CN106916581B - A kind of silicate ability of reverse photochromism material and preparation method thereof - Google Patents
A kind of silicate ability of reverse photochromism material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of silicate ability of reverse photochromism material, chemical formula Ca3‑x‑yZrSi2O9:xSm3+,yR3+, wherein 0 < x≤0.2,0≤y≤0.1；R is selected from one or more in Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.Under the irradiation of ultraviolet light, the color of sample surfaces becomes light brown from white to silicate ability of reverse photochromism material provided by the invention, and under the light of long wavelength or heat treatment, the color of sample surfaces reverts to white.The silicate ability of reverse photochromism material has good fatigue resistance and thermal stability.Such inorganic photochromic material can be used for the fields such as photoswitch, anti-fake, decoration, optical device materials, optical information storage, the photograph of autography holographic recording, inductor and radiation metering meter.In addition, the codope by other rare earth ions realizes the function of being regulated and controled to photochromic degree.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of silicate ability of reverse photochromism material and its preparation
Method.
Background technique
The mankind had found that photochromism before more than 100 years, but did not caused widely to pay attention to.Until
20th century 50, the sixties, Hirshberg propose that photochromic material can be applied to optical recording storage and U.S.'s Corning work
Making two material scholar's Amistead and Stooky first discoveries of room has ability of reverse photochromism containing silver halide (AgX) glass
Performance, the characteristic of photochromic material starts to cause the more and more interest of people at this time.
It is photochromic to refer to that certain compounds molecular structure under the light action of certain wavelength and intensity become
Change, so as to cause its corresponding change of absorption peak, that is, color to light, and this change is generally reversible.It is this unusual
Phenomenon changes self color according to environment just as chameleon in nature, to achieve the purpose that predation and self-protection.Institute
With photochromic material can be used in military affairs doing hidden material, and can reach by the change of self color can not examine in enemy
When feel lock onto target and hide enemy tracking purpose.Meanwhile photochromic material can be also used for RMB anti-counterfeiting
Ink, optical information gene material, the photograph of autography holographic recording etc., have good application prospect and are widely applied field.
Currently, photochromic material application on based on organic photochromic material, development trend is good.But
Organic photochromic material has some unavoidable birth defects, for example, the organic matter environmental pollution being used to prepare compared with
Greatly, thermal stability is poor, and fatigue resistance is poor, in practical applications discoloration reduction etc..In comparison, inorganic photochromic
The superior functions such as material has fatigue resistance good, and thermal stability is good, and discoloration is very fast and the duration is long.Reported inorganic light
Off-color material is caused to have: Mg4Ga8Ge2O20:Cr3+(J.Mater.Lett., Vol.4,6614, (2016)), CaAl2O4: Eu2+,Nd3+
(Opt.Mater.Express, Vol.3,787, (2013)), ZnGa2O4: Bi3+(Opt.Mater.Express,Vol.2,
1378, (2012)), Sr2SnO4: Eu3+(Appl.Phys.Lett.,Vol.102,031110,(2013)),Ba5(PO4)3Cl:Eu2 +,Y3+(J.Photochem.Photobiol A, Vol.251,100, (2013)), BaMgSiO4: Eu2+
(Appl.Phys.Lett., Vol.97,181905, (2010)), Sr3YNa(PO4)3F:Eu2+(J.Mater.Lett.,Vol.3,
9435, (2015)), SrTiO3And TiO2(Phys.Rev.Lett., Vol.21,1331, (1968)), Zn2GeO4:Eu2+
(Mater.Lett., Vol.134,187, (2014)), Na0.5Bi2.5Nb2O9:Er3+(Appl.Mater.Interfaces,
Vol.8,4789, (2016)), LiGa5O8:Cr3+(Sci.Rep., Vol.3,1554. (2013)), Ba3MgSi2O8:Eu2+
(J.Lumin., Vol.173,237, (2016)), Sr3GdNa(PO4)3F:Eu2+(Sensors and Actuators B,
Vol.245,256, (2017)), patent (application number: 201410622062.6) discloses a kind of halogen-phosphate ability of reverse photochromism
Material Sr3-xM1-yNa(PO4)3F:xEu2+,yR3+(M=Y, Gd).It can be seen that the type of current inorganic photochromic material is also
It is fewer.The research of inorganic photochromic material is in the initial development stage so far without biggish breakthrough, preparation method with
And the research with photochromic properties material is also immature.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of silicate ability of reverse photochromism material and its
Preparation method, silicate ability of reverse photochromism material provided by the invention can enrich the type of inorganic photochromic material, should
It is colourless reversible between light brown that silicate ability of reverse photochromism material can realize that the silicate of samaric ion doping is realized
It is photochromic.
The present invention provides a kind of silicate ability of reverse photochromism material, chemical formula Ca3-x-yZrSi2O9:xSm3+,yR3+,
Wherein, 0 < x≤0.2,0≤y≤0.1；R is selected from a kind of in Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu
Or it is a variety of.
The present invention also provides a kind of preparation methods of above-mentioned silicate ability of reverse photochromism material, comprising the following steps:
A) calcium source compound, zirconium source compound, silicon source compound, samarium source compound and compound containing R element are mixed
It is ground after conjunction, in air atmosphere by the first calcining, obtains presoma；
B) by after presoma grinding, in air atmosphere by the second calcining, it is reversible to obtain silicate for regrinding
Photochromic material.
Preferably, the calcium source compound is selected from calcium carbonate, calcium oxide or calcium nitrate.
Preferably, the zirconium source compound is selected from zirconium oxide or zirconium nitrate.
Preferably, the silicon source compound is selected from silica.
Preferably, the samarium source compound is selected from the oxide containing samarium or the nitrate containing samarium.
Preferably, the compound of the R element is selected from the oxide containing R element or the nitrate containing R element.
Preferably, the temperature of first calcining is 800~1000 DEG C, and the time of first calcining is 5~6 hours.
Preferably, the temperature of second calcining is 1350~1400 DEG C, and the time of second calcining is 8~10 small
When.
Compared with prior art, the present invention provides a kind of silicate ability of reverse photochromism material, chemical formula Ca3-x- yZrSi2O9:xSm3+,yR3+, wherein 0 < x≤0.2,0≤y≤0.1；R is selected from Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho,
It is one or more in Er, Tm, Yb and Lu.Silicate ability of reverse photochromism material provided by the invention under the irradiation of ultraviolet light,
The color of sample surfaces becomes light brown from white, and under the light of long wavelength or heat treatment, the color of sample surfaces is reverted to
White.The silicate ability of reverse photochromism material has good fatigue resistance and thermal stability.Such inorganic photochromic material
Material can be used for photoswitch, anti-fake, decoration, optical device materials, optical information storage, autography holographic recording take a picture, inductor and
The fields such as radiation metering meter.In addition, the codope by other rare earth ions realizes the function regulated and controled to photochromic degree
Energy.In addition, the preparation method of silicate ability of reverse photochromism material provided by the invention is simple, and it is low for equipment requirements, in air
It is prepared under atmosphere, and raw materials used cheap and easy to get.
Detailed description of the invention
Fig. 1 is silicate ability of reverse photochromism material C a prepared by embodiment 12.998ZrSi2O9:0.002Sm3+XRD diagram；
Fig. 2 is the silicate ability of reverse photochromism material of the preparation of embodiment 1 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Fig. 3 is the silicate ability of reverse photochromism material of the preparation of embodiment 2 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Fig. 4 is the silicate ability of reverse photochromism material of the preparation of embodiment 3 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Fig. 5 is the silicate ability of reverse photochromism material of the preparation of embodiment 4 under ultraviolet light and the irradiation of the alternating of heat treatment
Diffusing reflection spectrum；
Fig. 6 is the silicate ability of reverse photochromism material of the preparation of embodiment 5 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Fig. 7 is the silicate ability of reverse photochromism material of the preparation of embodiment 6 under ultraviolet light and the irradiation of the alternating of heat treatment
Diffusing reflection spectrum；
Fig. 8 is the silicate ability of reverse photochromism material of the preparation of embodiment 7 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Fig. 9 is the silicate ability of reverse photochromism material of the preparation of embodiment 8 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Figure 10 is the silicate ability of reverse photochromism material of the preparation of embodiment 9 under the irradiation of the alternating of ultraviolet light and visible light
Diffusing reflection spectrum；
Figure 11 is that silicate ability of reverse photochromism material prepared by embodiment 10 is irradiated in the alternating of ultraviolet light and visible light
Under diffusing reflection spectrum；
Figure 12 is that silicate ability of reverse photochromism material prepared by embodiment 11 is irradiated in ultraviolet light and the alternating of heat treatment
Under diffusing reflection spectrum；
Figure 13 is that silicate ability of reverse photochromism material prepared by embodiment 12 is irradiated in the alternating of ultraviolet light and visible light
Under diffusing reflection spectrum；
Figure 14 is that silicate ability of reverse photochromism material prepared by embodiment 13 is irradiated in the alternating of ultraviolet light and visible light
Under diffusing reflection spectrum；
Figure 15 is that silicate ability of reverse photochromism material prepared by embodiment 14 is irradiated in the alternating of ultraviolet light and visible light
Under diffusing reflection spectrum；
Figure 16 is that silicate ability of reverse photochromism material prepared by embodiment 15 is irradiated in the alternating of ultraviolet light and visible light
Under diffusing reflection spectrum.
Specific embodiment
The present invention provides a kind of silicate ability of reverse photochromism material, chemical formula Ca3-x-yZrSi2O9:xSm3+,yR3+,
Wherein, 0 < x≤0.2,0≤y≤0.1；R is selected from a kind of in Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu
Or it is a variety of.
In the present invention, x described in the chemical formula is Sm3+Doping content, 0 < x≤0.2, preferably 0.004≤x≤
0.006。
Y is R3+Doping content, 0≤y≤0.1, preferably, 0.004≤x≤0.006.
R is the rare earth element being doped in basis material, is selected from Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm,
It is one or more in Yb and Lu.Wherein, it may be implemented to regulate and control photochromic degree by the codope of R rare earth ion
Function.
Under the irradiation of ultraviolet light, the color of sample surfaces is by white for silicate ability of reverse photochromism material provided by the invention
Discoloration is light brown, and under the light of long wavelength or heat treatment, the color of sample surfaces reverts to white.
Wherein, the wavelength of the light of the long wavelength is preferably visible light, the wave-length coverage of the visible light: 400~
760nm。
The heat-treating methods are to be heated to 240 to 300 degree 3 to 6 minutes, and the temperature of the heating is preferably 270 degree,
The time of the heating is preferably 5 minutes.
The present invention also provides a kind of preparation methods of above-mentioned silicate ability of reverse photochromism material, comprising the following steps:
A) calcium source compound, zirconium source compound, silicon source compound, samarium source compound and compound containing R element are mixed
It is ground after conjunction, in air atmosphere by the first calcining, obtains presoma；
B) by after presoma grinding, in air atmosphere by the second calcining, it is reversible to obtain silicate for regrinding
Photochromic material.
The present invention compares calcium source compound, zirconium source compound, silicon source compound, samarium first, in accordance with the stoichiometry of final product
Source compound and compound containing R element are weighed.
Wherein, the calcium source compound is selected from calcium carbonate, calcium oxide or calcium nitrate, preferably silica.The zirconium source
It closes object and is selected from zirconium oxide or zirconium nitrate.The silicon source compound is selected from silica.The samarium source compound is selected from the oxidation containing samarium
Object or nitrate containing samarium, preferably samarium oxide.The compound of the R element is selected from the oxide containing R element or containing R element
Nitrate, preferably containing the oxide of R element.
Then it is ground after above-mentioned raw materials being mixed, preferably grinding uniformly, is mixed in the agate mortar for the grinding
Close object.
Then, the mixture is passed through into the first calcining in air atmosphere, obtains presoma.Wherein, it described first forges
The temperature of burning is 800~1000 DEG C, preferably 850~950 DEG C；The time of first calcining is 5~6 hours.In the present invention
In, mixture is preferably put into corundum Noah's ark by the calcining, is calcined in Muffle furnace in air atmosphere.
After obtaining presoma, ground being taken out after the presoma cooled to room temperature, then, in air atmosphere
Lower to calcine by second, regrinding obtains silicate ability of reverse photochromism material.
The temperature of second calcining is preferably 1350~1400 DEG C, and the time of second calcining is preferably 8~10 small
When.Second calcining carries out in the tube furnace of air atmosphere.
After second calcining, grinding after the calcined product cooled to room temperature is obtained into white powder, as silicon
Hydrochlorate ability of reverse photochromism material.
Under the irradiation of ultraviolet light, the color of sample surfaces is by white for silicate ability of reverse photochromism material provided by the invention
Discoloration is light brown, and under the light of long wavelength or heat treatment, the color of sample surfaces reverts to white.The silicate can backlight
Cause off-color material that there is good fatigue resistance and thermal stability.Such inorganic photochromic material can be used for photoswitch, it is anti-fake,
The fields such as decoration, optical device materials, optical information storage, the photograph of autography holographic recording, inductor and radiation metering meter.This
Outside, the function of being regulated and controled to photochromic degree is realized by the codope of other rare earth ions.In addition, provided by the invention
The preparation method of silicate ability of reverse photochromism material is simple, low for equipment requirements, prepares in air atmosphere, and institute
It is cheap and easy to get with raw material.
For a further understanding of the present invention, below with reference to embodiment to silicate ability of reverse photochromism material provided by the invention
Material and preparation method thereof is illustrated, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
According to chemical expression: Ca2.998ZrSi2O9:0.002Sm3+, weigh calcium carbonate, silica, zirconium oxide, samarium oxide,
It is put into corundum Noah's ark after grinding uniformly, is first warming up to 900 DEG C in Muffle furnace in air atmosphere, keeps the temperature 5 hours, it is natural
It is regrind after being cooled to room temperature, is then warming up to 1350 DEG C in tube furnace in air atmosphere, 8 hours are kept the temperature, in furnace
Regrinding is fine powder after cooled to room temperature in pipe, obtains silicate ability of reverse photochromism material C a2.998ZrSi2O9:
0.002Sm3+。
To above-mentioned silicate ability of reverse photochromism material C a2.998ZrSi2O9:0.002Sm3+XRD detection is carried out, as a result sees figure
1, Fig. 1 silicate ability of reverse photochromism material C a prepared for embodiment 12.998ZrSi2O9:0.002Sm3+XRD diagram.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 2, Fig. 2 are that silicate ability of reverse photochromism material prepared by embodiment 1 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 2
According to chemical expression: Ca2.995ZrSi2O9:0.005Sm3+Weigh calcium nitrate, silica, zirconium oxide, samarium oxide,
It is put into corundum Noah's ark after grinding uniformly, is first warming up to 900 DEG C in Muffle furnace in air atmosphere, keeps the temperature 6 hours, it is natural
It is regrind after being cooled to room temperature, is then warming up to 1350 DEG C in tube furnace in air atmosphere, 8 hours are kept the temperature, in furnace
Regrinding is fine powder after cooled to room temperature in pipe.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 3, Fig. 3 are that silicate ability of reverse photochromism material prepared by embodiment 2 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 3
According to chemical expression: Ca2.99ZrSi2O9:0.01Sm3+Weigh calcium carbonate, silica, zirconium oxide, samarium oxide grinds
It is put into corundum Noah's ark after mill is uniform, is first warming up to 950 DEG C in Muffle furnace in air atmosphere, keeps the temperature 6 hours, it is naturally cold
But to regrinding after room temperature, 1370 DEG C then is warming up in tube furnace in air atmosphere, 9 hours are kept the temperature, in boiler tube
Regrinding is fine powder after middle cooled to room temperature.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 4, Fig. 4 are that silicate ability of reverse photochromism material prepared by embodiment 3 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 4
According to chemical expression: Ca2.98ZrSi2O9:0.02Sm3+Weigh calcium nitrate, silica, zirconium oxide, samarium oxide grinds
It is put into corundum Noah's ark after mill is uniform, is first warming up to 1000 DEG C in Muffle furnace in air atmosphere, keeps the temperature 6 hours, it is natural
It is regrind after being cooled to room temperature, is then warming up to 1370 DEG C in tube furnace in air atmosphere, 10 hours are kept the temperature, in furnace
Regrinding is fine powder after cooled to room temperature in pipe.
Under conditions of ultraviolet light and 270 DEG C of heat treatment 5min alternately by above-mentioned silicate ability of reverse photochromism material
Diffusing reflection detection is carried out, as a result sees Fig. 5, Fig. 5 is the silicate ability of reverse photochromism material for preparing of embodiment 4 in ultraviolet light
With the diffusing reflection spectrum under heat treatment.The ability of reverse photochromism for showing that the material generates after ultraviolet light and heat treatment is existing
As.
Embodiment 5
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Ho3+, weigh calcium carbonate, silica, zirconium oxide, oxygen
Change samarium, holimium oxide is put into corundum Noah's ark after grinding uniformly, 950 DEG C is first warming up in Muffle furnace in air atmosphere, heat preservation
6 hours regrind after cooled to room temperature, 1400 DEG C are then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 6, Fig. 6 are that silicate ability of reverse photochromism material prepared by embodiment 5 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 6
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Dy3+, weigh calcium carbonate, silica, zirconium oxide, oxygen
Change samarium, dysprosia is put into corundum Noah's ark after grinding uniformly, 950 DEG C is first warming up in Muffle furnace in air atmosphere, heat preservation
6 hours regrind after cooled to room temperature, 1400 DEG C are then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Under conditions of ultraviolet light and 270 DEG C of heat treatment 5min alternately by above-mentioned silicate ability of reverse photochromism material
Diffusing reflection detection is carried out, as a result sees Fig. 7, Fig. 7 is the silicate ability of reverse photochromism material for preparing of embodiment 6 in ultraviolet light
With the diffusing reflection spectrum under heat treatment.The ability of reverse photochromism for showing that the material generates after ultraviolet light and heat treatment is existing
As.
Embodiment 7
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Gd3+Weigh calcium nitrate, silica, zirconium oxide, oxidation
Samarium, gadolinium oxide are put into corundum Noah's ark after grinding uniformly, 950 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 8, Fig. 8 are that silicate ability of reverse photochromism material prepared by embodiment 7 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 8
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Y3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, yttrium oxide are put into corundum Noah's ark after grinding uniformly, 950 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, as a result sees that Fig. 9, Fig. 9 are that silicate ability of reverse photochromism material prepared by embodiment 8 shines in the alternating of ultraviolet light and visible light
Diffusing reflection spectrum under penetrating.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 9
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Pr3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, praseodymium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 10, Figure 10 is alternating of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 9
Diffusing reflection spectrum under irradiation.The ability of reverse photochromism for showing that the material generates after the irradiation of the alternating of ultraviolet light and visible light is existing
As.
Embodiment 10
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Er3+Weigh calcium nitrate, silica, zirconium oxide, oxidation
Samarium, erbium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 11, Figure 11 is friendship of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 10
For the diffusing reflection spectrum under irradiation.Show the ability of reverse photochromism that the material generates after the irradiation of the alternating of ultraviolet light and visible light
Phenomenon.
Embodiment 11
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Yb3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, ytterbium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Under conditions of ultraviolet light and 270 DEG C of heat treatment 5min alternately by above-mentioned silicate ability of reverse photochromism material
Diffusing reflection detection, the result is shown in Figure 12 are carried out, Figure 12 is the silicate ability of reverse photochromism material of the preparation of embodiment 11 in ultraviolet light
Diffusing reflection spectrum under irradiation and heat treatment.Show the ability of reverse photochromism that the material generates after ultraviolet light and heat treatment
Phenomenon.
Embodiment 12
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Tm3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, thulium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 13, Figure 13 is friendship of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 12
For the diffusing reflection spectrum under irradiation.Show the ability of reverse photochromism that the material generates after the irradiation of the alternating of ultraviolet light and visible light
Phenomenon.
Embodiment 13
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Eu3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, europium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 14, Figure 14 is friendship of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 13
For the diffusing reflection spectrum under irradiation.Show the ability of reverse photochromism that the material generates after the irradiation of the alternating of ultraviolet light and visible light
Phenomenon.
Embodiment 14
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,Lu3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, luteium oxide are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 15, Figure 15 is friendship of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 14
For the diffusing reflection spectrum under irradiation.Show the ability of reverse photochromism that the material generates after the irradiation of the alternating of ultraviolet light and visible light
Phenomenon.
Embodiment 15
According to chemical expression: Ca1.995ZrSi2O9:0.005Sm3+,La3+Weigh calcium carbonate, silica, zirconium oxide, oxidation
Samarium, lanthana are put into corundum Noah's ark after grinding uniformly, 1000 DEG C are first warming up in Muffle furnace in air atmosphere, heat preservation 6
A hour regrinds after cooled to room temperature, 1400 DEG C is then warming up in tube furnace in air atmosphere, heat preservation 8
A hour, regrinding is fine powder after cooled to room temperature in boiler tube.
Above-mentioned silicate ability of reverse photochromism material is subjected to diffusing reflection inspection under the irradiation of the alternating of ultraviolet light and visible light
It surveys, the result is shown in Figure 16, Figure 16 is friendship of the silicate ability of reverse photochromism material in ultraviolet light and visible light of the preparation of embodiment 15
For the diffusing reflection spectrum under irradiation.Show the ability of reverse photochromism that the material generates after the irradiation of the alternating of ultraviolet light and visible light
Phenomenon.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of silicate ability of reverse photochromism material, chemical formula Ca3-x-yZrSi2O9:xSm3+,yR3+, wherein 0 < x≤0.2,
0≤y≤0.1；R is selected from one or more in Y, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
2. a kind of preparation method of silicate ability of reverse photochromism material as described in claim 1, which is characterized in that including with
Lower step:
A after) calcium source compound, zirconium source compound, silicon source compound, samarium source compound and compound containing R element are mixed
Grinding obtains presoma in air atmosphere by the first calcining；
B) by after presoma grinding, in air atmosphere by the second calcining, it is reversible photic to obtain silicate for regrinding
Off-color material.
3. preparation method according to claim 2, which is characterized in that the calcium source compound is selected from calcium carbonate, calcium oxide
Or calcium nitrate.
4. preparation method according to claim 2, which is characterized in that the zirconium source compound is selected from zirconium oxide or nitric acid
Zirconium.
5. preparation method according to claim 2, which is characterized in that the silicon source compound is selected from silica.
6. preparation method according to claim 2, which is characterized in that the samarium source compound be selected from oxide containing samarium or
Nitrate containing samarium.
7. preparation method according to claim 2, which is characterized in that the compound of the R element is selected from the oxygen containing R element
Compound or nitrate containing R element.
8. preparation method according to claim 2, which is characterized in that the temperature of first calcining is 800~1000 DEG C,
The time of first calcining is 5~6 hours.
9. preparation method according to claim 2, which is characterized in that the temperature of second calcining is 1350~1400
DEG C, the time of second calcining is 8~10 hours.
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