CN107474834A - A kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof - Google Patents

A kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof Download PDF

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CN107474834A
CN107474834A CN201710309955.9A CN201710309955A CN107474834A CN 107474834 A CN107474834 A CN 107474834A CN 201710309955 A CN201710309955 A CN 201710309955A CN 107474834 A CN107474834 A CN 107474834A
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elastic stress
stress
brightness
luminescent material
raw material
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张君诚
范新华
潘聪
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Qingdao University
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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    • C09K11/7703Chalogenides with alkaline earth metals

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Abstract

The present invention relates to a kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof, the material is with Ca3Ti2O7For matrix, with Pr3+For activator, its chemical expression is (Ca1‑ xMx)3‑z(Pr1‑yRy)zTi2O7, wherein 0≤x≤0.2,0≤y≤0.4, one or more of 0 the < z≤0.02, M in Mg, Sr, Ba, the one kind of R in Dy, Sm, Ho, x, y, z represent molar content.Material is synthesized in atmosphere using two step high temperature solid-state methods.The advantage of the invention is that:(1) material preparation method is simple to operation;(2) material prepared under mechanism stimulation there is strong elastic stress to light, and with the naked eye bright red emission is can observe in dark surrounds;(3) material is with a wide range of applications in various fields such as strain gauge, display, mechanical position, Architectural Equipment and entertainment devices.

Description

A kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof
Technical field
The invention belongs to stress irradiance functional material science and technology field, and being related to a kind of titanate red high brightness elasticity should Power luminescent material and preparation method thereof.
Background technology
Stress irradiance is to act on solid material by mechanical stress and cause its luminous phenomenon.This mechanical stress can be with It is the forms such as fracture, friction, extruding, shock, splitting.Stress light emitting material can be divided into bursting stress and light according to solid deformation Material and non-demolition stress light emitting material;Rather than bursting stress luminescent material can be divided into elastic stress luminescent material again and plasticity should Power luminescent material.Luminous elastic stress is to apply mechanical stress to it in elastic properties of materials deformation limit to make it luminous, and is had The characteristics of luminous intensity is directly proportional to applied stress.Meanwhile elastic stress luminescent material have repeatability, luminous intensity it is high, The advantages that summary responses, stress response are high regular.Therefore, elastic stress luminescent material pressure sensor, self-diagnosable system, The various fields performances such as artificial skin, City Building are taken precautions against natural calamities and the stress distribution of disaster reduction system, building and machine detects Go out good application prospect.Because the research for elastic stress luminescent material is shorter, only decades, the high-performance developed The luminous number of materials of elastic stress is limited, includes ZnS:Mn2+、Ca2Al2SiO7:Ce3+、SrAl2O4:Eu2+、SrAl2O4:Eu2 +, Dy3+、BaTiO3-CaTiO3:Pr3+、SrAl2O4:Ce3+、SrAl2O4:Ce3+, Ho3+、CaMgSi2O7:Eu2+, and LiNbO3: Pr3+Etc. material few in number.Wherein SrAl2O4:Eu2+, Dy3+Material shows excellent elastic stress luminescent properties, still Shortcoming is promoted and applied it is also clear that greatly reducing its commercialization, such as preparation technology complexity is, it is necessary under reducing atmosphere Sintering;Chemical property is not sufficiently stable, facile hydrolysis;Persistence is grown, and influences the display of stress irradiance.Therefore, preparation technology is developed Simply, the stable high brightness elastic stress luminescent material of chemical property is still a hot issue.It is an object of the invention to solve Certainly some drawbacks existing for current material, seek a kind of titanate red high-brightness elastic stress luminescent material and its preparation side Method, material high temperature process heat under air ambient, chemical property is stable, and elastic stress luminous intensity is high.
The content of the invention
It is an object of the invention to disclose a kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof. The material is with Ca3Ti2O7For matrix, with Pr3+For activator, its chemical expression is (Ca1-xMx)3-z(Pr1-yRy)zTi2O7, its In the one or more of the < of 0≤x≤0.2,0≤y≤0.4,0 z≤0.02, M in Mg, Sr, Ba, R is in Dy, Sm, Ho One kind, x, y, z represent molar content.
Titanate red high-brightness elastic stress luminescent material disclosed in this invention is using two step high temperature solid-state methods in sky Synthesized in gas.Preparation process comprises the following steps:
A) appropriate amount of deionized water or absolute ethyl alcohol are added, after being fully ground than weighing raw material respectively by element chemistry metering Drying obtains mixed powder;
B) by the pre-burning at 700~1100 DEG C in atmosphere of the powder obtained by step a), pre-burning soaking time is 2~7 small When;
C) after the pre-burning product after cooling is ground, calcined in atmosphere at 1200~1400 DEG C, sintering soak Time is 3~7 hours;
D) ground after the calcined product that step c) is obtained is cooled down, it is small in 1500~1600 DEG C of calcinings 3~7 in atmosphere When;
E) pulverized after the calcined product that step d) is obtained is cooled down and obtain titanate red high-brightness elastic stress Luminescent material.
Prepare titanate red high-brightness elastic stress luminescent material method, it is characterised in that Ca, Mg, Sr and Ba are used Its oxide or carbonate are raw material, and Ti uses its oxide as raw material, and Pr and R use its oxide, nitrate or carbonate For raw material.
By obtained titanate red high-brightness elastic stress luminescent material powder and optically transparent organic polymer bullet Property material (such as ABS resin, polyacetals (PA), makrolon (PC), polyethylene (PE), polystyrene (PS), polypropylene (PP), Polymethyl methacrylate (PMMA), polyurethane resin, polyester, epoxy resin, silicon rubber etc.) it is mixed and made into thin slice or cylindrical type Resinite or coated on the parts to be tested surface, can be converted to luminous energy by mechanical stress suffered by the part, realize that stress distribution is examined Survey.
Titanate red high-brightness elastic stress luminescent material obtained by the present invention, it is characterised in that the bullet of the material Property stress irradiance peak be wire peak near 615nm, monochromaticjty is good.
Titanate red high-brightness elastic stress luminescent material obtained by the present invention, it is characterised in that material is in machinery Effect under stimulating there is strong elastic stress to light, and bright red emission is with the naked eye can observe under dark surrounds.
Titanate red high-brightness elastic stress luminescent material obtained by the present invention, it is characterised in that material belongs to sunken Trap control type luminescent material, its elastic stress lights can recover after ultraviolet light irradiation, belong to non-demolition stress light emitting material.
Beneficial effects of the present invention are:
(1) prepared by material of the present invention uses traditional solid phase reaction method, preparation technology is simple, prepared under air atmosphere, Condition is easily controlled, equipment requirement is low, cost is cheap, is generated in preparation process without toxic gas, environmentally safe.
(2) obtained elastic stress luminescent material and optically transparent macromolecular material are mixed and made into thin slice or circle Column type resinite, also or coated on the parts to be tested surface, can by its suffered mechanical external force (pressure, pulling force, frictional force, impulsive force, Shearing force, distortion power, elastic force, ultrasound etc.) be converted to luminous energy and send.
(3) the titanate red high-brightness elastic stress luminescent material prepared by the present invention has strong elastic stress hair Light, directly it can be seen compared with dark situation by human eye.
(4) luminous intensity of titanate red high-brightness elastic stress luminescent material of the present invention, dependent on exciting The mechanical energy size in source.The luminous intensity of the material typically increases with the rise of mechanicals efforts, thus is causing light to be sent out Exist in the mechanical interaction power penetrated it is minimum can value, or stress threshold, the threshold value dominated by material component change.The material Expect the width of mechanical stress scope that can be responded, the energy that can destroy material structure is increased to from the weak stress of several newton to applying It can be made to produce stress irradiance.Titanate red high-brightness elastic stress luminescent material of the present invention and its composite As long as it can be lighted in the outside external force for applying very little, and in elastic deformation area, luminous intensity is with stress intensity into just Than relation, stress distribution detection can be achieved.
(5) the luminous decay of afterglow of the elastic stress of titanate red high-brightness elastic stress luminescent material of the present invention It hurry up.Stress apply terminate after, stress irradiance twilight sunset rapidly disappears (millisecond magnitude), the stress irradiance halation being visible by naked eyes and by Power track, measure of the performance without prejudice to material to follow-up weak stress.The elastic stress luminescent material can be used for part and structure The monitoring in real time of the stress distribution of part and adhesive strength measurement.
(6) titanate red high-brightness elastic stress luminescent material of the present invention, can be widely applied to pressure sensing Device, mechanical stress visualization, artificial skin, smart skins, self-diagnosable system, ultraprecise device fabrication, organism, building and The stress distribution detection of machine, City Building is taken precautions against natural calamities and disaster reduction system, prediction earthquake generation, the damage for detecting aircraft and automobile Evil, research human body diseases.
Brief description of the drawings
Fig. 1 is the x-ray diffractogram of powder of the sample of the embodiment of the present invention 1.
Fig. 2 is the excitation spectrum (monitoring 615nm red emissions) of the sample of the embodiment of the present invention 1.
Fig. 3 is the emission spectrum (excitation wavelength 327nm) of the sample of the embodiment of the present invention 1.
Fig. 4 is the elastic stress luminescent spectrum of the sample of the embodiment of the present invention 1.
Fig. 5 is the elastic stress luminous intensity of the embodiment of the present invention 1 with the change curve of pressure load.
Fig. 6 is elastic stress luminosity curve of the embodiment of the present invention 1 under rubbing action.
Fig. 7 is the Thermo-luminescence of the sample of the embodiment of the present invention 1
Embodiment
Below by way of particular specific embodiment and with reference to accompanying drawing, the present invention will be described in more detail.It should be understood that this A little examples are only illustrative of the invention and is not intended to limit the scope of the invention;It should also be understood that one or more that the present invention mentions Individual method and step does not repel also has other method and steps before and after the combination step, or these are specifically mentioned the step of Other method and steps can also be inserted before.Moreover, unless otherwise indicated, the numbering of various method steps is only to differentiate each method step Rapid convenient tool, rather than ordering or the enforceable scope of the restriction present invention for limitation various method steps, it is closed relatively System is altered or modified, in the case where changing technology contents without essence, when being also considered as enforceable category.
Specifically, table 1 lists material component, raw material weight, sintering temperature and the bullet of 9 specific embodiments of the present invention Property stress irradiance performance.
Material component, raw material weight, sintering temperature and the elastic stress luminescent properties of the embodiment 1-9 samples of table 1..
Embodiment 1. prepares titanate red high-brightness elastic stress luminescent material Ca2.991Pr0.009Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 900 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is Ca the product after cooling to be pulverized and obtain chemical constituent2.995Pr0.005Ti2O7Elastic stress hair Luminescent material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
The outer light of titanate red high-brightness elastic stress luminescent material that the example is prepared is white, and x-ray powder spreads out (XRD) test result is penetrated as shown in figure 1, the diffraction peak data and Ca of products obtained therefrom3Ti2O7Powder diffraction standard card (89- 1384) diffraction data is consistent, and without dephasign, illustrates the Ca that gained luminescent material is pure phase3Ti2O7Structure.It is red to monitor 615nm Photoemissive excitation spectrum is as shown in Fig. 2 the excitation spectrum of the material is made up of in the range of 200~550nm a series of peaks, most Strong peak is located at 327nm, and other peaks are located at 457nm, 476nm, 493nm.Fig. 3 is transmitting of the material under 327nm exciting lights Spectrum, emission spectrum come from Pr by 615nm3+Single wire peak composition.Fig. 4 is the elastic stress luminescent spectrum of the material, Emission spectrum comes from Pr by 615nm3+Single wire peak composition, it is consistent with photoluminescence spectra.Fig. 5 is the elasticity of the material Stress irradiance intensity with pressure load change curve.Fig. 6 is elastic stress luminosity curve of the material under rubbing action.Figure 7 compose for the thermoluminescence of the material, a strong thermal glow peak in the range of 25~225 DEG C be present, show that material belongs to trap control Type luminescent material processed, its elastic stress luminous intensity can be recovered after ultraviolet light irradiation, belong to non-demolition stress light emitting material.
Embodiment 2. prepares titanate red high-brightness elastic stress luminescent material Ca2.998Pr0.002Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 1000 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1350 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is Ca the product after cooling to be pulverized and obtain chemical constituent2.998Pr0.002Ti2O7Elastic stress hair Luminescent material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 3. prepares titanate red high-brightness elastic stress luminescent material Ca2.99Pr0.01Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 850 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1600 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is Ca the product after cooling to be pulverized and obtain chemical constituent2.99Pr0.01Ti2O7Elastic stress light Material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 4. prepares titanate red high-brightness elastic stress luminescent material (Ca0.97Ba0.03)2.995Pr0.005Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 900 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is (Ca the product after cooling to be pulverized and obtain chemical constituent0.97Ba0.03)2.995Pr0.005Ti2O7Bullet Property stress light emitting material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 5. prepares titanate red high-brightness elastic stress luminescent material (Ca0.95Sr0.05)2.997Pr0.003Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 950 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is (Ca the product after cooling to be pulverized and obtain chemical constituent0.95Sr0.05)2.997Pr0.003Ti2O7Bullet Property stress light emitting material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 6. prepares titanate red high-brightness elastic stress luminescent material (Ca0.94Mg0.03Sr0.03)2.99Pr0.01Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 900 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1350 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is (Ca the product after cooling to be pulverized and obtain chemical constituent0.94Mg0.03Sr0.03)2.99Pr0.01Ti2O7 Elastic stress luminescent material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 7. prepares titanate red high-brightness elastic stress luminescent material Ca2.994(Pr0.9Dy0.1)0.006Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 800 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1350 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1500 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is Ca the product after cooling to be pulverized and obtain chemical constituent2.994(Pr0.9Dy0.1)0.006Ti2O7Bullet Property stress light emitting material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 8. prepares titanate red high-brightness elastic stress luminescent material (Ca0.95Mg0.05)2.99 (Pr0.7Sm0.3)0.01Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 900 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1600 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is (Ca the product after cooling to be pulverized and obtain chemical constituent0.95Mg0.05)2.99(Pr0.7Sm0.3)0.01Ti2O7Elastic stress luminescent material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
Embodiment 9. prepares titanate red high-brightness elastic stress luminescent material (Ca0.92Mg0.04Sr0.04)2.988 (Pr0.6Ho0.4)0.012Ti2O7
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is placed into alumina crucible In in air atmosphere at 950 DEG C pre-burning 4 hours;
(2) it is positioned over after the powder after pre-burning is fully ground in aluminum oxide Noah's ark, with 4 DEG C/min's under atmospheric environment Heating rate is warming up to 1400 DEG C of calcinations 6 hours, cools with stove;
(3) it is placed in after the product after cooling is fully ground in aluminum oxide Noah's ark, with 3 DEG C/min liter under atmospheric environment Warm speed is warming up to 1550 DEG C of calcinations 6 hours, is cooled to 300 DEG C with 5 DEG C/min rate of temperature fall, furnace cooling;
(4) it is (Ca the product after cooling to be pulverized and obtain chemical constituent0.92Mg0.04Sr0.04)2.988 (Pr0.6Ho0.4)0.012Ti2O7Elastic stress luminescent material;
(5) it is the powder after sieving and optically transparent organic resin macromolecular material polyurethane resin is mixed with 1: 9 Close, diameter 2cm is made, thickness is 1cm cylindrical type resinite, the elastic stress luminescent properties for test sample.
The titanate red high-brightness elastic stress luminescent material that above-described embodiment 2-9 is prepared is white, x-ray powder Diffraction (XRD) test result is identical with the sample of embodiment 1, the diffraction peak data and Ca of products obtained therefrom3Ti2O7Powder diffraction standard The diffraction data of card (89-1384) is consistent, and without dephasign, illustrates the Ca that gained luminescent material is pure phase3Ti2O7Structure.Implement The excitation spectrum and emission spectrum of example 2-9 samples are consistent with the peak type and peak position of the sample of embodiment 1, are only that peak intensity is present not Together.The elastic stress luminescent spectrum of embodiment 2-9 samples is consistent with the peak type and peak position of the sample of embodiment 1, is only that peak intensity is deposited In difference.Elastic stress luminosity curve of the embodiment 2-9 samples under compression and rubbing action is similar to the sample of embodiment 1, only It is that relative intensity has difference, each sample is respectively provided with strong elastic stress luminous intensity, can with the naked eye seen under dark surrounds Bright red emission is measured, elastic stress luminous intensity strengthens with the increase for applying pressure load, and in pressure load most The elastic stress of strength is luminous the most obvious.During the release of pressure load, the luminous rapid decay of material.Embodiment 2- All there is strong thermal glow peak in 9 samples, show that material belongs to trap control type luminescent material in the range of 25-225 DEG C, its elasticity Stress irradiance intensity can be recovered after ultraviolet light irradiation, belong to non-destructive stress light emitting material.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation, Other substantially equivalent replacements that those skilled in that art are contemplated that, all fall in the scope of protection of the present invention.

Claims (3)

1. a kind of titanate red high-brightness elastic stress luminescent material, it is characterised in that with Ca3Ti2O7For matrix, with Pr3+For Activator, its chemical expression are (Ca1-xMx)3-z(Pr1-yRy)zTi2O7, wherein 0≤x≤0.2,0≤y≤0.4,0 < z≤ 0.02, M represents molar content selected from one or both of Mg, Sr, Ba, the one kind of R in Dy, Sm, Ho, x, y, z; The elastic stress glow peak of the material is the wire peak near 615nm, and monochromaticjty is good;Material has under mechanism stimulation There is strong elastic stress to light, red stress irradiance can use naked-eye observation under dark surrounds;The elastic stress of material lights It can recover after ultraviolet light irradiation, belong to trap control type non-demolition stress light emitting material;The material with it is optically transparent organic high After molecular elastic material mixing, laminate or cylindrical type resinite or coated on the parts to be tested surface, can should by suffered machinery Power is converted to luminous energy, realizes that stress distribution detects.
2. the preparation method of titanate red high-brightness elastic stress luminescent material as claimed in claim 1, it is characterised in that Ca, Mg, Sr and Ba use its oxide or carbonate as raw material, and Ti uses its oxide as raw material, and Pr and R are aoxidized using it Thing, nitrate or carbonate are raw material, are prepared using two step high temperature process heat methods, and preparation process comprises the following steps:
A) appropriate amount of deionized water or absolute ethyl alcohol are added, is dried after being fully ground than weighing raw material respectively by element chemistry metering Obtain mixed powder;
B) by the pre-burning at 700~1100 DEG C in atmosphere of the powder obtained by step a), pre-burning soaking time is 2~7 hours;
C) after the pre-burning product after cooling is ground, calcined in atmosphere at 1200~1400 DEG C, the sintering soak time For 3~7 hours;
D) grind after the calcined product that step c) is obtained is cooled down, calcined 3~7 hours in 1500~1600 DEG C in atmosphere;
E) it will be pulverized after the cooling of calcined product that step d) is obtained and obtain titanate red high-brightness elastic stress and light Material.
3. titanate red high-brightness elastic stress luminescent material as claimed in claim 1, can be widely applied to pressure sensing Device, mechanical stress visualization, artificial skin, smart skins, self-diagnosable system, ultraprecise device fabrication, organism, building and The stress distribution detection of machine, City Building is taken precautions against natural calamities and disaster reduction system, prediction earthquake generation, the damage for detecting aircraft and automobile Evil, research human body diseases.
CN201710309955.9A 2017-04-28 2017-04-28 A kind of titanate red high-brightness elastic stress luminescent material and preparation method thereof Pending CN107474834A (en)

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CN111325718A (en) * 2020-01-23 2020-06-23 深圳大学 Strain modal analysis method and related device
CN113372913A (en) * 2021-06-09 2021-09-10 中国科学院兰州化学物理研究所 Stress luminescent elastomer and preparation method and application thereof
US11203714B2 (en) 2018-07-19 2021-12-21 Qingdao University Luminescent material and preparation method thereof
CN114369367A (en) * 2022-01-20 2022-04-19 中国科学院兰州化学物理研究所 Temperature-stress dual-mode flexible sensing material and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11203714B2 (en) 2018-07-19 2021-12-21 Qingdao University Luminescent material and preparation method thereof
CN109468132A (en) * 2018-10-10 2019-03-15 阜阳师范学院 A kind of rear-earth-doped composite red color stress light emitting material and preparation method thereof
CN111325718A (en) * 2020-01-23 2020-06-23 深圳大学 Strain modal analysis method and related device
WO2021147191A1 (en) * 2020-01-23 2021-07-29 深圳大学 Strain mode analysis method and related device
CN113372913A (en) * 2021-06-09 2021-09-10 中国科学院兰州化学物理研究所 Stress luminescent elastomer and preparation method and application thereof
CN114369367A (en) * 2022-01-20 2022-04-19 中国科学院兰州化学物理研究所 Temperature-stress dual-mode flexible sensing material and preparation method thereof
CN114369367B (en) * 2022-01-20 2022-09-02 中国科学院兰州化学物理研究所 Temperature-stress dual-mode flexible sensing material and preparation method thereof

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