CN108840571A - A kind of twin crystal phase glass ceramics and preparation method thereof for fluorescence temperature probe - Google Patents
A kind of twin crystal phase glass ceramics and preparation method thereof for fluorescence temperature probe Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention propose a kind of achievable efficient temperature detection containing CsPbBr3And EuPO4The glass ceramics and its technology of preparing of crystal phase.Glass ingredient is with percentage composition (mol%) in glass ceramics of the invention：10-60mol%P2O5；0-40mol%SiO2；0-40mol%Al2O3；0-30mol%Cs2CO3；0-30mol%PbBr2；0-30mol%SrCO3；5-30mol%NaBr；5-30mol%EuCl3, the moles total number of said components is 100mol%.The present invention also provides the technologies of preparing of this glass ceramics.Wavelength be 393 nanometers ultraviolet light irradiation under, Eu3+611nm at red emission band and CsPbBr3The fluorescence intensity ratio of green emissive band at 516nm varies with temperature the temperature detection that obviously can be realized certain temperature range.In 303-483K temperature range, CsPbBr3/EuPO4The highest absolute sensitivity of two-phase glass ceramics has reached 0.082K‑1, highest relative sensitivity reached 1.8%K‑1.Moreover, this material has good thermal stability, can recycled for multiple times.It is indicated above that CsPbBr3/EuPO4Two-phase glass ceramics is a kind of fluorescence temperature probe material of achievable efficient temperature detection.
Description
Technical field
The present invention relates to solid luminescent material fields, more particularly, to a kind of twin crystal that can be applied to fluorescence temperature probe
Phase glass ceramics and its preparation process.
Background technique
Temperature is most basic thermodynamic parameter, it plays important role in industry and technological applications.Traditional
Thermometric mode needs to contact with object under test, representative to have thermometer, thermocouple etc..But this contact temperature-measuring can change object
The actual temperature of body be easy to cause thermometric inaccurate.In addition to this, object test volume small object and fast moved,
Effect is also not fully up to expectations.Recently, fluorescence intensity ratio base temperature probe material receives the extensive concern of people, this kind of phosphor
Material belongs to contactless, has high measurement accuracy and spatial resolution, and can use in rugged environment.Preferably
There are two distinguishable emission peak, high sensitivity and excellent thermal stability for the fluorescence probe needs of fluorescence intensity ratio base.
Most of researchs concentrate on rare-earth fluorescent intensity than base fluorescence temperature probe, and what this was mainly utilized is that rare earth is abundant
Energy level.Traditionally, the thermal coupling energy level of single rare earth (Er, Tm, Ho) is to fluorescence intensity ratio base fluorescent probe is commonly used for, with temperature
The variation of degree, electronics move round about in the layout of thermal coupling energy level.But thermal coupling energy level holds medium and small energy gap difference
The overlapping of two monitoring emission peaks is easily caused, it is inaccurate so as to cause thermometric.In order to solve this problem, double launching centre rare earths/
Rear-earth-doped material is used as fluorescence temperature probe material by report.However, the characteristic of rare earth 4f-4f parity forbidden determines it
Low absorption cross-section and weak fluorescence intensity.In addition to this, the price of rare earth is more expensive.
Therefore, people have turned one's attention to semiconductor nano crystal class temperature-measurement material, it has big absorption cross-section, and high is glimmering
Light quantity subfield, high photostability and regulatable emission band.These excellent properties make them suited as fluorescence temperature
Spend probe material.But semiconductor nano is unstable, and be easy to be influenced by other outside environmental elements (such as PH
Value), it is unfavorable for the detection of temperature.
Currently, most of fluorescent materials based on fluorescence intensity ratio base are fluorescent powder and crystal.However, fluorescent powder is easy to dissipate
It penetrates, causes thermometric inaccurate；And the preparation process of crystal is complicated, and needs to take a substantial amount of time, and needs high cost.Recently
In the past few years, glass ceramics base fluorescence temperature-measurement material receives the concern of people, and not only technology of preparing is simple, it is raw to be easy to high-volume
It produces, can be processed into various shape, and there is excellent thermal stability, and can be recycled.These excellent properties make it
There is potential application prospect in fluorescence temperature probe field.
The present invention proposes a kind of two-phase glass ceramics and preparation method thereof for highly sensitive temperature detection.It is received 393
Under rice ultraviolet excitation, CsPbBr3/EuPO4Two-phase glass ceramics shows CsPbBr3And Eu3+Fluorescent emission band, main peak point
Not Wei Yu 516 nanometers green emissive band and 593 nanometers, 611 nanometers, the red emission band of 700 nanometers.In 303K-
In 483K temperature range, its alternating temperature emission spectra is measured, using Eu3+In 611 nanometers and CsPbBr3516 nanometers, two peaks
Fluorescence intensity ratio as temperature detection signal, clearly, the highest of this material is absolute for the fluorescence intensity ratio variation of the two
Sensitivity has reached 0.082K-1, highest relative sensitivity reached 1.8%K-1, higher than the fluorescence temperature spy of overwhelming majority report
Needle material.This novel CsPbBr3/EuPO4Two-phase glass ceramics is a kind of fluorescence temperature probe material haveing excellent performance.
Summary of the invention
The present invention relates to CsPbBr3/EuPO4The preparation of two-phase glass ceramics, it is therefore intended that prepare high sensitivity and excellent
Different thermal stability, can glass ceramics base fluorescence temperature probe material by burst of ultraviolel, for temperature detection.
Above-mentioned CsPbBr is additionally provided in the present invention3/EuPO4The preparation method of two-phase glass ceramics passes through rational design
Forerunner's glass ingredient, and melt supercooled technology is used, by preparing required glass ceramics from crystallization, in cooling procedure,
CsPbBr3And EuPO4Crystal grain is precipitated in glass matrix simultaneously, forms CsPbBr3/EuPO4Two-phase glass ceramics.The material can
Purple light excited, highest absolute sensitivity has reached 0.082K-1, highest relative sensitivity reached 1.8%K-1, can be effectively
Carry out temperature detection.
CsPbBr3/EuPO4The preparation method of two-phase glass ceramics, includes the following steps：
(1) design of forerunner's glass matrix, the glass matrix constituent content are as follows：
10-60mol%P2O5；0-40mol%SiO2；0-40mol%Al2O3；0-30mol%Cs2CO3；0-30mol%
PbBr2；0-30mol%SrCO3；5-30mol%NaBr；5-30mol%EuCl3, the moles total number of said components is
100mol%.
According to the present invention, the preferred content of each component is as follows：
P2O5Preferably 20-50mol%；
SiO2Preferably 5-30mol%；
Al2O3Preferably 5-30mol%；
Cs2CO3Preferably 5-25mol%；
PbBr2Preferably 5-25mol%；
SrCO3Preferably 5-25mol%；
NaBr is preferably 5-25mol%；
EuCl3Preferably 10-25mol%；
(2) by P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、SrCO3、NaBr、EuCl3Equal powder materials are according to certain component
Proportion weighs, and mixes and is fully ground in agate jar and is uniformly placed in alumina crucible, heats and at one section of heat preservation
Between be allowed to melt, then, melt liquid is poured into mold rapidly and is shaped, by from crystallization i.e. obtain both bulk glasses ceramics, most
Afterwards, the glass ceramics of acquisition is put into annealing in resistance furnace and after furnace cooling, is cut into bulk to eliminate internal stress；
According to the present invention, in step (2), 900-1300 DEG C, preferably 1000-1200 DEG C are heated in resistance furnace.Heat preservation
1-4 hours, melt powder material within preferably 1-3 hours.
According to the present invention, it in step (2), glass melt is taken out and is quickly poured into mold shapes, obtain both bulk glasses
Ceramics.
According to the present invention, in step (2), annealing temperature is 200-400 DEG C.
According to the present invention, in step (2), in temperature-rise period, control heating rate be 1-10 DEG C/min, preferably 2-5 DEG C/
min。
In the present invention, using the above material component and preparation process, it can obtain and inlay CsPbBr in glass matrix3/
EuPO4The glass ceramics of crystal grain.
The invention further relates to a kind of applications of glass ceramics, which is characterized in that the glass ceramics fluorescence temperature probe is answered
For temperature detection.
Under the excitation of 393 nano-ultraviolet lights, CsPbBr3/EuPO4Two-phase glass ceramics shows CsPbBr3And Eu3+It is glimmering
Light emitting band, main peak be located at 516 nanometers green emissive band and 593 nanometers, 611 nanometers, the strong feux rouges of 700 nanometers
Transmitting band.Using Eu3+In 611 nanometers and CsPbBr3516 two peaks of nanometers fluorescence intensity ratio as temperature detection believe
Number.In 303K-483K temperature range, the fluorescence intensity ratio variation of the two is clearly.CsPbBr3Fluorescence intensity decline it is non-
Chang Mingxian, and Eu3+Emissive porwer there was only slight decrease.Fluorescence intensity ratio under different temperatures passes through exponential fitting, highest
Absolute sensitivity has reached 0.082K-1, highest relative sensitivity reached 1.8%K-1, performance reported better than the overwhelming majority
Fluorescence temperature probe material.Temperature locating for environment can be obtained by the fluorescence intensity ratio of both measurements.Simultaneously with temperature
The change of degree, color become red from green, are conducive to remote reviewing.In addition to this, CsPbBr3/EuPO4Two-phase glass pottery
Porcelain is proven to have excellent thermal stability.These results indicate that CsPbBr3/EuPO4Two-phase glass ceramics is a kind of ideal
Fluorescence temperature probe material has broad application prospects in temperature detection field.
Detailed description of the invention
Fig. 1：CsPbBr3/EuPO4The X-ray diffractogram of two-phase glass ceramics.
Fig. 2：CsPbBr3/EuPO4Two-phase glass ceramics scanning electron microscope (SEM) photograph.
Fig. 3：CsPbBr3/EuPO4The excitation spectrum of two-phase glass ceramics, monitoring wavelength are 516nm, 611nm.
Fig. 4：Under 393nm excitation, CsPbBr3/EuPO4The emission spectrum of two-phase glass ceramics.
Fig. 5：CsPbBr3/EuPO4The alternating temperature emission spectrum of two-phase glass ceramics, temperature change 303K-483K, 393nm
Excitation.
Fig. 6：CsPbBr3(516nm) and Eu3+The Eu of ion3+：5D0→7F1(593nm),5D0→7F2(611nm),5D0→7F4
(700nm) transition emissive porwer histogram.
Fig. 7：The emissive porwer ratio FIR that experimental measurements and fitting obtain611/516With the relational graph of temperature.
Fig. 8：Absolute sensitivity, the relative sensitivity being calculated, with corresponding matched curve.
Specific embodiment
Example 1：By pure P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、SrCO3、NaBr、EuCl3Powder, by 30P2O5；
20SiO2；10Al2O3；10Cs2CO3；10PbBr2；5SrCO3；5NaBr；10EuCl3The proportion of (molar ratio) is weighed, in Ma
It mixes and is fully ground in Nao ball grinder and be uniformly placed in alumina crucible, be put into resistance furnace and be heated to 1000 DEG C, and protect
Temperature is allowed to melt for 2 hours, then, melt liquid is poured into mold rapidly and is shaped, by obtaining both bulk glasses from crystallization mode
Ceramics, finally, the glass ceramics of acquisition is put into resistance furnace, annealing is at 200 DEG C to eliminate internal stress, after furnace cooling,
It is cut into bulk, obtains CsPbBr3/EuPO4Twin crystal phase glass ceramics.
X ray diffracting data shows that CsPbBr has been precipitated in glass matrix3And EuPO4Crystal phase (as shown in Figure 1).Scanning
Electron micrograph shows CsPbBr3And EuPO4Distribution situation (as shown in Figure 2) of the crystal phase in glass matrix.Sample passes through table
Face polishing measures the excitation of its room temperature and transmitting with FLS920 Fluorescence Spectrometer.In monitoring Eu3+The excitation of 611 nanometer emission of ion
In spectrum, detect corresponding to Eu3+-O2-Charge migration and Eu3+：(the highest wavelength of intensity is located at 393 and receives for 4f → 4f absorptive transition
Rice) excitation band (as shown in Figure 3).In monitoring CsPbBr3516 nanometer emissions excitation spectrum on, detect corresponding CsPbBr3
The excitation band (as shown in Figure 4) of transition.On the emission spectra that 393 nanometers excite, occur corresponding to Eu3+:5D0→7FJ(J=1,2,
3,4) the strong red emission of transition (central wavelength corresponds respectively to 593 nanometers, 611 nanometers, 652 nanometers, 700 nanometers).?
Under the ultraviolet excitation that wavelength is 393 nanometers, its alternating temperature emission spectra is measured, range of temperature is 303K-483K.It observes
CsPbBr3Fluorescence intensity decline clearly, and Eu3+Emissive porwer there was only slight decrease (as shown in Figure 5).?
CsPbBr3And Eu3+(as shown in Figure 6) can be further confirmed in ion transition emissive porwer histogram.Eu3+In 611 nanometers and
CsPbBr3The fluorescence intensity ratio at 516 two peaks of nanometers vary with temperature obvious (as shown in Figure 7).Utilize the fluorescence of the two
Intensity ratio has reached 0.082K as temperature detection signal, highest absolute sensitivity-1, highest relative sensitivity reached 1.8%
K-1(as shown in Figure 8).
Example 2：By pure P2O5、SiO2、Al2O3、Cs2CO3、PbBr2、EuCl3Powder, by 20P2O5；20SiO2；
10Al2O3；20Cs2CO3；20PbBr2；10EuCl3The proportion of (molar ratio) is weighed, and is mixed in agate jar and abundant
Grinding is uniformly placed in alumina crucible, is put into resistance furnace and is heated to 1300 DEG C, and keeps the temperature 2 hours and be allowed to melt, then,
Melt liquid is poured into mold rapidly and is shaped, by obtaining both bulk glasses ceramics from crystallization mode, finally, by the glass of acquisition
Ceramics are put into resistance furnace, and annealing after furnace cooling, is cut into bulk, obtains CsPbBr at 200 DEG C to eliminate internal stress3/EuPO4
Twin crystal phase glass ceramics.The alternating temperature emission spectra of twin crystal phase glass ceramics is tested, and utilizes Eu3+In 611 nanometers and CsPbBr3's
For the fluorescence intensity ratio at 516 two peaks of nanometers as temperature detection signal, highest absolute sensitivity has reached 0.064K-1, highest
Relative sensitivity has reached 1.5%K-1。
Example 3：By pure P2O5、Al2O3、Cs2CO3、PbBr2、NaBr、EuCl3Powder, by 40P2O5；5Al2O3；
15Cs2CO3；10PbBr2；10NaBr；20EuCl3The proportion of (molar ratio) is weighed, and is mixed in agate jar and abundant
Grinding is uniformly placed in alumina crucible, is put into resistance furnace and is heated to 900 DEG C, and keeps the temperature 4 hours and be allowed to melt, then,
Melt liquid is poured into mold rapidly and is shaped, by obtaining both bulk glasses ceramics from crystallization mode, finally, by the glass of acquisition
Ceramics are put into resistance furnace, and annealing after furnace cooling, is cut into bulk, obtains CsPbBr at 300 DEG C to eliminate internal stress3/
EuPO4Twin crystal phase glass ceramics.The alternating temperature emission spectra of twin crystal phase glass ceramics is tested, and utilizes Eu3+In 611 nanometers and
CsPbBr3516 two peaks of nanometers fluorescence intensity ratio as temperature detection signal, highest absolute sensitivity reaches
0.036K-1, highest relative sensitivity reached 1.2%K-1。
Example 4：By pure P2O5、SiO2、Cs2CO3、PbBr2、NaBr、SrCO3、EuCl3Powder, by 10P2O5；40SiO2；
20Cs2CO3；10PbBr2；10NaBr；5SrCO3；5EuCl3The proportion of (molar ratio) is weighed, and is mixed in agate jar
And be fully ground and be uniformly placed in alumina crucible, it is put into resistance furnace and is heated to 1400 DEG C, and keep the temperature 4 hours and be allowed to molten
Melt, then, melt liquid is poured into mold rapidly and is shaped, by obtaining both bulk glasses ceramics from crystallization mode, finally, will obtain
The glass ceramics obtained is put into resistance furnace, and annealing after furnace cooling, is cut into bulk, is obtained at 400 DEG C to eliminate internal stress
CsPbBr3/EuPO4Twin crystal phase glass ceramics.The alternating temperature emission spectra of twin crystal phase glass ceramics is tested, and utilizes Eu3+In 611 nanometers
Place and CsPbBr3516 two peaks of nanometers fluorescence intensity ratio as temperature detection signal, highest absolute sensitivity reaches
0.022K-1, highest relative sensitivity reached 0.8%K-1。
Claims (5)
1. a kind of glass matrix, it is characterised in that：The glass ingredient content of the glass matrix is as follows：
10-60mol%P2O5；0-40mol%SiO2；0-40mol%Al2O3；0-30mol%Cs2CO3；0-30mol%PbBr2；
0-30mol%SrCO3；5-30mol%NaBr；5-30mol%EuCl3, the moles total number of said components is 100mol%.
2. glass matrix according to claim 1, it is characterised in that：The glass ingredient preferred content of the glass matrix is as follows：
20-50%mol%P2O5；5-30mol%SiO2；5-30mol%Al2O3；5-25mol%Cs2CO3；5-25mol%
PbBr2；5-25mol%SrCO3；5-25mol%NaBr；10-25mol%EuCl3。
3. one kind contains CsPbBr3/EuPO4The glass ceramics of twin crystal phase, the glass matrix of the glass ceramics such as claim 1 institute
It states.
4. CsPbBr according to claim 33/EuPO4Glass ceramics, which is characterized in that micro-structural feature CsPbBr3/
EuPO4Crystallite is uniformly embedded in the glass matrix.
5. the CsPbBr of any one of claim 3-4 a kind of3/EuPO4The application of twin crystal phase glass ceramics, it is characterised in that:Use wave
The ultraviolet light CsPbBr of a length of 393nm3/EuPO4Twin crystal phase glass ceramics, temperature are increased to 483K from 303K, material
CsPbBr3Green emission intensity decline clearly, Eu3+Red light emitting intensity only slightly weaken, fluorescence is from green light
Become feux rouges, CsPbBr3(516 nanometers) and Eu3+：5D0→7F2The fluorescence intensity ratio of (611 nanometers) transmittings varies with temperature bright
It is aobvious, using the fluorescence intensity ratio of the two as temperature detection signal, so that it may measure environment temperature.
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| CN111732341A (en) * | 2020-07-03 | 2020-10-02 | 福建师范大学 | Double-crystal-phase microcrystalline glass material and preparation method thereof |
| CN112322287A (en) * | 2020-10-16 | 2021-02-05 | 厦门华厦学院 | Temperature sensing material and preparation method and application thereof |
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