CN107129154B - Transparent glass ceramics material and preparation method for fluorescence temperature probe - Google Patents
Transparent glass ceramics material and preparation method for fluorescence temperature probe Download PDFInfo
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- CN107129154B CN107129154B CN201710529826.0A CN201710529826A CN107129154B CN 107129154 B CN107129154 B CN 107129154B CN 201710529826 A CN201710529826 A CN 201710529826A CN 107129154 B CN107129154 B CN 107129154B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
Abstract
The transparent glass ceramics material and preparation method thereof that the invention discloses a kind of for fluorescence temperature probe, the transparent glass ceramics material are to be doped with Yb containing equally distributed in oxide glass matrix3+And Er3+NaZnPO4Crystal has included at least Na in oxide glass matrix composition2O、ZnO、P2O5、B2O3And Sb2O3.The transparent glass ceramics material is prepared in raw material, and the preferred value of each oxide ratios is respectively as follows: the Na of 19~23mol%2O；The ZnO of 36~44mol%；The P of 26~32mol%2O5；The B of 8~10mol%2O3；The Sb of 0.9~1.1mol%2O3；The additional Yb for accounting for above-mentioned 0.5~1.5mol% of oxide aggregate2O3With the Er of 0.02~0.08mol%2O3.Transparent glass ceramics material disclosed by the invention is a kind of temperature measuring area of existing wide scope while the new material for fluorescence temperature probe for guaranteeing enough thermotonus sensitivity.
Description
Technical field
The invention belongs to solid luminescent material fields, and in particular to a kind of transparent glass ceramics for fluorescence temperature probe
Material.
Background technique
Currently, thermometry is broadly divided into contact and contactless temperature-measuring method.Contact temperature-measuring utilizes heat exchange
Realize thermal equilibrium condition, this measurement method needs are directly contacted with object under test, therefore will receive very big limitation,
And contactless temperature-measuring can then substitute conventional contact thermometric in some particular surroundings, complete contact temperature-measuring and be difficult to complete
Measurement work.
Occurring a kind of novel contactless temperature-measuring technology in recent years --- fluorescence temperature Detection Techniques, the technology use
Luminescent material carries out temperature sensing by measuring the photoluminescent property variation with temperature of material as temperature probe.It is this glimmering
The key point of light temperature detection technique is exactly the fluorescent material as temperature probe, it is however generally that, this fluorescent material must have
There are two the strength versus temperatures of above fluorescence emission peak, and different emission peaks different reactions；In addition, different emission peaks it
Between also to have certain wavelength interval, so as to discriminator signal.The presently disclosed fluorescent material as temperature probe, strong light
The sensitivity that degree varies with temperature is high not enough or temperature measuring area range is not wide enough.As Chinese patent CN106634988A is disclosed
A kind of nanocrystalline material for fluorescence temperature probe, under 980nm laser excitation, which shows respectively
Er3+Ion and Tm3+Simple spectrum band of the ion at 650nm and 800nm shines, as temperature gradually increases to 200 DEG C from 60 DEG C, Er3+
The fluorescence intensity that ion is located at 650nm is constant, and Tm 3+The fluorescence intensity that ion is located at 800nm gradually increases, sensitivity
For 1.73%K-1, temperature measuring area range is only 60~200 DEG C.
Summary of the invention
The purpose of the present invention is not high enough etc. for existing fluorescent material temperature measuring area narrow range or thermotonus sensitivity
Deficiency provides a kind of temperature measuring area of existing wide scope while guaranteeing enough thermotonus sensitivity, for fluorescence temperature probe
Transparent glass ceramics material and preparation method thereof.Material temperature measuring area provided by the invention range reaches 30~480 DEG C, sensitivity
Also 1~1.35%K has been reached-1。
Transparent glass ceramics material provided by the invention are as follows: be doped in oxide glass matrix containing equally distributed
Yb3+And Er3+NaZnPO4Crystal has included at least Na in oxide glass matrix composition2O、ZnO、P2O5、B2O3With
Sb2O3.The transparent glass ceramics material is prepared in raw material, and the preferred value of each oxide ratios is respectively as follows: 19~23mol%
Na2O；The ZnO of 36~44mol%；The P of 26~32mol%2O5；The B of 8~10mol%2O3；0.9~1.1mol%'s
Sb2O3；The additional Yb for accounting for above-mentioned 0.5~1.5mol% of oxide aggregate2O3With the Er of 0.02~0.08mol%2O3.By above-mentioned institute
Some powder material ground and mixeds are uniformly placed in crucible, are heated to 1300~1400 DEG C, keep the temperature 1~2 hour；Then by institute
Glass melts are quickly poured into the copper mold of 400~420 DEG C of preheatings and form and anneal to obtain host glass；Matrix glass after annealing
Glass continues to be allowed to that crystallization occurs within 2~6 hours in 560~600 DEG C of heat preservations.
Detailed description of the invention
Fig. 1 is the transmitted light spectrogram of sample of the embodiment of the present invention.
Fig. 2 is the X-ray diffractogram of sample of the embodiment of the present invention.
Fig. 3 is the transmission electron microscope photo of sample of the embodiment of the present invention.
Fig. 4 is the temperature associated transmissions spectrogram of sample of the embodiment of the present invention.
Fig. 5 is that the intensity ratio of sample of the embodiment of the present invention varies with temperature figure.
Specific embodiment
The present invention is described further combined with specific embodiments below.
Embodiment 1: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 1Yb2O3、0.05Er2O3After the proportion of (molar percentage) calculates weighing
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more, be subsequently placed in crucible, be heated in high temperature resistance furnace
2 hours are kept the temperature after 1300 DEG C, melts it sufficiently；Then, glass melts are quickly poured into the copper mold of 400 DEG C of preheatings and are shaped,
The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；By acquisition
Host glass is put into resistor furnace for heat treatment, is kept the temperature 4 hours at 580 DEG C, is obtained transparent glass ceramics.
Transmitted spectrum shows that glass ceramics has the high grade of transparency (Fig. 1)；X-ray diffractogram shows in oxide glass matrix
Middle precipitation NaZnPO4Crystal phase (Fig. 2)；Transmission electron microscope observing confirms there is NaZnPO largely having a size of 20nm or so in glass ceramics4
Particle is uniformly distributed in matrix (Fig. 3)；Fluorescence Spectrometer measurement obtains the related photic hair of the temperature under 980nm shooting condition
Spectrum (Fig. 4) is penetrated, may detect and be originated from2H11/2Energy level radiation transistion transmitting and4S3/2The radiation transistion of energy level emits.With temperature
Degree increases,2H11/2The radiation transistion emissive porwer of energy level increases sharply, and4S3/2The radiation transistion emissive porwer of energy level only occurs
Faint variation, using the two fluorescence intensity ratio as temperature measuring parameter (Fig. 5), in 303K~753K (30~480 DEG C) temperature range,
The sensitivity for obtaining glass ceramics is 1.35%K-1。
Embodiment 2: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 1.5Yb2O3、0.08Er2O3The proportion of (molar percentage), which calculates, to be weighed
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more, be subsequently placed in crucible, heated in high temperature resistance furnace
1 hour is kept the temperature after to 1400 DEG C, melts it sufficiently；Then, by glass melts be quickly poured into 400 DEG C preheating copper mold at
Shape；The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；It will obtain
The host glass obtained is put into resistor furnace for heat treatment, is kept the temperature 2 hours at 560 DEG C, is obtained transparent glass ceramics, after tested, glass
The sensitivity of ceramics is 1.28%K-1。
Embodiment 3: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 1Yb2O3、0.08Er2O3After the proportion of (molar percentage) calculates weighing
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more；It is subsequently placed in crucible, is heated in high temperature resistance furnace
1.5 hours are kept the temperature after 1400 DEG C, melts it sufficiently；Then, by glass melts be quickly poured into 400 DEG C preheating copper mold at
Shape；The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；It will obtain
The host glass obtained is put into resistor furnace for heat treatment, is kept the temperature 2 hours at 600 DEG C, is obtained transparent glass ceramics, after tested, glass
The sensitivity of ceramics is 1.15%K-1。
Embodiment 4: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 1.5Yb2O3、0.02Er2O3The proportion of (molar percentage), which calculates, to be weighed
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more；It is subsequently placed in crucible, is heated in high temperature resistance furnace
2 hours are kept the temperature after to 1400 DEG C, melts it sufficiently；Then, by glass melts be quickly poured into 400 DEG C preheating copper mold at
Shape；The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；It will obtain
The host glass obtained is put into resistor furnace for heat treatment, is kept the temperature 4 hours at 560 DEG C, is obtained transparent glass ceramics, after tested, glass
The sensitivity of ceramics is 1.0%K-1。
Embodiment 5: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 0.5Yb2O3、0.04Er2O3The proportion of (molar percentage), which calculates, to be weighed
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more；It is subsequently placed in crucible, is heated in high temperature resistance furnace
2 hours are kept the temperature after to 1300 DEG C, melts it sufficiently；Then, by glass melts be quickly poured into 400 DEG C preheating copper mold at
Shape；The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；It will obtain
The host glass obtained is put into resistor furnace for heat treatment, is kept the temperature 2 hours at 580 DEG C, is obtained transparent glass ceramics；After tested, glass
The sensitivity of ceramics is 1.12%K-1。
Embodiment 6: by Na2CO3、ZnO、NH4H2PO4、H3BO3、Sb2O3、Yb2O3、Er2O3Powder, by 21Na2O:40ZnO:
29P2O5: 9B2O3: 1Sb2O3(molar percentage), additional 1Yb2O3、0.05Er2O3After the proportion of (molar percentage) calculates weighing
It is placed in agate mortar, mixes it uniformly within grinding 1 hour or more；It is subsequently placed in crucible, is heated in high temperature resistance furnace
2 hours are kept the temperature after 1350 DEG C, melts it sufficiently；Then, glass melts are quickly poured into the copper mold of 400 DEG C of preheatings and are shaped；
The glass of forming is put into furnace cooling after annealing 10 hours in the Muffle furnace of 420 DEG C of heat preservations, obtains host glass；By acquisition
Host glass is put into resistor furnace for heat treatment, is kept the temperature 6 hours at 580 DEG C, is obtained transparent glass ceramics；After tested, glass ceramics
Sensitivity be 1.30%K-1。
In the various embodiments described above, 21Na2O:40ZnO:29P2O5: 9B2O3: 1Sb2O3The ratio of (molar percentage) not be
Unique limit value, as known to those skilled in the art, above-mentioned each component are the basic component for constituting host glass, each component ratio
Value change in ± 10% range be all it is feasible, can't have an adverse effect to final effect of the invention.
Claims (1)
1. a kind of preparation method of the transparent glass ceramics material for fluorescence temperature probe, including oxide glass matrix, institute
It states in oxide glass matrix and is doped with Yb containing equally distributed3+And Er3+NaZnPO4Crystal；It is characterized by: described
The preparation method of bright glass ceramic material includes at least following steps: with the Na of 19~23 mol%2O, 36~44 mol%
The P of ZnO, 26~32 mol%2O5, 8~10 mol% B2O3, 0.9~1.1 mol% Sb2O3For glass matrix raw material, upper
State the Yb of additional 0.5~1.5 mol% in the total amount of glass matrix raw material2O3With the Er of 0.02~0.08 mol%2O3；It will be above-mentioned
All powder material ground and mixeds are uniformly placed in crucible, are heated to 1300~1400 DEG C, keep the temperature 1~2 hour；Then will
Gained glass melts, which are quickly poured into, to be formed in the copper mold of 400~420 DEG C of preheatings and anneals to obtain host glass；Matrix after annealing
Glass continues to be allowed to that crystallization occurs within 2~6 hours in 560~600 DEG C of heat preservations.
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| CN108840571B (en) * | 2018-07-03 | 2020-12-29 | 中国科学院福建物质结构研究所 | Double-crystal-phase glass ceramic for fluorescent temperature probe and preparation method thereof |
| CN109912224B (en) * | 2019-01-26 | 2021-09-21 | 桂林电子科技大学 | Fluorapatite nano glass ceramic material for optical temperature measurement and preparation method thereof |
| CN110156332B (en) * | 2019-05-10 | 2021-12-07 | 福建江夏学院 | Transparent long-afterglow microcrystalline glass and preparation method thereof |
| CN110228948B (en) * | 2019-05-14 | 2021-11-16 | 重庆邮电大学 | Novel photoluminescence transparent glass ceramic and preparation method thereof |
| CN110894425A (en) * | 2019-11-27 | 2020-03-20 | 南京邮电大学 | Rare earth and metal ion doped phosphor with light temperature sensing and multiband light emission functions and preparation method thereof |
| CN114230182B (en) * | 2021-12-16 | 2023-12-01 | 桂林电子科技大学 | Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof |
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| CN102730975A (en) * | 2012-06-20 | 2012-10-17 | 武汉理工大学 | Glass-ceramic and preparation method thereof |
| CN105198225A (en) * | 2015-10-13 | 2015-12-30 | 杭州电子科技大学 | Double active ion doped bicrystal glass ceramic fluorescence temperature probe materials and preparation method thereof |
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| CN102730975A (en) * | 2012-06-20 | 2012-10-17 | 武汉理工大学 | Glass-ceramic and preparation method thereof |
| CN105198225A (en) * | 2015-10-13 | 2015-12-30 | 杭州电子科技大学 | Double active ion doped bicrystal glass ceramic fluorescence temperature probe materials and preparation method thereof |
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