CN105060880B - A kind of low temperature sintering leadless piezoelectric luminescent ceramic powder, ceramics and preparation method thereof - Google Patents
A kind of low temperature sintering leadless piezoelectric luminescent ceramic powder, ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to leadless piezoelectric material material and photoelectric material crossing domain, a kind of the titanium barium stannate leadless piezoelectric luminescent ceramic powder and ceramics of Er doping are disclosed, its chemical general formula is Er x Ba1‑ x Ti0.96Sn0.04O3, whereinx=0.1~1.2%.Leadless piezoelectric luminescent ceramic of the present invention is obtained using piezoelectric ceramics technology of preparing and the raw material of industry, and ceramic sintering temperature is reduced to 1200~1400 DEG C, the piezoelectric constant of materiald 33Value is up to 400pC/N, while also having high light Photoluminescence Properties, the monochromaticjty that lights is good, belongs to new multifunctional material.The titanium barium stannate leadless piezoelectric luminescent material of Er doping has excellent piezoelectric property and photoelectric properties, is with a wide range of applications in fields such as the integrated, sensors of micro electronmechanical, photoelectricity.
Description
Technical field
The invention belongs to leadless piezoelectric material material and photoelectric material crossing domain, and in particular to a kind of titanium tin of rare earth Er doping
Sour barium low temperature sintering leadless piezoelectric luminescent ceramic powder, ceramics and preparation method thereof.
Background technology
Piezoelectricity ferro material has a wide range of applications in terms of the detection of information, conversion, processing, display and storage, is
Important high-tech functional material, but account for piezoelectric leading position at present is still lead base pressure that lead content is up to 70%
Electroceramics lead zirconate titanate (PZT).Lead base ceramics prepare, using and waste procedures in ecological environment and human health are caused sternly
Endanger again, countries in the world, such as European Union, the U.S. and Japan successively make laws, and the Ministry of Information Industry of China is also drafted《Electronic information is produced
Product prevention and cure of pollution management method》, it is prevented or restricted from the use of lead in the electronics industry.Therefore, finding can be instead of the unleaded of PZT
Piezoelectric turns into one of urgent task of field of electronic materials, and (silicate is circulated a notice of, 2010,29 (3)：616-626；Sichuan is pedagogical
College journal, 2010,33 (1)：117-131).According to PZT research experience, in order to improve the piezoelectricity of leadless piezoelectric ceramics
Can, research, which is concentrated mainly on, constructs in quasi- homotype phase boundary.Research discovery, barium calcium zirconate titanate (Ba0.99-xCa0.01Ti0.98Zr0.02O3)
Ceramics obtain great piezoelectric property d near quasi- homotype phase boundary33Up to 400-600pC/N (Physical Review
Letters,2009,103:257602；Applied Physics Letters,2011,99:122901).But the component
Contain dystectic Ca and Zr elements in piezoelectric ceramics, cause its sintering temperature higher, typically between 1400-1600 DEG C.Compared with
High sintering temperature is unfavorable for the preparation of ceramic material, does not also meet the requirement of energy-conserving and environment-protective.Find a kind of electrical with high pressure
Can and can low sintering ceramic material preparation method be referred to as the task of top priority.
Up-conversion luminescent material is that a kind of excited in infrared laser can launch the material of visible ray down, false proof, red
The field such as outer detection, three stereoscopic displays, short wavelength's all solid state laser, biomarkers is widely used.Upper conversion hair
Light host material mainly have fluoride, chloride, oxide etc. (《A kind of up-conversion fluorescence host material NaYF4Nanocrystalline system
Preparation Method》, Chinese invention patent, publication number CN1935938).But its preparation technology is complicated, high cost, environmental requirement is harsh,
And fluoride is toxic, heat endurance and chemical stability are poor, are difficult in synthesizer integrated.In the recent period, Zou et al. is dilute
(1-x) BaTiO of native Pr doping3-xCaTiO3Research (the Journal of up-conversion luminescence is carried out in perovskite structure oxide
of Applied Physics,2013,114:073103), piezoelectricity and it is luminous it is integrated on achieve initial achievements.
Therefore, there is the leadless piezoelectric material material of high piezoelectric property as a class, while its piezoelectric property is improved, also
It can realize that its efficiently upper conversion is luminous, be the material of great Research Significance and application value.According to the Patents and text found
In offering, the preparation and the electroactive correlative study of high pressure of the titanium stannic acid titanate ceramicses of rare earth oxide Er doping are had no.The present invention is
A kind of Multifunction material with high tension performance and luminescent properties, component is simple, and sintering temperature is low, in micro electronmechanical, light
It is electrically integrated, the field such as photoelectric sensor is with a wide range of applications.
The content of the invention
It is an object of the invention to provide a kind of luminous pottery of the titanium barium stannate low temperature sintering leadless piezoelectric of rare earth Er doping
Porcelain powder, ceramics and preparation method thereof, the component of the leadless piezoelectric luminescent ceramic are simple, and acquisition can be sintered at low temperature,
While keeping high tension performance, with efficient Upconversion luminescence.The present invention rare earth Er doping barium zirconium phthalate without
Lead piezoluminescence pressure material electrical property heat endurance, chemical stability are good, and luminous intensity is high, and is single green light, and material is easy
It is with low cost in synthesis.
In order to achieve the above objects and other related objects, first aspect present invention provides a kind of leadless piezoelectric luminescent ceramic powder
Body, its chemical general formula is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.1~1.2%.
Above-mentioned chemical general formula ErxBa1-xTi0.96Sn0.04O3In, the right index number of element and letter represent each corresponding element
Molar ratio relation.
X can for 0.1~0.2%, 0.2~0.4%, 0.4~0.5%, 0.5~0.6%, 0.6~0.8%, 0.8~
1.0% or 1.0~1.2%.
It is preferred that, x=0.1%, 0.2%, 0.4%, 0.5%, 0.6%, 0.8%, 1.0% or 1.2%.
Second aspect present invention provides a kind of leadless piezoelectric luminescent ceramic, and its chemical general formula is ErxBa1- xTi0.96Sn0.04O3, wherein x=0.1~1.2%.
Above-mentioned chemical general formula ErxBa1-xTi0.96Sn0.04O3In, the right index number of element and letter represent each corresponding element
Molar ratio relation.
X can for 0.1~0.2%, 0.2~0.4%, 0.4~0.5%, 0.5~0.6%, 0.6~0.8%, 0.8~
1.0% or 1.0~1.2%.
It is preferred that, x=0.1%, 0.2%, 0.4%, 0.5%, 0.6%, 0.8%, 1.0% or 1.2%.
Third aspect present invention provides a kind of leadless piezoelectric luminescent ceramic raw powder's production technology, comprises the following steps：
1) raw material is weighed by the stoichiometric proportion of element in above-mentioned chemical general formula：Compound containing Ba, compound containing Sn, containing Ti
Compound and compound containing Er；
2) by step 1) in the raw material that weighs using solvent as medium ball milling, obtain slurry；
3) slurry is dried, pre-burning, produce chemical general formula for ErxBa1-xTi0.96Sn0.04O3Leadless piezoelectric
Luminescent ceramic powder.
It is preferred that, the compound containing Ba is BaCO3。
It is preferred that, the compound containing Sn is SnO2。
It is preferred that, the compound containing Ti is TiO2。
It is preferred that, the compound containing Er is Er2O3。
It is preferred that, the step 2) in, the time of ball milling is 4-6h.It is furthermore preferred that the time of ball milling is 6h.
It is preferred that, the step 2) in, the solvent is selected from absolute ethyl alcohol or deionized water.
It is preferred that, the step 3) in, the condition of the drying is：8~12h of insulation drying at 80~100 DEG C.
It is preferred that, the step 3) in, the condition of the pre-burning is：Calcined temperature is 900~1200 DEG C, and burn-in time is
4~8h.
It is furthermore preferred that calcined temperature is 1100 DEG C.
It is furthermore preferred that burn-in time is 6h.
Fourth aspect present invention provides a kind of preparation method of leadless piezoelectric luminescent ceramic, comprises the following steps：Will be unleaded
The addition binding agent granulation of piezoluminescence ceramic powder, compressing, row is viscous, sintering, produces chemical general formula for ErxBa1- xTi0.96Sn0.04O3Leadless piezoelectric luminescent ceramic, the leadless piezoelectric luminescent ceramic powder be above-mentioned leadless piezoelectric luminescent ceramic
Leadless piezoelectric luminescent ceramic powder made from powder or above-mentioned preparation method.
It is preferred that, the binding agent is selected from polyvinyl butyral resin (PVB) or polyvinyl alcohol (PVA).
It is preferred that, the consumption of the binding agent is 5~8wt% of the leadless piezoelectric luminescent ceramic powder.It is furthermore preferred that
The consumption of the binding agent is the 6wt% of the leadless piezoelectric luminescent ceramic powder.
It is preferred that, the compressing relative pressure is 100~200MPa.It is furthermore preferred that the compressing phase
It is 150MPa to pressure.Diameter 10mm, thickness 1mm disk can be pressed under 100~200MPa relative pressure.
It is preferred that, the condition of the sintering is：In atmosphere 2~6h is sintered in 1200~1400 DEG C.It is furthermore preferred that described
The condition of sintering is：In atmosphere 4h is sintered in 1300 DEG C.
The present invention is obtained using piezoelectric ceramics technology of preparing and the raw material of industry, and the principal crystalline phase of the system is perovskite structure,
Er prepared by the present inventionxBa1-xTi0.96Sn0.04O3Ceramic material, by rare earth Er doping by before orthogonal opposite tetragonal phase converting peak
Move, ceramics are in single phase structure, obtain preferable piezoelectric property temperature stability.Piezoelectric constant d33It is all higher than 200pC/N,
Reach as high as 400pC/N.Meanwhile, the present invention is infrared ray excited up-conversion luminescent material, and luminous intensity is high, in wavelength
980nm's is infrared ray excited lower with very strong Upconversion luminescence, and is single green light, and luminous intensity is adjustable.This hair
Bright stable preparation process is reliable, is efficient piezoelectricity, the photoelectric material of a kind of Multifunction, micro electronmechanical, photoelectricity it is integrated, pass
The fields such as sensor are with a wide range of applications.
Brief description of the drawings
Fig. 1 is XRD spectra of the embodiment one to the sample of embodiment eight；
Fig. 2 be embodiment one to the sample of embodiment eight ferroelectric hysteresis loop and piezoelectric constant with change of component graph of a relation；
Fig. 3 is luminous collection of illustrative plates of the embodiment one to the sample of embodiment eight in the case where wavelength 980nm is infrared ray excited；
Fig. 4 is that the single green light that embodiment one to the sample of embodiment eight is sent in the case where wavelength 980nm is infrared ray excited is shone
Piece.
Brief description of the drawings：The color of Fig. 4 grey parts is green.
Embodiment
The present invention is expanded on further with reference to specific embodiment, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It should be clear that in the following example not specifically dated process equipment or device using conventional equipment in the art or
Device；All pressure values and scope are all referring to relative pressure, and the raw material used is also conventional use of raw material in the art.
In addition, it is to be understood that the one or more method and steps mentioned in the present invention do not repel before and after the combination step
There can also be other method step or other method step can also be inserted between the step of these are specifically mentioned, unless separately
It is described；It should also be understood that the combination annexation between the one or more equipment/devices mentioned in the present invention is not repelled
Can also have other equipment/device before and after the unit equipment/device or two equipment/devices specifically mentioning at these it
Between can also insert other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the numbering of various method steps is only
Differentiate the convenient tool of various method steps, rather than ordering or restriction enforceable model of the invention for limitation various method steps
Enclose, being altered or modified for its relativeness is of the invention enforceable when being also considered as in the case of without essence change technology contents
Category.
The chemical general formula of embodiment 1 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.1%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using absolute ethyl alcohol as medium ball milling 4h, and slurry obtained by ball milling is pre- at 900 DEG C in being incubated at 80 DEG C after 10h drying powders
4h is burnt, chemical formula is obtained for Er0.001Ba0.999Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 5wt% polyvinyl butyral resin (PVB) granulation,
It is compressing under 100MPa relative pressure, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, in sky
2h is sintered in 1200 DEG C in gas, chemical formula is obtained for Er0.001Ba0.999Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is orthorhombic phase perovskite structure.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=7.4 μ C/cm2For,
Piezoelectric constant d33=260pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 180.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 2 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.2%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using absolute ethyl alcohol as medium ball milling 4h, and slurry obtained by ball milling at 80 DEG C in being incubated after 8h drying powders, in 900 DEG C of pre-burnings
4h, obtains chemical formula for Er0.002Ba0.998Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 5wt% PVB granulations, under 100MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 2h are sintered in 1200 DEG C in atmosphere,
Chemical formula is obtained for Er0.002Ba0.998Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is orthorhombic phase perovskite structure.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=8 μ C/cm2For pressure
Electric constant d33=320pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 280.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 3 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.4%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using absolute ethyl alcohol as medium ball milling 4h, and slurry obtained by ball milling is pre- at 1000 DEG C in being incubated at 80 DEG C after 10h drying powders
4h is burnt, chemical formula is obtained for Er0.004Ba0.996Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 6wt% PVB granulations, under 100MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 5h are sintered in 1200 DEG C in atmosphere,
Chemical formula is obtained for Er0.004Ba0.996Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is the perovskite structure that orthorhombic phase and Tetragonal coexist.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=8.5 μ C/cm2For,
Piezoelectric constant d33=380pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 460.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 4 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.5%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using deionized water as medium ball milling 5h, and slurry obtained by ball milling is pre- at 1100 DEG C in being incubated at 90 DEG C after 9h drying powders
4h is burnt, chemical formula is obtained for Er0.005Ba0.995Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 7wt% PVB granulations, under 150MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 6h are sintered in 1250 DEG C in atmosphere,
Chemical formula is obtained for Er0.005Ba0.995Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is the perovskite structure that orthorhombic phase and Tetragonal coexist.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=10.5 μ C/cm2
For piezoelectric constant d33=400pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 560.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 5 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.6%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using deionized water as medium ball milling 6h, and slurry obtained by ball milling is pre- at 1100 DEG C in being incubated at 90 DEG C after 8h drying powders
4h is burnt, chemical formula is obtained for Er0.006Ba0.994Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 7wt% PVB granulations, under 150MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 7h are sintered in 1300 DEG C in atmosphere,
Chemical formula is obtained for Er0.006Ba0.994Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is the perovskite structure that orthorhombic phase and Tetragonal coexist.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=9.5 μ C/cm2For,
Piezoelectric constant d33=380pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 660.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 6 is ErxBa1-xTi0.96Sn0.04O3, wherein x=0.8%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using deionized water as medium ball milling 6h, and slurry obtained by ball milling is pre- at 1200 DEG C in being incubated at 90 DEG C after 10h drying powders
4h is burnt, chemical formula is obtained for Er0.008Ba0.992Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 8wt% PVB granulations, under 200MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 7h are sintered in 1400 DEG C in atmosphere,
Chemical formula is obtained for Er0.008Ba0.992Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is Tetragonal perovskite structure.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=8.5 μ C/cm2For,
Piezoelectric constant d33=270pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 960.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 7 is ErxBa1-xTi0.96Sn0.04O3, wherein x=1.0%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using absolute ethyl alcohol as medium ball milling 4h, and slurry obtained by ball milling is pre- at 1200 DEG C in being incubated at 80 DEG C after 8h drying powders
12h is burnt, chemical formula is obtained for Er0.01Ba0.99Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 8wt% PVB granulations, under 200MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 2h are sintered in 1400 DEG C in atmosphere,
Chemical formula is obtained for Er0.01Ba0.99Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is Tetragonal perovskite structure.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=8 μ C/cm2For pressure
Electric constant d33=220pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 700.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The chemical general formula of embodiment 8 is ErxBa1-xTi0.96Sn0.04O3, wherein x=1.2%
Raw material is weighed by the stoichiometric proportion of element in chemical general formula：BaCO3、SnO2、TiO2And Er2O3；By the original weighed
Feed powder body is using absolute ethyl alcohol as medium ball milling 6h, and slurry obtained by ball milling at 100 DEG C in being incubated after 10h drying powders, at 1100 DEG C
Pre-burning 4h, obtains chemical formula for Er0.012Ba0.988Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic powder.
The leadless piezoelectric luminescent ceramic powder of acquisition is added to its weight 8wt% PVB granulations, under 200MPa pressure
It is compressing, obtain diameter 10mm, thickness 1mm disk；After ceramic abundant row is glued, 2h are sintered in 1200 DEG C in atmosphere,
Chemical formula is obtained for Er0.012Ba0.988Ti0.96Sn0.04O3Leadless piezoelectric luminescent ceramic.
Leadless piezoelectric luminescent ceramic fine grinding processing to acquisition, by silver electrode after ultrasonic cleaning, tests the electricity of ceramics sample
Hysteresis curves, polarize 20 minutes at room temperature, test the piezoelectric property parameters of ceramics sample；By the sample after polishing in 980nm ripples
Long infrared ray excited lower test up-conversion luminescence.
Fig. 1 gives the XRD spectrum of gained sample, it is seen that material is Tetragonal perovskite structure.
Fig. 2 gives the ferroelectric hysteresis loop and piezoelectric constant of gained sample.Its residual polarization P at room temperaturer=5.5 μ C/cm2For,
Piezoelectric constant d33=200pC/N.
Fig. 3 gives the infrared ray excited up-conversion luminescence collection of illustrative plates of gained sample, and emission wavelength 550nm, hair are changed thereon
Luminous intensity is 600.
Fig. 4 gives the single green radiograph sent in the case where wavelength 980nm is infrared ray excited of gained sample.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of leadless piezoelectric luminescent ceramic powder, it is characterised in that the chemical general formula of the leadless piezoelectric luminescent ceramic powder
For ErxBa1-xTi0.96Sn0.04O3, wherein x=0.1~0.8%.
2. a kind of leadless piezoelectric luminescent ceramic, it is characterised in that the chemical general formula of the leadless piezoelectric luminescent ceramic is ErxBa1- xTi0.96Sn0.04O3, wherein x=0.1~0.8%.
3. a kind of leadless piezoelectric luminescent ceramic raw powder's production technology as claimed in claim 1, it is characterised in that including as follows
Step：
1) stoichiometric proportion of element weighs raw material in the chemical general formula according to claim 1：Compound containing Ba, compound containing Sn,
Compound containing Ti and compound containing Er；
2) by step 1) in the raw material that weighs using solvent as medium ball milling, obtain slurry；
3) slurry is dried, pre-burning, produce chemical general formula for ErxBa1-xTi0.96Sn0.04O3The luminous pottery of leadless piezoelectric
Porcelain powder.
4. leadless piezoelectric luminescent ceramic raw powder's production technology according to claim 3, it is characterised in that the step 2)
In, the time of ball milling is 4-6h.
5. leadless piezoelectric luminescent ceramic raw powder's production technology according to claim 3, it is characterised in that the step 2)
In, the solvent is selected from absolute ethyl alcohol or deionized water.
6. leadless piezoelectric luminescent ceramic raw powder's production technology according to claim 3, it is characterised in that the step 3)
In, the condition of the drying is：8~12h of insulation drying at 80~100 DEG C；The condition of the pre-burning is：Calcined temperature is
900~1200 DEG C, burn-in time is 4~8h.
7. a kind of preparation method of leadless piezoelectric luminescent ceramic as claimed in claim 2, it is characterised in that including following step
Suddenly：By the addition binding agent granulation of leadless piezoelectric luminescent ceramic powder, compressing, row is viscous, sintering, and producing chemical general formula is
ErxBa1-xTi0.96Sn0.04O3Leadless piezoelectric luminescent ceramic, the leadless piezoelectric luminescent ceramic powder be claim 1 described in
Leadless piezoelectric luminescent ceramic made from preparation method described in leadless piezoelectric luminescent ceramic powder or claim 3 to 6 any one
Powder.
8. the preparation method of leadless piezoelectric luminescent ceramic according to claim 7, it is characterised in that the use of the binding agent
Measure as 5~8wt% of the leadless piezoelectric luminescent ceramic powder.
9. the preparation method of leadless piezoelectric luminescent ceramic according to claim 7, it is characterised in that described compressing
It is 100~200MPa with respect to pressure.
10. the preparation method of leadless piezoelectric luminescent ceramic according to claim 7, it is characterised in that the bar of the sintering
Part is：In atmosphere 2~6h is sintered in 1200~1400 DEG C.
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