CN101343180A - Complex-phase ceramic material with stress irradiance and electroluminescence characters and preparation thereof - Google Patents

Complex-phase ceramic material with stress irradiance and electroluminescence characters and preparation thereof Download PDF

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CN101343180A
CN101343180A CNA2008100421880A CN200810042188A CN101343180A CN 101343180 A CN101343180 A CN 101343180A CN A2008100421880 A CNA2008100421880 A CN A2008100421880A CN 200810042188 A CN200810042188 A CN 200810042188A CN 101343180 A CN101343180 A CN 101343180A
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stress
content
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ceramic material
stress irradiance
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CN101343180B (en
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王旭升
张君诚
杨伟
李艳霞
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Tongji University
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Abstract

The invention discloses a self-assembly bi-phase composite ceramic powder, which is characterized in that the powder has a molecular formula of Ba(1-x1-x2-x3-ySrx1Cax2Ax3Ry)Ti(1-zMz)O3, wherein, 0<=x1<=0.18, 0.21<=x2<=0.90, 0.0001<=x3<=0.13, 0.0001<=y<=0.05, 0<=z<=0.20; A is a bivalent element of Mg, Pb, Zn, Cu or Cr, R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is a quadrivalent element of Zr, Ce, Cu or Sn. The composite ceramic includes two phases, the content of barium in the first phase is larger than the calcium content, and the calcium content in the second phase is larger than the barium content. The ceramic powder has the features of stress luminescence and electroluminescence, and can be used for the stress distribution measurement and adhesive strength measurement of various parts and members and in plane illumination devices. The parts can be luminous when being coated with ceramic powder on surfaces and applied with stress. The luminous intensity of stress luminescence is in direct ratio with the applied stress in the elastic limit.

Description

A kind of diphase ceramic material and preparation method thereof with stress irradiance and electroluminescence characters
Technical field
The present invention relates to diphase ceramic material that has stress irradiance and electroluminescence characters and preparation method thereof.
Background technology
Some materials can be luminous under outer field action, and as UV-light and excited by visible light (photoluminescence), electron beam, X-ray excite, and electric field excites (electroluminescent) etc., and this phenomenon is widely known by the people and is widely used.In recent years, a kind of novel effect one stress irradiance effect, new stress light emitting material and the exploitation of advanced testing method cause people's attention.Stress irradiance is the phenomenon that a kind of mechanical energy is converted to luminous energy, promptly applies mechanical stress to material and makes it luminous.Can be divided into luminous and nondestructive (elasticity) stress irradiance of destructive stress.The destructive stress luminescence phenomenon promptly be it is found that as far back as 16th century at the occurring in nature ubiquity, discharges cause luminous as huge energy such as earthquake, rock cracks.Substantial progress is not arranged so far.Elastic stress is luminous to be to apply mechanical stress to it to make it luminous in elastic properties of materials deformation limit, has the advantages that luminous intensity is directly proportional with applied stress.Because the height regularity of its nondestructive and luminous intensity and stress makes people detect stress distribution by the intensity distribution that detects stress irradiance, realizes that nondestructive stress detects and stress is visual.It can be used in artificial skin, smart skins, the self-diagnosable system, takes precautions against natural calamities at stress distribution detection, monitoring, the City Building of buildings and machine part, all has wide practical use in the disaster reduction system.
The luminous research history of elastic stress has only the more than ten years, and India and Japan start to walk early, and Japan's research and application in this respect is active, mainly contains Japanese state-run industrial technology synthetic study institute (AIST) and Sony company, has succeeded in developing SrAl 2O 4: Eu and (Ba, Ca) TiO 3: Pr equal stress luminescent material and corresponding patented technology.In recent years, the research of this respect enlivened in the world, and countries such as Korea S, the U.S. have also begun research.At present, the subject matter that stress light emitting material research exists has: (1) stress irradiance mechanism it be unclear that, though it is believed that stress irradiance is relevant with piezoelectric effect, also only is to find out from material properties, be confined to phenomenon talking stage, go back the theoretical model that none is generally acknowledged; (2) kind of existing high performance stress luminescent material very little, institute's luminous spectrum is limited, as SrAl 2O 4: Eu green light, (Ba, Ca) TiO 3: Pr glows, and has hindered the application in wider field; In addition, the latter's luminous intensity is also strong inadequately; (3) appraisement system of stress irradiance performance is not set up as yet, does not also have standard international or that certain is national.
Summary of the invention
The objective of the invention is provides a kind of diphase ceramic material with stress irradiance and electroluminescence characters in order to solve deficiency of the prior art.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of diphase ceramic material with stress irradiance and electroluminescence characters is characterized in that, its molecular formula is Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Wherein, 0≤x1≤0.18,0.21≤x2≤0.90,0.0001≤x3≤0.13,0.0001≤y≤0.05,0≤z≤0.20; A is dyad Mg, Pb, Zn, Cu or Cr, and R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is quadrivalent element Zr, Ce, Cu or Sn.
Wherein, the diphase ceramic material with stress irradiance and electroluminescence characters comprises two-phase, first mutually in the content of barium greater than the content of calcium, second mutually in the content of calcium greater than the content of barium.
Wherein, first mutually in, 0≤x1≤0.15,0.21≤x2≤0.50; Second mutually in, 0≤x1≤0.15,0.21≤x2≤0.50.
Another object of the present invention provides the method that a kind of preparation has the diphase ceramic material of stress irradiance and electroluminescence characters, it is characterized in that, comprise step: a, Ba, Sr, Ca adopt its carbonate raw material or part to adopt the titanate raw material, Mg, Pb, Zn, Cu, Cr adopt its carbonate or oxide compound, Ti adopts titanate or its oxide compound, rare earth element R adopts its oxide compound or nitrate raw material, and quadrivalent element M adopts its oxide raw material, according to its molecular formula Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Wherein, 0≤x1≤0.18,0.21≤x2≤0.90,0.0001≤x3≤0.13,0.0001≤y≤0.05,0≤z≤0.20; A is dyad Mg, Pb, Zn, Cu or Cr, and R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is quadrivalent element Zr, Ce, Cu or Sn, selects to mix behind the raw material; Add dehydrated alcohol or deionized water and in mortar, grind, obtain powder after the discharging oven dry;
B, place crucible to carry out pre-burning powder, calcined temperature 900-1100 ℃, be incubated 1-7 hour;
C, preburning powdered material is ground,, can obtain having the multiple phase ceramic material of stress irradiance and electroluminescence characters 1100 ℃～1500 ℃ insulations 2～4 hours.
Preferably, the diphase ceramic material with stress irradiance and electroluminescence characters comprises two-phase, first mutually in the content of barium greater than the content of calcium, second mutually in the content of calcium greater than the content of barium.
More preferably be, first mutually in, 0≤x1≤0.15,0.21≤x2≤0.50; Second mutually in, 0≤x1≤0.15,0.21≤x2≤0.50.
Beneficial effect of the present invention is:
(1) material preparation technology of the present invention is simple, and cost is low, the content of raw material Pb seldom or even do not have, preparation process and the complex phase ceramic made pollute and toxic side effect less; This complex phase ceramic is a kind of natural two-phase composite material, has the self-assembly characteristic;
(2) this complex phase ceramic powder has good stress irradiance characteristic, and (500-100N) can observe with the naked eye bright luminous under general stress condition.This powder can be coated on various parts, component surface, imposes stress and can test wherein stress distribution; Sneak in the caking agent, can also test, compare the stress distribution and the bonding strength of caking agent.
(3) this complex phase ceramic powder has good electroluminescence characters, and (20-30kV/cm) can observe with the naked eye bright luminous under common strength of electric field.This powder can be used for preparing electroluminescent cell, is applied to design, the preparation of flat-panel screens.
(4) this complex phase ceramic powder also has the excellent dielectric characteristic, as has characteristics such as dielectric tunable characteristic under the external electric field, ferroelectric, piezoelectricity, is a kind of multifunctional material.
Description of drawings:
Fig. 1, Ba 0.998-x1-x2Sr X1Ca X2Pr 0.002TiO 3The X-ray diffraction analysis collection of illustrative plates of ceramic powder.
Fig. 2, Ba 0.1Ca 0.898Pr 0.002Ti 1-zZr zO 3The photoluminescence curve of ceramic powder.
Fig. 3, Ba 1-x2Ca X2Pr 0.002Ti 0.95Zr 0.05O 3The photoluminescence curve of ceramic powder.
Fig. 4, embodiment 5 ceramic powders are applied to the stress irradiance characteristic of circular resin cylinder.
The electroluminescence characters of the film of Fig. 5, the preparation of embodiment 5 ceramic powders.
Embodiment:
The present invention is further described below in conjunction with embodiment.
Ba, Sr, Ca adopt its carbonate raw material or part to adopt the titanate raw material, Mg, Pb, Zn, Cu, Cr adopt its carbonate or oxide compound, Ti adopts titanate or its oxide compound, rare earth element R adopts its oxide compound or nitrate raw material, quadrivalent element M adopts its oxide raw material, according to its molecular formula Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Wherein, 0≤x1≤0.18,0.21≤x2≤0.90,0.0001≤x3≤0.13,0.0001≤y≤0.05,0≤z≤0.20; A is dyad Mg, Pb, Zn, Cu or Cr, and R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is quadrivalent element Zr, Ce, Cu or Sn, selects to mix behind the raw material.
Proportioning and each raw material weight of embodiment 1#-7# sample are as shown in table 1.
Table 1.Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Complex phase ceramic powder proportioning and performance
Raw material (g) Phase structure PL (intensity) (612nm) ML (intensity) (1000N) EL (intensity) (25kv/cm, 60Hz)
1 #(x1＝0， x2＝0.898， x3＝0， y＝0.002， z＝0) BaCO 3＝0.7910 CaCO 3＝3.5956 Pr 6O 11＝0.0136 TiO 2＝3.1992 Rich barium (Ba, Ca) TiO 3-Fu calcium (Ba, Ca) TiO 3 30 10 8
2 #(x1＝0.1， x2＝0.45， x3＝0， y＝0.002， z＝0) BaCO 3＝3.5436 SrCO 3＝0.5911 CaCO 3＝1.8018 Pr 6O 11＝0.0136 TiO 2＝3.1992 Rich barium (Ba, Sr, Ca) TiO 3-Fu calcium (Ba, Sr, Ca) TiO 3 136 23 18
3 #(x1＝0， x2＝0.898， x3＝0， y＝0.002， z＝0.05) BaCO 3＝0.7910 CaCO 3＝3.5956 Pr 6O 11＝0.0136 TiO 2＝3.0381 ZrO 2＝0.2489 Rich barium (Ba, Ca) (Ti, Zr) O 3-Fu calcium (Ba, Ca) (Ti, Zr) O 3 480 137 93
4 #(x1＝0， x2＝0.698， x3＝0， y＝0.002， z＝0.05) BaCO 3＝2.3729 CaCO 3＝2.7948 Pr 6O 11＝0.0136 TiO 2＝3.0381 ZrO 2＝0.2489 Rich barium (Ba, Ca) (Ti, Zr) O 3-Fu calcium (Ba, Ca) (Ti, Zr) O 3 510 142 97
5 #(x1＝0， x2＝0.5， x3＝0.1， y＝0.002， z＝0.01) BaCO 3＝3.1481 CaCO 3＝2.0020 ZnO＝0.3256 Pr 6O 11＝0.0136 TiO 2＝3.1672 ZrO 2＝0.0498 Rich barium (Ba, Ca, Zn) (Ti, Zr) O 3-Fu calcium (Ba, Ca, Zn) (Ti, Zr) O 3 874 535 386
6 #(x1＝0.16， x2＝0.42， x3＝0， y＝0.002， z＝0) BaCO 3＝3.3063 SrCO 3＝0.9458 CaCO 3＝1.602 Pr 6O 11＝0.0136 TiO 2＝3.1992 Rich barium (Ba, Sr, Ca) TiO 3-Fu calcium (Ba, Sr, Ca) TiO 3
7 #(x1＝0， x2＝0.5， x3＝0.01， y＝0.002， z＝0.01) BaCO 3＝3.8600 CaCO 3＝2.0020 ZnO＝0.0326 Pr 6O 11＝0.0136 TiO 2＝3.1672 ZrO 2＝0.0498 Rich barium (Ba, Ca, Zn) (Ti, Zr) O 3-Fu calcium (Ba, Ca, Zn) (Ti, Zr) O 3
* annotate: PL is a photoluminescence, and ML is a stress irradiance, and EL is electroluminescent; Intensity is relative value.
The compound of above-mentioned each prescription is put into mortar, add dehydrated alcohol and ground 1 hour, the discharging oven dry; Place crucible to carry out pre-burning 900-1100 ℃ then, be incubated 1-7 hour; Pre-imitation frosted glass powder is done grinding slightly, place crucible, under oxygen atmosphere, sintering temperature is in 1100 ℃～1450 ℃ scopes, is incubated after 4 hours, obtains rich barium phase Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3-Fu calcium phase Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3The two-phase coexistent ceramic composite powders.With the ceramic powder that makes mix with organic resin be coated on cylindrical resin surface or directly make the cylindrical resin body after, can the test stress luminescent properties.The ceramic powder that makes mixed being coated on the ito glass surface with organic resin, apply back electrode then, can the testing electroluminescent performance.
Embodiment 1 #-7 #Prepared Ba fills a prescription 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3The two-phase composite ceramics is a kind of natural two-phase composite material with self-assembly characteristic, by the Ba of rich Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Ba with rich Ca 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Form, the ratio of Ba/Ca is relevant with the content that other adds element separately.Embodiment 1 #-7 #The chemical dosage ratio of each component of filling a prescription is as shown in table 1.The X-ray diffraction analysis collection of illustrative plates of the two-phase composite ceramics that makes as shown in Figure 1, biphase form be respectively the rich barium of uhligite four directions mutually with rich calcium quadrature mutually.The rational curve of photoluminescence (PL) has provided Ba respectively as shown in Figures 2 and 3 0.1Ca 0.898Pr 0.002Ti 1-zZr zO 3(z=0.05 is embodiment 3#) and Ba 1-x2Ca X2Pr 0.002Ti 0.95Zr 0.05O 3The photoluminescence curve of (x2=0.698 is embodiment 4#) ceramic powder.The relation curve of the luminous intensity-stress of stress irradiance (ML) is (embodiment 5#) as shown in Figure 4, and the peak strength of stress irradiance increases with the increase of stress application, and is linear.This shows the information that can obtain stress by the measurement of stress irradiance intensity.To some large-scale components, parts, the stress distribution of irregular element, parts adopts other method can't obtain the information of stress distribution, adopts material of the present invention to test, and promptly can be resolved.The transient response of electroluminescent (EL) and the relation curve of luminous intensity-strength of electric field be (embodiment 5#) as shown in Figure 5.Material of the present invention can be used as electroluminescent device, as the material use of flat-panel screens.
Embodiment among the present invention only is used for that the present invention will be described, does not constitute the restriction to the claim scope, and other substituting of being equal in fact that those skilled in that art can expect are all at protection domain of the present invention.

Claims (6)

1, a kind of diphase ceramic material with stress irradiance and electroluminescence characters is characterized in that, its molecular formula is Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Wherein, 0≤x1≤0.18,0.21≤x2≤0.90,0.0001≤x3≤0.13,0.0001≤y≤0.05,0≤z≤0.20; A is dyad Mg, Pb, Zn, Cu or Cr, and R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is quadrivalent element Zr, Ce, Cu or Sn.
2, the diphase ceramic material with stress irradiance and electroluminescence characters according to claim 1 is characterized in that it comprises two-phase, first mutually in the content of barium greater than the content of calcium, second mutually in the content of calcium greater than the content of barium.
3, the diphase ceramic material with stress irradiance and electroluminescence characters according to claim 2 is characterized in that, first mutually in, 0≤x1≤0.15,0.21≤x2≤0.50; Second mutually in, 0≤x1≤0.15,0.21≤x2≤0.50.
4, a kind of preparation has the method for the diphase ceramic material of stress irradiance and electroluminescence characters, it is characterized in that, comprise step: a, Ba, Sr, Ca adopt its carbonate raw material or part to adopt the titanate raw material, Mg, Pb, Zn, Cu, Cr adopt its carbonate or oxide compound, Ti adopts titanate or its oxide compound, rare earth element R adopts its oxide compound or nitrate raw material, and quadrivalent element M adopts its oxide raw material, according to its molecular formula Ba 1-x1-x2-x3-ySr X1Ca X2A X3R yTi 1-zM zO 3Wherein, 0≤x1≤0.18,0.21≤x2≤0.90,0.0001≤x3≤0.13,0.0001≤y≤0.05,0≤z≤0.20; A is dyad Mg, Pb, Zn, Cu or Cr, and R is La, Pr, Nd, Sm, Eu, Gd, Tb, Dy or Er, and M is quadrivalent element Zr, Ce, Cu or Sn, selects to mix behind the raw material; Add dehydrated alcohol or deionized water and in mortar, grind, obtain powder after the discharging oven dry;
B, place crucible to carry out pre-burning powder, calcined temperature 900-1100 ℃, be incubated 1-7 hour;
C, preburning powdered material is ground,, can obtain having the multiple phase ceramic material of stress irradiance and electroluminescence characters 1100 ℃～1500 ℃ insulations 2～4 hours.
5, preparation according to claim 4 has the method for the diphase ceramic material of stress irradiance and electroluminescence characters, it is characterized in that, diphase ceramic material with stress irradiance and electroluminescence characters comprises two-phase, first mutually in the content of barium greater than the content of calcium, second mutually in the content of calcium greater than the content of barium.
6, preparation according to claim 5 has the method for the diphase ceramic material of stress irradiance and electroluminescence characters, it is characterized in that, first mutually in, 0≤x1≤0.15,0.21≤x2≤0.50; Second mutually in, 0≤x1≤0.15,0.21≤x2≤0.50.
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CN103194223A (en) * 2012-01-06 2013-07-10 中国科学院城市环境研究所 Novel difunctional ultraviolet luminescent material having long afterglow and mechanoluminescence
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CN104774613A (en) * 2015-03-17 2015-07-15 同济大学 Stannate based elastic stress luminescent material, preparation method, and applications thereof
CN105542768A (en) * 2016-01-25 2016-05-04 深圳市聚飞光电股份有限公司 Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs
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CN103194223A (en) * 2012-01-06 2013-07-10 中国科学院城市环境研究所 Novel difunctional ultraviolet luminescent material having long afterglow and mechanoluminescence
CN103923653A (en) * 2014-05-05 2014-07-16 青岛大学 Red long-afterglow luminescent material and preparation method thereof
CN103923653B (en) * 2014-05-05 2015-12-30 青岛大学 A kind of red long afterglow luminous material and preparation method thereof
CN104774613A (en) * 2015-03-17 2015-07-15 同济大学 Stannate based elastic stress luminescent material, preparation method, and applications thereof
CN105542768A (en) * 2016-01-25 2016-05-04 深圳市聚飞光电股份有限公司 Preparation method of MxSr(1-x)TiO3:Eu3+ high-purity red fluorescent powder used for high-color-gamut LEDs
CN105567232A (en) * 2016-01-25 2016-05-11 深圳市聚飞光电股份有限公司 Preparation method of titanate fluorescent powder for LED
CN105567232B (en) * 2016-01-25 2018-08-24 深圳市聚飞光电股份有限公司 A kind of preparation method of LED titanate fluorescent powders

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