CN110511754A - A kind of tantalic acid alkali photostimulated phosphor and preparation method thereof - Google Patents
A kind of tantalic acid alkali photostimulated phosphor and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of tantalic acid alkali photostimulated phosphors and preparation method thereof, belong to field of inorganic materials.Tantalic acid alkali photostimulated phosphor provided by the invention, chemical structure expression formula are Li1‑xBixTaO3.The preparation method of tantalic acid alkali photostimulated phosphor provided by the invention, includes the following steps: S1, weighs raw material, and ethyl alcohol, grinding is added；S2, high temperature sintering, cooling；S3, be ground into powder to get.A kind of tantalic acid alkali photostimulated phosphor involved according to the present invention, after ultraviolet light irradiation fills energy, it can produce blue afterglow, it can produce high-intensitive short wavelength's blue optical stimulated luminescence by near-infrared laser irradiation, with instantaneity, high contrast and good repeatability, so can be realized the coupling of the multiple performances such as heat, light, electricity, can be used for advanced erasable formula high density large capacity optical information storage part and realizing the multipath write-in of optical information and read.
Description
Technical field
The present invention relates to a kind of photostimulated phosphors, and in particular to a kind of tantalic acid alkali photostimulated phosphor and its system
Preparation Method belongs to field of inorganic materials.
Background technique
The concept of light stimulus material is to be proposed by Lindmayer in 1988.Photostimulated phosphor belongs to special electricity
Muon capture material, can be irradiated by using suitable low energy rays is stimulated, and the electronics of capture is discharged into shallowly from deep trap
Trap (such as 980nm near infrared light or visible light).Electron capture material can be used for data encoding, thus light stimulus material is available
In the decoding of data, the write-in of optical information and reading, it is erasable with re-writable optical storage media in terms of have and widely answer
With prospect, thus gets the attention and study.Rare earth luminescence material have luminescent color it is rich and varied, it is with high purity,
The advantage that fluorescence lifetime range is wide, light conversion efficiency is high, thus with the high speed development of laser and optical storage technology, it is rear-earth-doped
Light stimulus material is applied the fields such as dose of radiation quantitative test, infrared band upper conversion imaging, infrared acquisition, optical storage
To being extensively studied.However, studying more rear-earth-doped light stimulus material at present is to utilize alkaline earth sulfide and halogenation
Object is made as host material incorporation rare earth element, these materials are not only poor in chemical stability, thermal stability, the feature of environmental protection
It is unfavorable for popularization and practical application for a long time, since single rare earth luminescence color is more single, to realize the tune of luminescent color
Section, it is also necessary to which a variety of rare earth ions of codope simultaneously accurately control proportion, thus traditional rare earth doping light stimulus material produces and makes
With the cost is relatively high.The tantalic acid based material of doped transition metal ions has chemistry steady compared with traditional light stimulus material
Qualitative feature high, preparation method is simple, thermal stability is good.Transition metal ions activator has emission spectra bandwidth, and color can
The advantages of tune, can be such that transition metal ions sensitizer realizes by the regulation of parent lattice local environment or co-dopant ions
Different colours from blue light to near-infrared shine, and are greatly expanded it in the range of signal of optical information storage.Therefore transition gold
Belong to ion doping light stimulus material has great potentiality in the exploitation of low cost new electron capture material.
Up to the present, people have developed the light stimulus material of tens of kinds of doped transition metal ions, comprising:
Sr2SnO4:Sb3+, SrGa2O4:Bi3+, ZnS:Cu+, ZnO-B2O3-SiO2:Mn2+Optical storage glass etc..The ZnS material of semi-conductor type
It is that current light stimulus is most outstanding, the light stimulus material that is most widely used, it has high sensitivity, optical stimulated luminescence intensity
Big feature.But the type host material needs easily to cause environmental pollution using sulfide as raw material during the preparation process,
And its property is also not so good as oxide type material settling out.Further, since thermal excitation luminescence phenomenon leads to the response of light stimulus material
Threshold value improves, poor to the excitation light detection effect of long wave segment limit, limits its practical application.
Summary of the invention
The present invention is to carry out to solve the above-mentioned problems, and it is an object of the present invention to provide a kind of tantalic acid alkali optical stimulated luminescence material
Material and preparation method thereof.
The present invention provides a kind of tantalic acid alkali photostimulated phosphors, have the feature that, chemical structure expression formula
For Li1-xBixTaO3(it is denoted as Li1-xTaO3: xBi), wherein 0 x≤0.10 <
In tantalic acid alkali photostimulated phosphor provided by the invention, it can also have the following features: and pass through high temperature
Solid phase method is sintered in air.
The present invention also provides a kind of preparation methods of tantalic acid alkali photostimulated phosphor, have a feature in that packet
Include following steps: step 1, weighing raw material containing Li by the molar ratio of Li, Bi, Ta element in chemical structural formula, raw material containing Bi with
And raw material containing Ta, it is added to the container, ethyl alcohol is then added, mixed grinding -2 hours 1 hour, obtains grinding powder；Step 2, will
Grinding powder be placed in crucible, in air atmosphere with 1 DEG C/min~5 DEG C/min heating rate be gradually warming up to 1000 DEG C-
1250 DEG C, high temperature sintering 8h~12h, in air atmosphere with 3 DEG C/min~10 DEG C/min rate of temperature fall be cooled to 200 DEG C~
With furnace natural cooling after 600 DEG C, bulk material is obtained；Step 3, bulk material is smashed and ground into 30min~60min powdering object,
Up to tantalic acid alkali photostimulated phosphor.
A kind of preparation method of tantalic acid alkali photostimulated phosphor provided by the invention, also has a feature in that it
In, raw material containing Li is Li2CO3。
A kind of preparation method of tantalic acid alkali photostimulated phosphor provided by the invention, also has a feature in that it
In, wherein raw material containing Bi is Bi2O3。
A kind of preparation method of tantalic acid alkali photostimulated phosphor provided by the invention, also has a feature in that it
In, raw material containing Ta is Ta2O5。
The action and effect of invention
A kind of tantalic acid alkali photostimulated phosphor involved according to the present invention, fills energy by 254nm ultraviolet light irradiation
Afterwards, it can produce blue afterglow, high-intensitive short wavelength's blue optical stimulated luminescence, tool can produce by near-infrared laser irradiation
There are instantaneity and high contrast, generates high-strength light excitation immediately in the case where motivating light action and emit and can maintain the long period, to remove
Light source is deactivated, optical stimulated luminescence rapidly disappears；Can visible near ultraviolet-- close, middle infrared band range excitation light generate sound
It answers；And there are high-intensitive blue optical stimulated luminescence, under the visible light stimulus of near ultraviolet-, light stimulus under near infrared light excitation
It shines quick disappearance and blue afterglow quenches simultaneously, there is good repeatability, need to only irradiate again and fill energy, more
It remains to restore optical stimulated luminescence intensity after secondary excitation, so tantalic acid alkali photostimulated phosphor provided by the invention has well
Piezoelectricity, photoelectricity, pyroelectric property, can be realized the coupling of the multiple performances such as heat, light, electricity, it is high to can be used for advanced erasable formula
Density large capacity optical information storage part and the multipath write-in and reading for realizing optical information.
A kind of preparation method of tantalic acid alkali photostimulated phosphor involved according to the present invention, because using traditional
High temperature solid phase synthesis is prepared in air, so, synthesis technology of the present invention is simple, preparation cost is cheap, advantages of nontoxic raw materials
And preparation process cleaning does not generate environmentally harmful product.
Detailed description of the invention
Fig. 1 is tantalic acid alkali photostimulated phosphor and LiTaO made from the embodiment of the present invention 3-53The XRD of crystal
The X ray diffracting spectrum of standard PDF card 29-0836；
Fig. 2 is the optical stimulated luminescence spectrogram for the tantalic acid alkali photostimulated phosphor that the embodiment of the present invention 4 provides；
Fig. 3 is the tantalic acid alkali photostimulated phosphor of the offer of the embodiment of the present invention 4 under near-infrared laser excitation
Luminous photo；And
Fig. 4 is the luminous intensity attenuation curve for the tantalic acid alkali photostimulated phosphor that the embodiment of the present invention 4 provides.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Examples and drawings are closed to be specifically addressed the present invention.
<embodiment 1>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.997Bi0.003TaO3It (is denoted as
Li0.997TaO3:0.003Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2210g Li is taken2CO3(purity 99.99%), 1.3258g Ta2O5(purity 99.99%) and
0.0045g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in corundum crucible, in air atmosphere gradually with the heating rate of 2.5 DEG C/min
1100 DEG C, high temperature sintering 10h are warming up to, with furnace nature after being cooled to 400 DEG C in air atmosphere with the rate of temperature fall of 7 DEG C/min
It is cooling, obtain bulk material；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 2>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.995Bi0.005TaO3It (is denoted as
Li0.995TaO3:0.005Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2206g Li is taken2CO3(purity 99.99%), 1.3257g Ta2O5(purity 99.99%) and
0.0070g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 3>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.993Bi0.007TaO3It (is denoted as
Li0.993TaO3:0.007Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2201g Li is taken2CO3(purity 99.99%), 1.3257g Ta2O5(purity 99.99%) and
0.0098g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 4>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.99Bi0.01TaO3It (is denoted as
Li0.99TaO3:0.01Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2195g Li is taken2CO3(purity 99.99%), 1.3258g Ta2O5(purity 99.99%) and
0.0141g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 5>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.97Bi0.03TaO3It (is denoted as
Li0.97TaO3:0.03Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2150g Li is taken2CO3(purity 99.99%), 1.3258g Ta2O5(purity 99.99%) and
0.0419g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 6>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.95Bi0.05TaO3It (is denoted as
Li0.95TaO3:0.05Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2106g Li is taken2CO3(purity 99.99%), 1.3257g Ta2O5(purity 99.99%) and
0.0700g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<embodiment 7>
A kind of tantalic acid alkali photostimulated phosphor, chemical structure expression formula are Li0.93Bi0.07TaO3It (is denoted as
Li0.93TaO3:0.07Bi)。
Tantalic acid alkali photostimulated phosphor provided in this embodiment the preparation method is as follows:
Step 1,0.2065g Li is taken2CO3(purity 99.99%), 1.3257g Ta2O5(purity 99.99%) and
0.0979g Bi2O3(purity 99.99%) is added in corundum crucible, and 10mL dehydrated alcohol is then added, mixed grinding 1 hour, obtains
Grind powder；
Step 2, grinding powder is placed in crucible, is gradually heated up in air atmosphere with the heating rate of 2.5 DEG C/min
To 1100 DEG C, high temperature sintering 10h, it is cooled in air atmosphere with the rate of temperature fall of 7 DEG C/min naturally cold with furnace after 400 DEG C
But, bulk material is obtained；
Step 3, by bulk material smashing and grinding 45min powdering object to get photostimulated phosphor.
<test case 1>
X-ray diffraction analysis is carried out to the tantalic acid alkali photostimulated phosphor that embodiment 3-5 is provided.
Fig. 1 is tantalic acid alkali photostimulated phosphor and LiTaO made from the embodiment of the present invention 3-53The XRD of crystal
The X ray diffracting spectrum of standard PDF card 29-0836.
As shown in Figure 1, the map and LiTaO of embodiment 3-5 tantalic acid alkali photostimulated phosphor3The XRD standard of crystal
The data of PDF card 29-0836 are consistent, and show to have synthesized single-phase LiTaO3Micron is brilliant, a small amount of doped transition metal ions
Fail that sample is made to generate apparent impurity phase or distortion of lattice.
<test case 2>
After filling energy by 254nm ultraviolet light irradiation to the tantalic acid alkali photostimulated phosphor that embodiment 4 provides, with
Its optical stimulated luminescence spectrogram is recorded after 980nm near-infrared laser excitation different time.
Fig. 2 is the optical stimulated luminescence spectrogram for the tantalic acid alkali photostimulated phosphor that the embodiment of the present invention 4 provides.
As shown in Fig. 2, the tantalic acid alkali photostimulated phosphor that embodiment 4 provides can generate response near infrared light,
And generate optical stimulated luminescence.
<test case 3>
After filling energy by 254nm ultraviolet light irradiation to the tantalic acid alkali photostimulated phosphor that embodiment 4 provides, with
980nm near-infrared laser motivates luminous photo after different time.
Fig. 3 is the tantalic acid alkali photostimulated phosphor of the offer of the embodiment of the present invention 4 under near-infrared laser excitation
Luminous photo.
As shown in figure 3, the tantalic acid alkali photostimulated phosphor that embodiment 4 provides can be with after ultraviolet light irradiation fills energy
Generate macroscopic bright blue optical stimulated luminescence, luminous intensity extends with irradiation time and decayed, when optical stimulated luminescence
Between can effectively maintain 60 seconds or so.
<test case 4>
The tantalic acid alkali photostimulated phosphor of the offer of embodiment 4 is recorded after 254nm ultraviolet light irradiation fills energy, in difference
The 430nm luminous intensity attenuation curve of wavelength light source.
Fig. 4 is the luminous intensity attenuation curve for the tantalic acid alkali photostimulated phosphor that the embodiment of the present invention 4 provides.
As shown in figure 4, bottom is shining under the tantalic acid alkali photostimulated phosphor Natural Attenuation that embodiment 4 provides
Intensity curve, centre are shining for the tantalic acid alkali photostimulated phosphor that the embodiment 4 under the irradiation of 365nm black light provides
Intensity curve, the top are the strong light for the tantalic acid alkali photostimulated phosphor that the embodiment 4 under 465nm blue light illumination provides
It writes music line, the results showed that the tantalic acid alkali photostimulated phosphor being irradiated after filling energy can be near ultraviolet to visible light wave range model
The light stimulus enclosed generates response, and afterglow can be made quickly to quench.
The action and effect of embodiment
A kind of tantalic acid alkali photostimulated phosphor, fills by 254nm ultraviolet light irradiation according to involved in the present embodiment
After energy, blue afterglow can produce, high-intensitive short wavelength's blue optical stimulated luminescence can produce by near-infrared laser irradiation,
With instantaneity and high contrast, generates high-strength light excitation immediately in the case where motivating light action and emits and can maintain the long period,
Excitation light source is removed, optical stimulated luminescence rapidly disappears；Can visible near ultraviolet-- close, middle infrared band range excitation light generate
Response；And have high-intensitive blue optical stimulated luminescence under near infrared light excitation, under the visible light stimulus of near ultraviolet-, light swashs
It encourages luminous quick disappearance and blue afterglow while quenching, there is good repeatability, need to only irradiate again and fill energy, In
It repeatedly remains to restore optical stimulated luminescence intensity after excitation, so tantalic acid alkali photostimulated phosphor provided in this embodiment has
Good piezoelectricity, photoelectricity, pyroelectric property can be realized the coupling of the multiple performances such as heat, light, electricity, can be used for advanced erasable
Formula high density large capacity optical information storage part and the multipath write-in and reading for realizing optical information.
A kind of preparation method of tantalic acid alkali photostimulated phosphor according to involved in the present embodiment, because using tradition
High temperature solid phase synthesis be prepared in air, so, the present embodiment synthesis technology is simple, preparation cost is cheap, raw material
The cleaning of nontoxic and preparation process does not generate environmentally harmful product.
Above embodiment is preferred case of the invention, the protection scope being not intended to limit the invention.
Claims (6)
1. a kind of tantalic acid alkali photostimulated phosphor, which is characterized in that chemical structure expression formula is Li1-xBixTaO3,
Wherein, 0 x≤0.10 <.
2. tantalic acid alkali photostimulated phosphor according to claim 1, it is characterised in that:
It is sintered in air by high temperature solid-state method.
3. the preparation method of tantalic acid alkali photostimulated phosphor of any of claims 1 or 2, it is characterised in that: including as follows
Step:
Step 1, raw material containing Li is weighed by the molar ratio of Li, Bi, Ta element in the chemical structural formula, raw material containing Bi and contain
Ta raw material, is added to the container, and ethyl alcohol is then added, mixed grinding -2 hours 1 hour, obtains grinding powder；
Step 2, the grinding powder is placed in crucible, in air atmosphere with 1 DEG C/min~5 DEG C/min heating rate by
Step is warming up to 1000 DEG C -1250 DEG C, high temperature sintering 8h~12h, with 3 DEG C/min~10 DEG C/min cooling speed in air atmosphere
Rate is cooled to after 200 DEG C~600 DEG C with furnace natural cooling, obtains bulk material；
Step 3, by bulk material smashing and grinding 30min~60min powdering object to get tantalic acid alkali optical stimulated luminescence material
Material.
4. the preparation method of tantalic acid alkali photostimulated phosphor according to claim 3, it is characterised in that:
Wherein, the raw material containing Li is Li2CO3。
5. the preparation method of tantalic acid alkali photostimulated phosphor according to claim 3, it is characterised in that:
Wherein, the raw material containing Bi is Bi2O3。
6. the preparation method of tantalic acid alkali photostimulated phosphor according to claim 3, it is characterised in that:
Wherein, the raw material containing Ta is Ta2O5。
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| CN114437721A (en) * | 2020-11-05 | 2022-05-06 | 中国科学院上海硅酸盐研究所 | Rare earth ion Tb3+Doped LiTaO3Multi-band emission pressure luminescent material and preparation method and application thereof |
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| CN114907847B (en) * | 2022-05-18 | 2023-01-03 | 五邑大学 | Fluorescent temperature measuring material and preparation method and application thereof |
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