Fe3+ y,Yb3+ z, wherein M is made of at least one of Li, Na, K；Ln is made of at least one of Ce, Tb, Dy, Eu, and x, y, z is respectively Ln, Fe, Yb ion and MAl adulterated5O8Molar ratio, permissible value range is all 0.0001 ~ 0.1.The fluorescent powder is combined and is prepared using wet-mixing and high temperature solid-state method, and product has the characteristics that purity is high, uniformity is good, can be widely used in optical-fibre communications, infrared remote control and silicon solar transition material.
Description
Technical field
The present invention relates to a kind of near-infrared shortwave fluorescent powders, and provide the preparation method of the fluorescent powder, belong to luminous material
Material field.
Background technology
It is logical in optical fiber since near infrared light (near-infrared, NIR) penetration depth is big, interferes the special advantages such as few
Application in news, infrared remote control and silicon solar transition material increasingly attracts people's attention.It is special that rare earth element has
4f electronics shell structure and abundant energy level, and can emit the light of various near infrared bands as Validation Counter's doping.Cause
This, the concern of scientific research personnel is received based on rare earth ion doped near infrared light material.Due to Yb3+'s2F5/2→2F7/2Radiation jump
It moves, launches the near infrared light of 900 ~ 1100nm, and Yb3+The absorption intensity that ion doping near-infrared light-emitting material is shown mostly
Weak, the problems such as luminous intensity is not strong enough, it is caused to receive limitation in practical applications.Therefore, suitable sensitizer and base are selected
Matter improves Yb3+The near infrared luminous intensity of ion is extremely urgent.
Contain O-H and c h bond in rare earth organic complex, both keys have high-frequency vibration, it is easy to keep excitation state non-
It is radiated ground state, causing to shine is quenched, and then substantially reduces near-infrared luminous efficiency.And select inorganic compound as near-infrared
Luminescent ceramic matrix, can be to avoid generation fluorescent quenching.Currently, near-infrared light-emitting material matrix mainly has oxide-base both at home and abroad
Matter, molybdate substrate, borate, vanadate and fluoride matrix, sensitizer mainly have Mn, Cr, Pr, Nd etc..But due to
It is limited by material and preparation method, the stability and luminous intensity of these materials all have certain defect.Therefore there is an urgent need for into
One step is deeply researched and developed, to build the good near-infrared light-emitting material of high-performance stability from new approach.
Invention content
The purpose of the present invention is with defect, provide that a kind of chemical property is stable, luminescent properties in view of the deficiencies of the prior art
Excellent near-infrared shortwave phosphor material powder, the fluorescent powder are that a kind of ultraviolet lower conversion near-infrared to blue light broadband excitation is glimmering
Light powder, excitation spectrum ranging from 250 ~ 500nm, emission spectrum ranging from 900 ~ 1100nm, chemical formula are：MAl5O8: Ln3+ x,
Fe3+ y,Yb3+ z, wherein M is made of at least one of Li, Na, K, and Ln is made of at least one of Ce, Tb, Dy, Eu, x,
Y, z is respectively Ln, Fe, Yb ion and MAl adulterated5O8Molar ratio, permissible value range is all 0.0001 ~ 0.1.
It is a further object of the present invention to provide a kind of methods preparing the phosphor material powder, and this method is simple, easily operated,
It is pollution-free, at low cost.
To achieve the above object, the present invention uses following technical scheme：
（1）M is weighed by the molar ratio of fluorescent powder chemical formula2CO3、Al(NO3)3·9H2O and the corresponding nitric acid of Doped ions
Salt is mixed, and suitable dust technology is added, is sufficiently stirred, and adds deionized water to being completely dissolved, and continues 1 ~ 2h of stirring, is stood
After 30min, it is evaporated under reduced pressure and dries；
（2）Samples weighing after drying, is added the HBO of 0 ~ 5wt%3It is uniformly mixed, is put into high purity aluminium oxide crucible, 1200
2 ~ 4h is calcined at ~ 1500 DEG C, cooled to room temperature pulverizes and sieves, and obtains final products.
Compared with the prior art, the present invention has the following advantages：
（1）Lower conversion near-infrared shortwave fluorescent powder prepared by the present invention, matrix has good chemistry, thermal stability, with Fe3+
And Ln3+（Ln is made of at least one of Ce, Tb, Dy, Eu）Sensitizer is made jointly, with other undoped with Fe3+、Ln3+It is close red
Outer shortwave fluorescent powder is compared, and under same excitation light source, luminous intensity significantly improves.
（2）The present invention, which using wet-mixing increases temperature solid phase method and is combined, prepares near-infrared shortwave fluorescent powder, this method
The product that purity is high, uniformity is good can be prepared, manufacturing method is simple, pollution-free, at low cost, has and commercially uses valence well
Value.
Description of the drawings
Fig. 1 is LiAl prepared by embodiment 15O8:0.001Ce3+,0.006Fe3+,0.01Yb3+Exciting light spectrogram.
Fig. 2 is LiAl prepared by embodiment 15O8:0.001Ce3+,0.006Fe3+,0.01Yb3+Launching light spectrogram.
Specific implementation mode
For a further understanding of the present invention, with reference to embodiment to near-infrared shortwave fluorescent powder provided by the invention and its
Preparation method illustrates, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
（1）According to chemical formula LiAl5O8:0.001Ce3+,0.006Fe3+,0.01Yb3+, raw material Li is weighed respectively2CO3 0.5mol,
Al(NO3) 3·9H2O 5mol, Ce (NO3)3·6H2O 0.001mol, Fe (NO3) 3·9H2O 0.006mol, Yb (NO3)3·
6H2O 0.01mol, are mixed and are placed in beaker, and the nitric acid of 500ml 10% is added, is sufficiently stirred, and add deionized water to complete
Dissolving continues to stir 1.5h, after standing 30min, is evaporated under reduced pressure and dries；
（2）Samples weighing after drying, is added the HBO of 1wt%3It is uniformly mixed, is put into high purity aluminium oxide crucible, at 1300 DEG C
Lower calcining 2h, cooled to room temperature pulverize and sieve, and obtain final products.
Embodiment 2
（1）According to chemical formula NaAl5O8:0.001Tb3+,0.003Fe3+,0.05Yb3+, raw material Na is weighed respectively2CO3 0.5mol,
Al(NO3) 3·9H2O 5mol, Tb (NO3)3·6H2O 0.001mol, Fe (NO3) 3·9H2O 0.003mol, Yb (NO3)3·
6H2O 0.05mol, are mixed and are placed in beaker, and the nitric acid of 500ml 10% is added, is sufficiently stirred, and add deionized water to complete
Dissolving continues to stir 1h, after standing 30min, is evaporated under reduced pressure and dries；
（2）Sample after drying is put into high purity aluminium oxide crucible, 2h is calcined at 1500 DEG C, cooled to room temperature crushes
Sieving, obtains final products.
Embodiment 3
（1）According to chemical formula KAl5O8:0.005Dy3+,0.0001Fe3+,0.1Yb3+, raw material K is weighed respectively2CO3 0.5mol, Al
(NO3) 3·9H2O 5mol, Dy (NO3)3·6H2O 0.005mol, Fe (NO3) 3·9H2O 0.0001mol, Yb (NO3)3·
6H2O 0.1mol, are mixed and are placed in beaker, and the nitric acid of 500ml 10% is added, is sufficiently stirred, and add deionized water to complete
Dissolving continues to stir 1h, after standing 30min, is evaporated under reduced pressure and dries；
（2）Samples weighing after drying, is added the HBO of 3wt%3It is uniformly mixed, calcines 4h at 1200 DEG C, naturally cool to room
Temperature pulverizes and sieves, and obtains final products.
Embodiment 4
（1）According to chemical formula LiAl5O8:0.005Eu3+,0.005Fe3+,0.05Yb3+, raw material Li is weighed respectively2CO3 0.5mol,
Al(NO3) 3·9H2O 5mol, Eu (NO3)3·6H2O 0.005mol, Fe (NO3) 3·9H2O 0.005mol, Yb (NO3)3·
6H2O 0.05mol, are mixed and are placed in beaker, and the nitric acid of 500ml 10% is added, is sufficiently stirred, and add deionized water to complete
Dissolving continues to stir 2h, after standing 30min, is evaporated under reduced pressure and dries；
（2）Samples weighing after drying, is added the HBO of 5wt%3It is uniformly mixed, calcines 3h at 1300 DEG C, naturally cool to room
Temperature pulverizes and sieves, and obtains final products.
Claims (2)
1. a kind of near-infrared shortwave fluorescent powder, it is characterised in that：The fluorescent powder is a kind of ultraviolet lower turn to blue light broadband excitation
Near-infrared fluorescent powder, excitation spectrum ranging from 250 ~ 500nm, emission spectrum ranging from 900 ~ 1100nm are changed, chemical formula is：
MAl5O8: Ln3+ x,Fe3+ y,Yb3+ z, wherein M is made of at least one of Li, Na, K, Ln by Ce, Tb, Dy, Eu at least
A kind of composition, x, y, z are respectively Ln, Fe, Yb ion and MAl adulterated5O8Molar ratio, permissible value range is all 0.0001 ~
0.1。
2. a kind of preparation method of near-infrared shortwave fluorescent powder as described in claim 1, the specific steps are：
（1）M is weighed by the molar ratio of fluorescent powder chemical formula described in claim 12CO3、Al(NO3)3·9H2O and adulterate from
The corresponding nitrate of son, is mixed, and adds suitable dust technology, is sufficiently stirred, and adds deionized water to being completely dissolved, continues
1 ~ 2h is stirred, after standing 30min, is evaporated under reduced pressure and dries；
（2）Samples weighing after drying, is added the HBO of 0 ~ 5wt%3It is uniformly mixed, is put into high purity aluminium oxide crucible, 1200 ~
2 ~ 4h is calcined at 1500 DEG C, cooled to room temperature pulverizes and sieves, and obtains final products.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538464A (en) * | 2009-04-23 | 2009-09-23 | 江苏泽铭荧光材料有限公司 | Vacuum ultraviolet excited red fluorescent material and preparation method and application thereof |
| CN101694862B (en) * | 2009-10-27 | 2012-12-12 | 罗维鸿 | Warm white light light-emitting diode (LED) and lithium matter fluorescent powder thereof |
-
2018
- 2018-06-13 CN CN201810604872.7A patent/CN108531167A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538464A (en) * | 2009-04-23 | 2009-09-23 | 江苏泽铭荧光材料有限公司 | Vacuum ultraviolet excited red fluorescent material and preparation method and application thereof |
| CN101694862B (en) * | 2009-10-27 | 2012-12-12 | 罗维鸿 | Warm white light light-emitting diode (LED) and lithium matter fluorescent powder thereof |
Non-Patent Citations (1)
| Title |
|---|
| JINDENG CHEN ET AL.: "Near-infrared quantum cutting in Ce3+, Yb3+ co-doped YBO3 phosphors by cooperative energy transfer", 《OPTICAL MATERIALS》 * |
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Application publication date: 20180914 |