CN102634335A - Piezoelectric elastic-stress luminescent material and production method thereof - Google Patents
Piezoelectric elastic-stress luminescent material and production method thereof Download PDFInfo
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- CN102634335A CN102634335A CN2012100824981A CN201210082498A CN102634335A CN 102634335 A CN102634335 A CN 102634335A CN 2012100824981 A CN2012100824981 A CN 2012100824981A CN 201210082498 A CN201210082498 A CN 201210082498A CN 102634335 A CN102634335 A CN 102634335A
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Abstract
The invention belongs to the technical field of materials physics and relates to piezoelectric elastic-stress luminescent material and a production method thereof. The piezoelectric elastic-stress luminescent material is produced by using CaZnOS:Mn (thioxo-inorganic compound) activated by transitional metal manganous ions as substrate, subsitituting Ca-site and Zn-site metallic ions, and subjecting transitional metal and rear earth sensitizer ions to co-doping. A chemical formula of the luminescent material is (Ca1-xMx)(Zn1-yNy)1-aOS:(Mn1-zRz)a, wherein M stands for Ca-site substitute ions, Mg2+, Sr2+ and Ba2+ are selected, N stands for Zn-site substitute ions, Mg2+ and Al3+ selected, R stands for co-doped transitional metal or rear earth sensitive ions from Cu+, Cu2+, Cr3+, Ag+ and the like, and x, y, z and a stand for molar content and are not zero simultaneously. The production method of the material is simple in process, reliable in principle, low in cost, high in stress luminescence quality, fine in mechanical property, high in processibility, wide in application range and evident in economic value.
Description
Technical field:
The invention belongs to the Material Physics technical field; Relate to a kind of piezoelectric type elastic stress luminescent material and preparation method thereof; Particularly a kind of piezoelectric type elastic stress luminescent material and fabricating technology thereof that multiple stress is had response; This stress light emitting material is a matrix with transition metal divalent manganesetion activated sulphur oxygen base mineral compound CaZnOS:Mn, through Ca position and Zn position metals ion are substituted, adopts transition metal and rare earth sensitizer ion to carry out codoped and prepares.
Background technology:
At present, the real-time detection technology of stress distribution is very extensive in the application in fields such as robot manufacturing, industrial production monitoring, urban architecture security control, aerospace, is domestic and international professional's research focus.The elastic stress luminescent material developed of people has the advantages that luminous intensity is directly proportional with stress intensity in recent years; The more important thing is; Stress irradiance technology based on this elastic stress luminescent material exploitation makes stress test not receive the restriction of object moving state and shape; Overcome the traditional electrical signal and needed the drawback that point-to-point physics contacts between electrode and the object under test in measuring; And improved the spatial resolution of stress distribution, have broad application prospects in the visual inspection field of dynamic object three-dimensional space stress distribution.In order to realize the elastic stress luminescent material in the sense of touch of simulating human skin, the practical application of complicated earth movement equal stress DISTRIBUTED REAL-TIME field of detecting when surveying different stress to machine part effect, perception earthquake, modern technologies have proposed following requirement to the elastic stress luminescent material: the one, requirement elastic stress luminescent material can to different stress stimulations (like compression, stretch, crooked, collide, rub, reverse, ultrasonic etc.) make summary responses; The 2nd, requirement elastic stress luminescent material has stronger luminous intensity (under common stress test condition, naked eyes can be observed significantly luminous); The 3rd, the stress irradiance twilight sunset of requirement elastic stress luminescent material is short, and after stress applied end, luminous halation of no obvious stress and stressed track did not influence strain gauge and continue weak stress signal is made resolution.Yet developed the also SrAl of public use at present
2O
4: Eu
2+(Dy
3+, Nd
3+), ZnS:Mn
2+, Ca
2Al
2SiO
7: Ce
3+, BaTiO
3-CaTiO
3: Pr
3+, SrAl
2O
4: Ce
3+(Ho
3+), CaMgSi
2O
7: Eu
2+(Dy
3+), CaAl
2Si
2O
8: Eu
2+, CaYAl
3O
7: Eu
2+And SrMg
2(PO
4)
2: Eu
2+All can not satisfy above-mentioned requirements simultaneously Deng kind of elastic stress luminescent material surplus ten, particularly in having the elastic stress luminescent material of strong stress irradiance characteristic, ZnS:Mn
2+And BaTiO
3-CaTiO
3: Pr
3+The mechanical stress form that material can respond is single, can't make response to multiple stress; And SrAl
2O
4: Eu
2+Though material can be made response to multiple stress, stress irradiance is long after time, and luminous halation and the triboluminescent movement locus of its compression can be seriously undermined the resolving power of optical signal and stress image by the clear observation of naked eyes in several minutes.
Summary of the invention:
The objective of the invention is to overcome the deficiency that prior art exists, seeking to prepare provides a kind of high brightness to multiple stress response, fast attenuation type piezoelectric type elastic stress luminescent material and preparation method thereof.
To achieve these goals; The piezoelectric type elastic stress luminescent material that the present invention relates to is a matrix with transition metal divalent manganesetion activated sulphur oxygen base mineral compound CaZnOS:Mn; Through Ca position and Zn position metals ion are substituted; Adopt transition metal and rare earth sensitizer ion to carry out codoped and prepare, the chemical expression of this luminescent material is (Ca
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
a, (0≤x≤0.5,0≤y≤0.5,0≤z≤0.5,0≤a≤0.3), wherein, M representes Ca position substitutional ion, is selected from Mg
2+, Sr
2+And Ba
2+In a kind of or more than two kinds; N representes Zn position substitutional ion, is selected from Mg
2+And Al
3+In one or both; R representes the transition metal or the rare earth sensitizer ion of codoped, and the monovalent base metals ion that plays the electric charge coordination, is selected from transition metal ion Cu
+, Cu
2+, Cr
3+, Ag
+And Cd
2+, or rare earth sensitizer ion Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
2+, Eu
3+, Tb
3+, Dy
3+, Ho
3+, Er
3+And Tm
3+, and alkalimetal ion Li
+, Na
+, K
+And Rb
+In a kind of or more than two kinds; X, y, z, a represent molar content, and wherein x, y, z, a are not zero simultaneously.
The preparation method of piezoelectric type elastic stress luminescent material of the present invention may further comprise the steps:
(1) choose raw material, wherein Ca, Sr or Ba its carbonate of employing or oxide compound or sulfide are raw material, and it is raw material that Zn adopts zinc sulphide; It is raw material that Mg, Al, Mn adopt its carbonate or oxide compound; Transition metal Cu, Cr, Ag and Cd, rare earth sensitizing agent Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er and Tm, it is raw material that basic metal Li, Na, K and Rb adopt its oxide compound, nitrate salt or carbonate; By the metering of each element chemistry than taking by weighing starting material, and mix mixed raw material;
(2) adding absolute ethyl alcohol or deionized water grind in the agate alms bowl and stirred 1-4 hour in mixed raw material, in 50-100 ℃ of baking oven, obtain mixed powder after the oven dry;
(3) again mixed powder is placed alumina crucible sample after carrying out getting pre-burning in pre-burning 3-5 hour under the 700-900 ℃ of atmospheric environment;
(4) sample after the taking-up pre-burning grinds the back again in 40-80kgf/cm
2Pressure under carry out packing into behind the compressing tablet in the crucible, in argon atmosphere, be warming up to 1000-1300 ℃ and be incubated 4-8 hour after, naturally cool to room temperature with stove and get sheeted product;
(5) with cooled sheeted product pulverize the back in the 20-50 eye mesh screen sieve the Powdered elastic stress luminescent material product of crystalline-granular texture.
The stress irradiance intensity of the piezoelectric type elastic stress luminescent material that the present invention relates to depends on the grain-size in the material; When grain-size becomes big; Luminous intensity reduces, and when grain-size is little during to nano level, luminous intensity raises; Grain-size is 50-120nm, and grain-size is measured with X-ray diffractometer.
The present invention is mixed and made into stress light emitting material powder that makes and optically transparent organic resin macromolecular material thin slice or cylinder shape resinite or is coated on the UUT surface, can be luminous behind the stress application; The stress that is applied comprises compression, stretching, bending, collides, rubs, reverses with ultrasonic; In elastic limit, stress irradiance intensity is directly proportional with institute stress application intensity, and the brightness naked eyes can be observed; After stress applied end, the stress irradiance decay of afterglow did not have macroscopic stress irradiance halation and stressed track; This stress light emitting material is used for the stress distribution of parts and member is measured and the adhesive strength measurement in real time.
The luminous intensity of the piezoelectric type elastic stress luminescent material that the present invention relates to depends on the mechanical energy size of excitaton source; Rising with mechanical interaction force raises; In causing photoemissive mechanical interaction power, exist minimum can value or threshold value, this threshold value receives the domination of material component variation; The mechanical energy width of its response is lower than 3 milliwatts, and it is wide to adapt to energy region.
The present invention compared with prior art, the preparation process of its material is simple, principle is reliable, cost is low, the stress irradiance quality is good, physicals is good, workability is good, has wide range of applications, economic worth is obvious.
Description of drawings:
Fig. 1 is the pressure and the luminous intensity funtcional relationship synoptic diagram of material of the present invention; The funtcional relationship of luminous intensity and pressure intensity when showing on mechanical pressure (compression speed 3mm/min, peak pressure 1000N) is applied to the elastic stress luminescent material of multiple stress response.
Fig. 2 is the luminous intensity of material of the present invention and concerns synoptic diagram fall time; Show when frictional force (end points diameter 1mm transparent resin rod; Load 5N, speed of rotation 150rpm) luminous intensity and the funtcional relationship of fall time when being applied on the elastic stress luminescent material that multiple stress is responded.
Fig. 3 is the luminous intensity of material of the present invention and concerns synoptic diagram fall time, luminous intensity and the funtcional relationship of fall time when showing on impact force (collision energy is 30mJ) is applied to the elastic stress luminescent material of multiple stress response.
The luminous intensity of Fig. 4 material of the present invention and fall time concern synoptic diagram, luminous intensity and the funtcional relationship of fall time when showing on ultrasonication (ultrasonic energy is 2.94mW) is applied to the elastic stress luminescent material of multiple stress response.
Embodiment:
Below through embodiment and combine accompanying drawing the present invention will be described in more detail.
Embodiment 1-6:
It is raw material that raw material Ba in the present embodiment, Sr, Ca adopt its carbonate; It is raw material that Zn adopts zinc sulphide; It is raw material that Mg, Al, Mn adopt its carbonate or oxide compound, transition metal Cu, Cr, Ag and Cd, rare earth sensitizing agent Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er and Tm; It is raw material that basic metal Li, Na, K and Rb adopt its oxide compound or nitrate salt, according to its molecular formula (Ca
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
a, wherein, 0≤x≤0.5,0≤y≤0.5,0≤z≤0.5,0≤a≤0.3; M representes Ca position substitutional ion, is selected from Mg
2+, Sr
2+, Ba
2+A kind of in the divalent ion or more than two kinds; N representes Zn position substitutional ion, is selected from Mg
2+, Al
3+In the ion one or both; R representes the transition metal or the rare earth sensitizer ion of codoped, and the monovalent base metals ion that plays the electric charge coordination, is selected from transition metal ion Cu
+, Cu
2+, Cr
3+, Ag
+And Cd
2+, or rare earth sensitizer ion Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
2+, Eu
3+, Tb
3+, Dy
3+, Ho
3+, Er
3+And Tm
3+, and alkalimetal ion Li
+, Na
+, K
+, Rb
+In a kind of or more than two kinds; X, y, z, a represent molar content, and x, y, z, a are not zero simultaneously, mix after selecting and take by weighing each raw material, and its select materials ratio and quantity are referring to shown in the table 1.
Table 1 prepares luminescent material (Ca for embodiment 1-6
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
aProportioning and raw material weight
Again the compound of the prescription in the table 1 is put into agate mortar, add an amount of absolute ethyl alcohol and ground 1.5 hours, after 50 ℃ of oven for drying, obtain mixed powder; Place alumina crucible then, pre-burning is 4 hours under 800-900 ℃ atmospheric environment; After powder after the pre-burning remake grinding, in 50kgf/cm
2The pressure lower sheeting, in the crucible of packing into, in argon atmosphere, be warming up to 1100-1200 ℃; Be incubated 5 hours; Naturally cool to room temperature with stove afterwards, being sieved in 25 eye mesh screens in its pulverizing back obtains powdery product, multiple stress is had the elastic stress luminescent material (Ca of response
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
aPowdery product that makes and optically transparent resene macromolecular material (like ABS resin, polyacetal (PA), polycarbonate (PC), Vilaterm (PE), PS (PS), Vestolen PP 7052 (PP), polymethylmethacrylate (PMMA), urethane resin, polyester, epoxy resin, Zylox etc.) are mixed and made into thin slice or cylinder shape resinite or are coated on the UUT surface, can test its luminescence response performance different stresses.
Prepared (the Ca of present embodiment 1-6
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
aMaterial has the piezoelectric type elastic stress luminescent material to multiple stress response characteristic, and the chemical dosage ratio of each component of prescription of embodiment 1-6 is as shown in table 1; Fig. 1 has provided (Ca
0.9Ba
0.1) Zn
0.99OS:Mn
0.01Stress irradiance intensity and the relation curve of stress intensity of (embodiment 2) material under mechanical pressure (compression speed 3mm/min, peak pressure 1000N) effect, stress irradiance intensity strengthens with the increase of stress application, and is linear.This shows the information that can obtain stress intensity through the measurement of stress irradiance intensity; Fig. 2 has provided (Ca
0.9Ba
0.1) Zn
0.99OS:Mn
0.01Luminous intensity and the relation curve of fall time of (embodiment 2) material under frictional force (end points diameter 1mm transparent resin rod, load 5N, speed of rotation 150rpm) effect; Fig. 3 has provided (Ca
0.9Ba
0.1) Zn
0.99OS:Mn
0.01Luminescent material and the funtcional relationship of fall time of (embodiment 2) material under impact force (collision energy is 30mJ) effect; Fig. 4 has provided (Ca
0.9Ba
0.1) Zn
0.99OS:Mn
0.01Luminous intensity and the funtcional relationship of fall time of (embodiment 2) material under ultrasonication (ultrasonic energy is 2.94mW), this ultrasonic energy is that medical ultrasound image is used, and is harmless; Equally; The stress intensity and the Energy value relation in direct ratio of the stress irradiance intensity of this material under frictional force, impact force and ultrasonication and the frictional force, impact force and the ultrasonication that apply; The stress irradiance that shows this material is that elastic stress is luminous, can be through measuring the value and the energy of the different mechanical interaction power that luminous intensity obtains to be applied.To some large-scale components, parts, irregular element, the stress distribution of parts under different mechanical stress effects adopt other method can't obtain the information of stress distribution, adopt the material of present embodiment to test, and can be resolved.
Claims (5)
1. piezoelectric type elastic stress luminescent material; It is characterized in that with transition metal divalent manganesetion activated sulphur oxygen base mineral compound CaZnOS:Mn be matrix; Through Ca position and Zn position metals ion are substituted; Adopt transition metal and rare earth sensitizer ion to carry out codoped and prepare, the chemical expression of this luminescent material is (Ca
1-xM
x) (Zn
1-yN
y)
1-aOS: (Mn
1-zR
z)
a, (0≤x≤0.5,0≤y≤0.5,0≤z≤0.5,0≤a≤0.3), wherein, M representes Ca position substitutional ion, is selected from Mg
2+, Sr
2+And Ba
2+In a kind of or more than two kinds; N representes Zn position substitutional ion, is selected from Mg
2+And Al
3+In one or both; R representes the transition metal or the rare earth sensitizer ion of codoped, and the monovalent base metals ion that plays the electric charge coordination, is selected from transition metal ion Cu
+, Cu
2+, Cr
3+, Ag
+And Cd
2+, or rare earth sensitizer ion Ce
3+, Pr
3+, Nd
3+, Sm
3+, Eu
2+, Eu
3+, Tb
3+, Dy
3+, Ho
3+, Er
3+And Tm
3+, and alkalimetal ion Li
+, Na
+, K
+And Rb
+In a kind of or more than two kinds; X, y, z, a represent molar content, are not zero simultaneously.
2. piezoelectric type elastic stress luminescent material according to claim 1; The stress irradiance intensity that it is characterized in that piezoelectric type elastic stress luminescent material depends on the grain-size in the material, and when grain-size became big, luminous intensity reduced; When grain-size little when the nano level; Luminous intensity raises, and grain-size is 50-120nm, and grain-size is measured with X-ray diffractometer.
3. piezoelectric type elastic stress luminescent material according to claim 1; It is characterized in that stress light emitting material powder that makes and optically transparent organic resin macromolecular material are mixed and made into thin slice or cylinder shape resinite or are coated on the UUT surface, can be luminous behind the stress application; The stress that is applied comprises compression, stretching, bending, collides, rubs, reverses with ultrasonic; In elastic limit, stress irradiance intensity is directly proportional with institute stress application intensity, and the brightness naked eyes can be observed; After stress applied end, the stress irradiance decay of afterglow did not have macroscopic stress irradiance halation and stressed track; This stress light emitting material is used for the stress distribution of parts and member is measured and the adhesive strength measurement in real time.
4. piezoelectric type elastic stress luminescent material according to claim 1; The luminous intensity of the piezoelectric type elastic stress luminescent material that it is characterized in that relating to depends on the mechanical energy size of excitaton source; Rising with mechanical interaction force raises; In causing photoemissive mechanical interaction power, exist minimum can value or threshold value, this threshold value receives the domination of material component variation; The mechanical energy width of its response is lower than 3 milliwatts, and it is wide to adapt to energy region.
5. the preparation method of a piezoelectric type elastic stress luminescent material is characterized in that may further comprise the steps:
(1) choose raw material, wherein Ca, Sr or Ba its carbonate of employing or oxide compound or sulfide are raw material, and it is raw material that Zn adopts zinc sulphide; It is raw material that Mg, Al, Mn adopt its carbonate or oxide compound; Transition metal Cu, Cr, Ag and Cd, rare earth sensitizing agent Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er and Tm, it is raw material that basic metal Li, Na, K and Rb adopt its oxide compound, nitrate salt or carbonate; By the metering of each element chemistry than taking by weighing starting material, and mix mixed raw material;
(2) adding absolute ethyl alcohol or deionized water grind in the agate alms bowl and stirred 1-4 hour in mixed raw material, in 50-100 ℃ of baking oven, obtain mixed powder after the oven dry;
(3) again mixed powder is placed alumina crucible sample after carrying out getting pre-burning in pre-burning 3-5 hour under the 700-900 ℃ of atmospheric environment;
(4) sample after the taking-up pre-burning grinds the back again in 40-80kgf/cm
2Pressure under carry out packing into behind the compressing tablet in the crucible, in argon atmosphere, be warming up to 1000-1300 ℃ and be incubated 4-8 hour after, naturally cool to room temperature with stove and get sheeted product;
(5) with cooled sheeted product pulverize the back in the 20-50 eye mesh screen sieve the Powdered elastic stress luminescent material product of crystalline-granular texture.
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| CN102936498A (en) * | 2012-11-11 | 2013-02-20 | 青岛大学 | Zirconium phosphate-based elastic stress luminescent material and preparation method thereof |
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| CN116254106A (en) * | 2023-03-17 | 2023-06-13 | 中国科学院兰州化学物理研究所 | ZnS-based stress luminescent material and preparation method thereof, and polymer stress luminescent composite material and preparation method thereof |
| CN116254106B (en) * | 2023-03-17 | 2024-04-12 | 中国科学院兰州化学物理研究所 | ZnS-based stress luminescent material and preparation method thereof, and polymer stress luminescent composite material and preparation method thereof |
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