CN105349141B - A kind of niobate luminescent material of flexible stress irradiance performance and preparation method thereof - Google Patents
A kind of niobate luminescent material of flexible stress irradiance performance and preparation method thereof Download PDFInfo
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- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 6
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- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 3
- 239000012190 activator Substances 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 12
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000005976 Citrus sinensis Nutrition 0.000 description 1
- 240000002319 Citrus sinensis Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
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- 229910052758 niobium Inorganic materials 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a kind of niobate luminescent material of flexible stress irradiance performance and preparation method thereof, the material is with CaNb2O6For matrix, with rare earth ion Pr3+For activator, its chemical expression is [(Ca1‑xMx)1‑z]Nb2O6：(Pr1‑yRy)z(0≤x≤0.2,0≤y≤0.5,0 ＜ z≤0.1), wherein M represent Ca positions substitute element, the one or more in Mg, Sr, Ba；R represents the rare earth or transition metal of codope, the one or more in La, Nd, Sm, Eu, Gd, Yb, Lu, Cr, Mn, Ag, Cd；X, y, z represents molar content.Material is synthesized in atmosphere using high temperature solid-state method.The advantage of the invention is that：(1) material preparation method is simple, easy to operate, equipment requirement is low；(2) there is the material prepared strong elastic stress to light, and the luminous naked eyes of elastic stress are high-visible under dark place, and have preferable heat resistance and water resistance, and machinability is good, has a wide range of application；(3) matrix material of material be it is tellurian be rich in element, belong to environmentally friendly material.
Description
Technical field
The invention belongs to stress irradiance functional material science and technology field, is related to a kind of flexible stress irradiance performance
Niobate luminescent material and preparation method thereof.
Background technology
Stress irradiance (mechanoluminescence) refers to object by various stress, such as expansion, stretching,
Emitted beam under fracture, the friction even effect such as sound vibrations, i.e., mechanical energy is converted into luminous energy.Stress hair is produced according to material
The deformation degree of light time, stress light emitting material can be divided into destructive stress and light and non-destructive stress irradiance, and non-demolition
Property stress irradiance can be divided into that elastic stress is luminous and plastic stress lights again.Although the research to elastic stress luminescent material is only
There is the history of more than ten years, but due to characteristic possessed by elastic stress luminescent material, such as in elastic deformation limit, it is sent out
Light light intensity and deformation degree are directly proportional, and detection object is not damaged, and can be made according to this feature of material
Into sensor, for the stress distribution situation of each position of monitoring component, stress distribution visualization real-time monitoring is realized；When suffered
When stress intensity is increased to beyond elastic properties of materials deformation range arrival plasticity and destructive deformation region, elastic stress luminescent material
The characteristics of having taken into account plastic stress luminescent material and destructive stress luminescent material simultaneously again, this is beneficial to detect various differences
Elastic deformation, plastic deformation and the destructive distortion of structure, the real-time monitoring available for object under test stress and damage situations.
The stressing conditions of conventional telecommunications number measurement object, it is necessary to point-to-point physical contact between electrode and object under test,
And limited by object moving state and shape, it can not be tested in many cases, such as engine in working etc..And
When measuring the stressing conditions of object using elastic stress luminescent material, these shortcomings can be overcome, and remote monitoring can be realized,
The spatial resolution of stress distribution is improved, is had in terms of the visualization measurement of dynamic object three dimensions stress distribution wide
Application prospect.In recent years, with the synthesis of elastic stress luminescent material and the raising of development technique, CCD camera and optical fiber skill
Art develops rapidly, using camera technique, large area deformation is visual in the detection process of elastic stress luminescence sensor
Change, it is easy-to-look-up to arrive hidden danger position, to be repaired in time, play the effect to prevent trouble before it happens.The luminous sensing of elastic stress
Device can react the stress deformation of object in real time, carry out detection object dynamic process so as to develop new stress irradiance sensor
Degree of fatigue.But be a kind of new luminescence phenomenon because elastic stress is luminous, that studies at present is less, it is known that elasticity
Stress light emitting material has the ZnS of Yellow light-emitting low temperature：Mn2+, (Ba, Ca) TiO for glowing3：Pr3+, the SrAl of green light2O4：Eu2+, hair
The Sr of blood orange coloured light3Sn2O7：Sm3+, the BaS for green light of turning blue2O2N2：Eu2+Deng, but comparatively, the elasticity developed should
Power luminescent material species is less, the wavelength of light limitednumber sent, and luminous intensity is extremely difficult to the requirement of practical application,
So this area is badly in need of developing the high elastic stress luminescent material of novel elastic stress light emitting material, particularly luminous intensity.
The content of the invention
It is an object of the invention to disclose niobate luminescent material and its preparation of a kind of flexible stress irradiance performance
Method.The material is with calcium niobate CaNb2O6For matrix, with rare earth ion Pr3+For activator, its chemical expression is [(Ca1- xMx)1-z]Nb2O6：(Pr1-yRy)z(0≤x≤0.2,0≤y≤0.5,0 ＜ z≤0.1), wherein M represent Ca positions substitute element, choosing
From the one or more in Mg, Sr, Ba；R represent codope rare earth or transition metal, selected from La, Nd, Sm, Eu, Gd,
One or more in Yb, Lu, Cr, Mn, Ag, Cd；X, y, z represents molar content.
The niobate luminescent material of flexible stress irradiance performance disclosed in this invention is using high temperature solid-state method 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 800~1000 DEG C in atmosphere of the powder obtained by step a), pre-burning soaking time is 3~6 small
When；
C) after the pre-burning product after cooling is ground, calcined in atmosphere at 1200~1500 DEG C, sintering soak
Time is 3~8 hours；
D) pulverized after the calcined product that step c) is obtained is cooled down and obtain the niobium of flexible stress irradiance performance
Salt luminescent material.
Prepare the niobate luminescent material method of flexible stress irradiance performance, it is characterised in that Ca, Mg, Sr and Ba
Its oxide or carbonate are used as raw material, Nb uses its oxide as raw material, rare earth and the transition metal member of Pr and codope
Element uses its oxide, nitrate or carbonate as raw material.
By the niobate luminescent material powder of obtained flexible stress irradiance performance and optically transparent organic high score
Elastic 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.) be mixed thin slice or
Cylindrical type resinite or coated on the parts to be tested surface, mechanical stress suffered by the part can be converted to luminous energy, realize stress
Distribution detection.
The niobate luminescent material of flexible stress irradiance performance obtained by the present invention, it is characterised in that the material
Elastic stress glow peak be wire peak near 610nm, monochromaticjty is good.
The niobate luminescent material of flexible stress irradiance performance obtained by the present invention, it is characterised in that material has
There is strong elastic stress luminous intensity, can with the naked eye be observed under dark surrounds.
The niobate luminescent material of flexible stress irradiance performance obtained by the present invention, it is characterised in that in elasticity
In limit, the elastic stress luminous intensity of material is directly proportional to load intensity.
The niobate luminescent material of flexible stress irradiance performance obtained by the present invention, it is characterised in that material category
In trap control type luminescent material, its elastic stress luminous intensity can be recovered after ultraviolet light irradiation, belong to non-destructive stress
Luminescent 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) niobate luminescent material of the flexible stress irradiance performance prepared by the present invention should with stronger elasticity
Power luminous intensity, directly it can be seen compared with dark situation by human eye.
(4) luminous intensity of the niobate luminescent material of flexible stress irradiance performance of the present invention, is depended on
The mechanical energy size of excitaton source.The luminous intensity of the material typically increases with the rise of mechanicals efforts, thus is causing
Being worth for minimum in photoemissive mechanical interaction power be present, or stress threshold, the threshold value are dominated by material component change.
The width for the mechanical stress scope that the material can respond, material structure can be destroyed from the weak stress of several newton to applying to be increased to
Energy can make it produce stress irradiance.The niobate luminescent material of flexible stress irradiance performance of the present invention and its
If composite can light from the outside external force for applying very little, and in elastic deformation area, luminous intensity and stress
Intensity is proportional, and stress distribution detection can be achieved.
(5) the luminous twilight sunset of the elastic stress of the niobate luminescent material of flexible stress irradiance performance of the present invention
Decay is fast.After stress application terminates, stress irradiance twilight sunset rapidly disappears (millisecond magnitude), the stress irradiance halation being visible by naked eyes
And stress track, measure of the performance without prejudice to material to follow-up weak stress.The elastic stress luminescent material can be used for part
Measured in real time with the stress distribution of component in being measured with adhesive strength.
(6) niobate luminescent material of flexible stress irradiance performance of the present invention, can be widely applied to pressure
Sensor, mechanical stress visualization, artificial skin, smart skins, self-diagnosable system, ultraprecise device fabrication, organism, building
The detection of the stress distribution of thing and machine, City Building is taken precautions against natural calamities and disaster reduction system, prediction earthquake produce, detect aircraft and automobile
Infringement, research human body diseases etc..
Brief description of the drawings
Fig. 1 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001X-ray diffractogram of powder.
Fig. 2 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Excitation spectrum (monitoring 605nm red emissions).
Fig. 3 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Emission spectrum (excitation wavelength 280nm).
Fig. 4 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Elastic stress luminescent spectrum.
Fig. 5 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Elastic stress under pressure load effect lights
Photo.
Fig. 6 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Between suffered load and elastic stress luminous intensity
Relation curve.
Fig. 7 is the products C a of the embodiment of the present invention 10.999Nb2O6：Pr0.001Thermo-luminescence.
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
One or more method and steps that invention is mentioned do not repel also has other method and steps before and after the combination step, or
Other method and steps can also be inserted before the step of these are specifically mentioned；It should also be understood that these embodiments are merely to illustrate this
Invention rather than limitation the scope of the present invention.Moreover, unless otherwise indicated, the numbering of various method steps is only to differentiate each method
The convenient tool of step, rather than ordering or the enforceable scope of the restriction present invention for limitation various method steps, its is relative
Relation is altered or modified, in the case where changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Specifically, table 1 list the material component of 12 specific embodiments of the present invention, raw material weight, calcining heat and
Elastic stress luminescent properties.
Material component, raw material weight, sintering temperature and the elastic stress luminescent properties of the embodiment 1-12 samples of table 1.
Embodiment 1
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.999Nb2O6：Pr0.001：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 800 DEG C；
(3) preburning powdered material after grinding is calcined 4 hours at 1300 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.999Nb2O6：Pr0.001Elastic stress hair
Luminescent material.
(5) by the niobate luminescent material powder of obtained flexible stress irradiance performance with it is optically transparent organic high
Molecular elastic material polyurethane resin is mixed with mass ratio 1: 10, be made diameter and thickness be 1cm cylindrical type resinite, use
In the elastic stress luminescent properties of measurement sample.
The niobates elastic stress luminescent material white in appearance that the embodiment is prepared, X-ray powder diffraction (XRD) are surveyed
Test result is as shown in figure 1, the diffraction peak data and CaNb of products obtained therefrom2O6Powder diffraction standard card (00-039-1392's) spreads out
It is consistent to penetrate data, and without dephasign, illustrates the CaNb that gained luminescent material is pure phase2O6Structure.Monitor swashing for 605nm red emissions
As shown in Fig. 2 the excitation spectrum of the material is made up of in the range of 250~550nm a series of peaks, highest peak is located at luminous spectrum
280nm, other peaks are located at 457nm, 476nm and 493nm.Fig. 3 be the material in the case where 280nm light excites in 590-670nm models
Interior emission spectrum is enclosed, the emission spectrum mainly nearby comes from Pr by 610nm3+Wire peak composition.Fig. 4 is the elasticity of the material
Stress irradiance spectrum, the emission spectrum positioned at 610nm by nearby coming from Pr3+Wire peak composition.Fig. 5 is that the material is born in pressure
Elastic stress luminous photo under lotus effect.As can be seen that elastic stress under pressure light it is high-visible, in pressure
The elastic stress of load most strength is luminous the most obvious.Fig. 6 is the elastic stress luminous intensity of the material with the change of pressure load
Change curve.The luminous intensity of elastic stress strengthens with the increase for applying pressure load, in 0-1000N pressure limit, material
Material elastic stress luminous intensity shows accurate linear functional relation with the increase of the intensity of pressure.In the release of pressure load
Cheng Zhong, the luminous rapid decay of material.Fig. 7 is that the thermoluminescence of material is composed, and is released in the range of 25-225 DEG C in the presence of a strong heat
Photopeak, show that material belongs to trap control type luminescent material, its elastic stress luminous intensity can be recovered after ultraviolet light irradiation, category
In non-destructive stress light emitting material.
Embodiment 2
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.998Nb2O6：Pr0.002：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 5 hours at 900 DEG C；
(3) preburning powdered material after grinding is calcined 5 hours at 1200 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.998Nb2O6：Pr0.002Elastic stress hair
Luminescent material.
Embodiment 3
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.997Nb2O6：Pr0.003：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 5 hours at 900 DEG C；
(3) preburning powdered material after grinding is calcined 6 hours at 1350 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.997Nb2O6：Pr0.003Elastic stress hair
Luminescent material.
Embodiment 4
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.996Nb2O6：Pr0.004：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 5 hours at 800 DEG C；
(3) preburning powdered material after grinding is calcined 6 hours at 1400 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.996Nb2O6：Pr0.004Elastic stress hair
Luminescent material.
Embodiment 5
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.995Nb2O6：Pr0.005：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 800 DEG C；
(3) preburning powdered material after grinding is calcined 4 hours at 1450 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.995Nb2O6：Pr0.005Elastic stress hair
Luminescent material.
Embodiment 6
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.994Nb2O6：Pr0.006：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 900 DEG C；
(3) preburning powdered material after grinding is calcined 5 hours at 1400 DEG C in air atmosphere；
(4) it is Ca the product after cooling to be pulverized and obtain chemical composition0.994Nb2O6：Pr0.006Elastic stress hair
Luminescent material.
Embodiment 7
Prepare the niobate luminescent material (Ca of flexible stress irradiance performance0.95Ba0.05)0.996Nb2O6：Pr0.004：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 3 hours at 850 DEG C；
(3) preburning powdered material after grinding is calcined 3 hours at 1350 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.95Ba0.05)0.996Nb2O6：Pr0.004's
Elastic stress luminescent material.
Embodiment 8
Prepare the niobate luminescent material (Ca of flexible stress irradiance performance0.99Mg0.01)0.995Nb2O6：Pr0.005：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 850 DEG C；
(3) preburning powdered material after grinding is calcined 4 hours at 1400 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.99Mg0.01)0.995Nb2O6：Pr0.005's
Elastic stress luminescent material.
Embodiment 9
Prepare the niobate luminescent material (Ca of flexible stress irradiance performance0.97Sr0.02Ba0.01)0.99Nb2O6：Pr0.01：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 5 hours at 950 DEG C；
(3) preburning powdered material after grinding is calcined 4 hours at 1450 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.97Sr0.02Ba0.01)0.99Nb2O6：
Pr0.01Elastic stress luminescent material.
Embodiment 10
Prepare the niobate luminescent material Ca of flexible stress irradiance performance0.997Nb2O6：(Pr0.7Eu0.3)0.003：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 3 hours at 1000 DEG C；
(3) preburning powdered material after grinding is calcined 3 hours at 1500 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.997Nb2O6：(Pr0.7Eu0.3)0.003's
Elastic stress luminescent material.
Embodiment 11
Prepare the niobate luminescent material (Ca of flexible stress irradiance performance0.97Sr0.03)0.99Nb2O6：
(Pr0.8Mn0.2)0.01：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 900 DEG C；
(3) preburning powdered material after grinding is calcined 4 hours at 1400 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.97Sr0.03)0.99Nb2O6：
(Pr0.8Mn0.2)0.01Elastic stress luminescent material.
Embodiment 12
Prepare the niobate luminescent material (Ca of flexible stress irradiance performance0.94Sr0.03Ba0.03)0.993Nb2O6：
(Pr0.5Gd0.5)0.007：
(1) raw material is weighed according to table 1, above raw material is that analysis is pure, after being sufficiently mixed raw material, is dried in 60 DEG C of baking ovens；
(2) mixed powder after drying is placed into alumina crucible in air atmosphere pre-burning 4 hours at 1000 DEG C；
(3) preburning powdered material after grinding is calcined 5 hours at 1500 DEG C in air atmosphere；
(4) it is (Ca the product after cooling to be pulverized and obtain chemical composition0.94Sr0.03Ba0.03)0.993Nb2O6：
(Pr0.5Gd0.5)0.007Elastic stress luminescent material.
By the niobate luminescent material powder of the flexible stress irradiance performance obtained by embodiment 2-12 respectively with light
Learn transparent organic elastomeric polymer materials A BS resins, polyacetals (PA), makrolon (PC), polyethylene (PE), polystyrene
(PS), polypropylene (PP), polymethyl methacrylate (PMMA), polyurethane resin, polyester, epoxy resin, silicon rubber are with 1: 10-
5: 10 mass ratio is mixed and made into thin slice, cylindrical type resinite, coated on the parts to be tested surface, and the elasticity for measuring sample should
Power luminescent properties.
The niobates elastic stress luminescent material white in appearance that above-described embodiment 2-12 is prepared, X-ray powder diffraction
(XRD) test result is identical with the sample of embodiment 1, the diffraction peak data and CaNb of products obtained therefrom2O6Powder diffraction standard card
The diffraction data of (00-039-1392) is consistent, and without dephasign, illustrates the CaNb that gained luminescent material is pure phase2O6Structure.Implement
The excitation spectrum and emission spectrum of example 2-12 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 2-12 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.The elastic stress luminous intensity of each sample under dark surrounds can naked-eye observation, and in pressure load most strength
Elastic stress is luminous the most obvious.The elastic stress luminous intensity of each sample strengthens with the increase for applying pressure load, in 0-
In 1000N pressure limit, elastic properties of materials stress irradiance intensity shows accurate linear function with the increase of the intensity of pressure and closed
System.During the release of pressure load, the luminous rapid decay of material.Each sample all has strong in the range of 25-225 DEG C
Thermal glow peak, show that material belongs to trap control type luminescent material, its elastic stress luminous intensity can be extensive after ultraviolet light irradiation
It is multiple, 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 (4)
1. a kind of niobate luminescent material of flexible stress irradiance performance, it is characterised in that with CaNb2O6Material is matrix,
With trivalent rare earth ionses Pr3+For activator, its chemical expression is [(Ca1-xMx)1-z]Nb2O6：(Pr1-yRy)z, wherein 0≤x≤
0.2,0≤y≤0.5,0.005 ＜ z≤0.1；One or more of the M in Mg, Sr, Ba, R in Eu, Gd, Mn one
Kind, x, y, z represents molar content；The elastic stress glow peak of the material is wire peak near 610nm, monochromaticjty
It is good；Material has strong elastic stress luminous intensity, and red stress irradiance can use naked-eye observation under dark surrounds；Limited in elasticity
In degree, the elastic stress luminous intensity of material is directly proportional to load intensity；The elastic stress of material lights after ultraviolet light irradiation
It can recover, belong to trap control type non-demolition stress light emitting material.
2. the preparation method of the niobate luminescent material of flexible stress irradiance performance as claimed in claim 1, its feature
It is, Ca, Mg, Sr and Ba use its oxide or carbonate as raw material, and Nb uses its oxide as raw material, and Pr and R use it
Oxide, nitrate or carbonate are raw material, are prepared using high temperature process heat method, 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 800~1000 DEG C in atmosphere of the powder obtained by step a), pre-burning soaking time is 3~6 hours；
C) after the pre-burning product after cooling is ground, calcined in atmosphere at 1200~1500 DEG C, the sintering soak time
For 3~8 hours；
D) pulverized after the calcined product that step c) is obtained is cooled down and obtain the niobates of flexible stress irradiance performance
Luminescent material.
3. the niobate luminescent material of flexible stress irradiance performance as claimed in claim 1, it is characterised in that will be made
Elastic stress luminescent material powder mixed with optically transparent organic elastomeric polymer material after, laminate or cylindrical type tree
Fat body 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 detects.
4. the niobate luminescent material of flexible stress irradiance performance as claimed in claim 1, can be widely applied to pressure
Sensor, mechanical stress visualization, artificial skin, smart skins, self-diagnosable system, ultraprecise device fabrication, organism, building
The detection of the stress distribution of thing and machine, City Building is taken precautions against natural calamities and disaster reduction system, prediction earthquake produce, detect aircraft and automobile
Infringement, research human body diseases.
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