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CN102173453A - Optical temperature sensor material Bi3TiNbO9:Er3+/Yb3+ and preparation method of Bi3TiNbO9:Er3+/Yb3+ film - Google Patents

Optical temperature sensor material Bi3TiNbO9:Er3+/Yb3+ and preparation method of Bi3TiNbO9:Er3+/Yb3+ film Download PDF

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CN102173453A
CN102173453A CN201110030003.6A CN201110030003A CN102173453A CN 102173453 A CN102173453 A CN 102173453A CN 201110030003 A CN201110030003 A CN 201110030003A CN 102173453 A CN102173453 A CN 102173453A
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tinbo
sensing material
temperature sensing
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陈恒智
杨彬
张明福
王竹
张锐
张治国
曹文武
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Harbin Institute of Technology
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Abstract

The invention relates to a preparation method of optical temperature sensor materials, in particular relates to an optical temperature sensor material Bi3TiNbO9:Er3+/Yb3+ and a preparation method of a Bi3TiNbO9:Er3+/Yb3+ film, and aims to provide an optical temperature sensor material with wide temperature measurement range, which can be applied to high-temperature environmental detection and low-temperature environmental measurement. The preparation method provided by the invention comprises the following steps of: feeding a ball-milled powdery mixture of Bi2O3, TiO2, Nb2O5, Er2O3 and Yb2O3 to a high-temperature furnace for pre-burning, then ball-milling, and finally sintering. The optical temperature sensor material Bi3TiNbO9:Er3+/Yb3+ has the advantages of wide temperature measurement range (working temperature range from 123 K to 693 K) and high measurement sensitivity (maximum sensitivity of 0.0032/K), and serves as an optical temperature sensor material with wide temperature measurement range which can be used in high-temperature environmental detection and low-temperature environmental measurement.

Description

Optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+And the preparation method of film
Technical field
The present invention relates to a kind of preparation method of optical temperature sensing material.
Background technology
The major cause that optic temperature sensor comes into the picture is to come from the optical waveguides that is used for signal transmission and the basic difference of plain conductor, and these differences have given optical pickocff following valuable characteristic: to little, safe, the remote sensing survey ability of insensitivity, size sensor of electricity and magnetic.But because the symmetric restriction of rare earth ion local, make Er 3+Adulterated material is luminous not to be very strong.And excite down Yb at near-infrared laser 3+Absorption cross will be much larger than Er 3+Absorption cross, Yb 3+Give Er with transmission ofenergy after absorbing photon energy 3+Thereby, increase up-conversion luminescence efficient greatly.People such as nineteen ninety-five Maciel mix Er in fluoride glass 3+Ion utilizes 2H 11/2With 4S 2/3The temperature variant characteristic of energy level emitted fluorescence strength ratio is prepared into the fluorescence temperature sensing material.Temperature-measuring range be 300K to 448K, the peak response of sensing material is 0.0040/K (Maciel G S et al.IEEE Photonic Tech.Lett., 1995,7 (12): 1474～1476) in this temperature range.People such as Dos Santos had prepared Er in 1998 3+The single doping and Er 3+, Yb 3+The chalcogenide glass temperature sensing material of codoped.Temperature-measuring range be 293K to 523K, Er in this scope 3+The single doping and Er 3+, Yb 3+The peak response of the chalcogenide glass temperature sensing material of codoped is respectively 0.0052/K and 0.0102/K (Dos SantosP V et al.Appl.Phys.Lett., 1998,73 (5): 578～580).People such as Li had prepared Er in 2007 3+, Yb 3+The chalcogenide glass temperature sensing material of codoped, temperature-measuring range be 300K to 723K, its peak response is 0.0033/K (Li C et al.Chem.Phys.Lett., 2007,443 (5): 426-429) in this temperature range.
Summary of the invention
The purpose of this invention is to provide a kind of wide temperature measurement range optical temperature sensing material that can be used for hot environment detection and low temperature environment measurement, that concrete is a kind of optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+And the preparation method of film.
Optical temperature sensing material Bi of the present invention 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 24～48 hours with 150 rev/mins～200 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.11～1.395: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.075～0.015, Er 2O 3With Yb 2O 3Mol ratio be 0.075～0.015: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3～4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 850 ℃～950 ℃ pre-burnings 2～3 hours, put into ball grinder with 150 rev/mins～200 rev/mins speed ball milling 24～48 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3～4 hours, get optical temperature sensing material Bi at 1000 ℃～1100 ℃ 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3～4: 1 in described mixed powder and the ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method of film is as follows: with above-mentioned optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Put into the vacuum chamber of pulse deposit system, then oxygen press to 13Pa～26Pa, underlayer temperature be under 550 ℃～600 ℃ the condition with excimer laser bombardment 30 minutes～60 minutes, promptly get optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Film.
Description of drawings
Fig. 1 is embodiment 13 gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve, ■ is optical temperature sensing material Bi under the condition of 693K among the figure 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve, is optical temperature sensing material Bi under the condition of 603K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve, be optical temperature sensing material Bi under the condition of 513K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve.Be optical temperature sensing material Bi under the condition of 423K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve, ▲ be optical temperature sensing material Bi under the condition of 333K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve, △ is optical temperature sensing material Bi under the condition of 243K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve,
Figure BDA0000045697340000021
Be optical temperature sensing material Bi under the condition of 153K 3TiNbO 9: Er 3+/ Yb 3+Fluorescence with the variation of temperature relation curve; Fig. 2 is embodiment 13 gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+ 2H 11/2→ 4I 15/2With 4S 3/2→ 4I 15/2Luminous integration beam intensity ratio is with variation of temperature figure, and ■ is an experimental data point among the figure ,-be matched curve; Fig. 3 is with embodiment 13 gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The temperature sensor sensitivity of preparation is with the variation of temperature curve.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 24～48 hours with 150 rev/mins～200 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.11～1.395: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.075～0.015, Er 2O 3With Yb 2O 3Mol ratio be 0.075～0.015: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3～4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 850 ℃～950 ℃ pre-burnings 2～3 hours, put into ball grinder with 150 rev/mins～200 rev/mins speed ball milling 24～48 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3～4 hours, get optical temperature sensing material Bi at 1000 ℃～1100 ℃ 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3～4: 1 in described mixed powder and the ball grinder.
Embodiment two: present embodiment and embodiment one are different be abrading-ball used in the step 1 ball grinder by diameter is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming.Other is identical with embodiment one.
Embodiment three: that present embodiment and embodiment one are different is Bi in the step 1 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Mol ratio be 1.395: 1: 0.5: 0.06: 0.075.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different be abrading-ball used in the step 2 ball grinder by diameter is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is in the step 2 mixed powder to be put into High Temperature Furnaces Heating Apparatus 860 ℃～920 ℃ pre-burnings.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is in the step 2 mixed powder to be put into High Temperature Furnaces Heating Apparatus 900 ℃ of pre-burnings.Other is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is in the step 2 thin slice to be put into High Temperature Furnaces Heating Apparatus to carry out sintering at 1050 ℃.Other is identical with embodiment one.
Embodiment eight: present embodiment optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method of film is as follows: with embodiment one gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Put into the vacuum chamber of pulse deposit system, then oxygen press to 13Pa～26Pa, underlayer temperature be under 550 ℃～600 ℃ the condition with excimer laser bombardment 30 minutes～60 minutes, promptly get optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Film.
The optical temperature sensing material Bi of gained in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The thickness of film is 650nm～1300nm.
Embodiment nine: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 24 hours with 150 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.11: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.075, Er 2O 3With Yb 2O 3Mol ratio be 0.075: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 850 ℃ of pre-burnings 2 hours, put into ball grinder with the speed ball milling of 150 rev/mins of clocks 24 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3 hours at 1000 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3: 1 in described mixed powder and the ball grinder.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Embodiment ten: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 48 hours with 200 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.395: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.015, Er 2O 3With Yb 2O 3Mol ratio be 0.015: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 950 ℃ of pre-burnings 3 hours, put into ball grinder with 200 rev/mins speed ball milling 48 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 4 hours at 1100 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 4: 1 in described mixed powder and the ball grinder.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Embodiment 11: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 28 hours with 160 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.11: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.075, Er 2O 3With Yb 2O 3Mol ratio be 0.075: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3～4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 880 ℃ of pre-burnings 2.3 hours, put into ball grinder with 160 rev/mins speed ball milling 28 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3.5 hours at 1050 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3.5: 1 in described mixed powder and the ball grinder.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Embodiment 12: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 30 hours with 180 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.395: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.015, Er 2O 3With Yb 2O 3Mol ratio be 0.015: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3.4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 900 ℃ of pre-burnings 2.8 hours, put into ball grinder with 180 rev/mins speed ball milling 30 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3.8 hours at 1080 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3.4: 1 in described mixed powder and the ball grinder.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Embodiment 13: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, with Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3According to mol ratio is 1.395: 1: 0.5: 0.06: 0.075 ratio weighing, put into ball grinder then and mixed in 24 hours with 150 rev/mins speed ball milling, mixed powder, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 900 ℃ of pre-burnings 3 hours, put into ball grinder with 150 rev/mins speed ball milling 24 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3 hours at 1050 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3: 1 in described mixed powder and the ball grinder.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.
Find out along with the radiationless relaxation benefit of the increase of temperature strengthens by Fig. 1, cause the absolute strength of up-conversion fluorescence to reduce.In order to contrast the relative intensity of fluorescence, we carry out normalization method to fluorescence spectrum.As can be seen after the normalization method, 2H 11/2→ 4I 15/2With 4S 4/2→ 4I 15/2The ratio of the fluorescent emission relative intensity of emission band increases along with the increase of temperature.This be because 2H 11/2With 4S 4/2Energy bite between the energy level is very for a short time to be the thermal coupling energy level, when temperature increases 4S 4/2Particle on the energy level helps being dealt into by heat shock 2H 11/2On the energy level.In this case, the emission of these two energy levels can be used formula (1) expression
R ≡ I H / I S = Cexp ( - ΔE k B T ) - - - ( 1 )
Δ E in the formula--- 2H 11/2With 4S 4/2Energy level spacing Δ E=E ( 2H 11/2)-E ( 4S 3/2);
k B---Boltzmann constant;
T---temperature;
C---the constant relevant with the life time of the level.
By Fig. 2 be 2H 11/2→ 4I 15/2With 4S 3/2→ 4I 15/2Luminous integration beam intensity ratio is with variation of temperature figure.Experimental data is carried out match, and the slope of matched curve is 646.5, and the value of C is 3.84.We are dR/dT=R (Δ E/k with sensitivity definition BT 2).
Fig. 3 adopts present embodiment gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The temperature sensor of preparation is in subzero 423 sensitivity of arriving in the 693K temperature range, and the sensitivity of temperature sensor reaches maximum value 0.0032/K when 324K.Present embodiment gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Compare with existing fluorescence temperature sensing material working parameter, having bigger operating temperature range is 123K～693K, and its sensitivity and existing temperature sensing material are comparable.And present embodiment gained optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The physical and chemical stability height, preserving property when helping device and in complex environment, working.
Embodiment 14: optical temperature sensing material Bi in the present embodiment 3TiNbO 9: Er 3+/ Yb 3+The preparation method of film is as follows: one, with Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3According to mol ratio is 1.395: 1: 0.5: 0.06: 0.075 ratio weighing, put into ball grinder then and mixed in 24 hours with 150 rev/mins speed ball milling, mixed powder, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 900 ℃ of pre-burnings 3 hours, put into ball grinder with 150 rev/mins speed ball milling 24 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3 hours at 1050 ℃, optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3: 1 in described mixed powder and the ball grinder; Three, with optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Put into the vacuum chamber of pulse deposit system, then oxygen press to 13Pa, underlayer temperature be under 600 ℃ the condition with excimer laser bombardment 60 minutes, promptly get optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Film.
Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the present embodiment step 1 ball grinder; Used abrading-ball is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter in the step 2 ball grinder.

Claims (8)

1. optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method as follows: one, weighing Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3, put into ball grinder then and mixed in 24～48 hours with 150 rev/mins～200 rev/mins speed ball milling, mixed powder, wherein Bi 2O 3, TiO 2With Nb 2O 5Mol ratio be 1.11～1.395: 1: 0.5, Nb 2O 5With Er 2O 3Mol ratio be 0.5: 0.075～0.015, Er 2O 3With Yb 2O 3Mol ratio be 0.075～0.015: 0.075, described Bi 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Total mass and ball grinder in the mass ratio of abrading-ball be 3～4: 1; Two, mixed powder is put into High Temperature Furnaces Heating Apparatus 850 ℃～950 ℃ pre-burnings 2～3 hours, put into ball grinder with 150 rev/mins～200 rev/mins speed ball milling 24～48 hours, and then be pressed into thin slice with the steel grinding tool, thin slice is put into High Temperature Furnaces Heating Apparatus carried out sintering 3～4 hours, get optical temperature sensing material Bi at 1000 ℃～1100 ℃ 3TiNbO 9: Er 3+/ Yb 3+, the mass ratio of abrading-ball is 3～4: 1 in described mixed powder and the ball grinder.
2. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that abrading-ball used in the step 1 ball grinder is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter.
3. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that Bi in the step 1 2O 3, TiO 2, Nb 2O 5, Er 2O 3And Yb 2O 3Mol ratio be 1.395: 1: 0.5: 0.06: 0.075.
4. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that abrading-ball used in the step 2 ball grinder is the agate ball of 20mm, agate ball that diameter is 10mm and the diameter agate ball that is 6mm according to 1: 10: 15 number than forming by diameter.
5. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that in the step 2 mixed powder being put into High Temperature Furnaces Heating Apparatus 860 ℃～920 ℃ pre-burnings.
6. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that in the step 2 mixed powder being put into High Temperature Furnaces Heating Apparatus 900 ℃ of pre-burnings.
7. according to the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method, it is characterized in that in the step 2 thin slice being put into High Temperature Furnaces Heating Apparatus carries out sintering at 1050 ℃.
8. optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method of film is characterized in that optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+The preparation method of film is as follows: with the described optical temperature sensing material of claim 1 Bi 3TiNbO 9: Er 3+/ Yb 3+Put into the vacuum chamber of pulse deposit system, then oxygen press to 13Pa～26Pa, underlayer temperature be under 550 ℃～600 ℃ the condition with excimer laser bombardment 30 minutes～60 minutes, promptly get optical temperature sensing material Bi 3TiNbO 9: Er 3+/ Yb 3+Film.
CN201110030003.6A 2011-01-27 2011-01-27 Optical temperature sensor material Bi3TiNbO9:Er3+/Yb3+ and preparation method of Bi3TiNbO9:Er3+/Yb3+ film Pending CN102173453A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
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CN106082338A (en) * 2016-06-13 2016-11-09 东北大学 A kind of nano-oxide Ti2nb10o29preparation method
CN106908168A (en) * 2017-02-19 2017-06-30 燕山大学 A kind of high sensitivity temperature sensing method based on neodymium ion near-infrared fluorescent
CN110078508A (en) * 2019-05-07 2019-08-02 哈尔滨工业大学 A kind of additive Mn niobium indium zincic acid lead-lead titanate piezoelectric ceramics, preparation method and applications
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
CN110926649A (en) * 2019-11-27 2020-03-27 燕山大学 High-sensitivity temperature measurement method based on different rare earth ion near-infrared fluorescence
CN116462506A (en) * 2023-04-14 2023-07-21 厦门乃尔电子有限公司 Bismuth layered ceramic with excellent high-temperature insulation and piezoelectricity and preparation method thereof

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CN106082338A (en) * 2016-06-13 2016-11-09 东北大学 A kind of nano-oxide Ti2nb10o29preparation method
CN106908168A (en) * 2017-02-19 2017-06-30 燕山大学 A kind of high sensitivity temperature sensing method based on neodymium ion near-infrared fluorescent
CN106908168B (en) * 2017-02-19 2018-12-28 燕山大学 A kind of highly sensitive temperature sensing method based on neodymium ion near-infrared fluorescent
CN110078508A (en) * 2019-05-07 2019-08-02 哈尔滨工业大学 A kind of additive Mn niobium indium zincic acid lead-lead titanate piezoelectric ceramics, preparation method and applications
CN110078508B (en) * 2019-05-07 2021-09-10 哈尔滨工业大学 Manganese-doped lead indium niobate zincate-lead titanate piezoelectric ceramic, and preparation method and application 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
CN110926649A (en) * 2019-11-27 2020-03-27 燕山大学 High-sensitivity temperature measurement method based on different rare earth ion near-infrared fluorescence
CN116462506A (en) * 2023-04-14 2023-07-21 厦门乃尔电子有限公司 Bismuth layered ceramic with excellent high-temperature insulation and piezoelectricity and preparation method thereof
CN116462506B (en) * 2023-04-14 2024-06-11 厦门乃尔电子有限公司 Bismuth layered ceramic with excellent high-temperature insulation and piezoelectricity and preparation method thereof

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