CN108892504A - A kind of blue-green multicomponent light storage ceramic material and preparation method thereof - Google Patents
A kind of blue-green multicomponent light storage ceramic material and preparation method thereof Download PDFInfo
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- CN108892504A CN108892504A CN201810602568.9A CN201810602568A CN108892504A CN 108892504 A CN108892504 A CN 108892504A CN 201810602568 A CN201810602568 A CN 201810602568A CN 108892504 A CN108892504 A CN 108892504A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 29
- 238000003860 storage Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 29
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 29
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 29
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000011656 manganese carbonate Substances 0.000 claims description 6
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 9
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 238000007811 spectroscopic assay Methods 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- 238000010586 diagram Methods 0.000 abstract description 2
- 238000000634 powder X-ray diffraction Methods 0.000 abstract description 2
- 238000003836 solid-state method Methods 0.000 abstract 1
- 230000002688 persistence Effects 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000000904 thermoluminescence Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910021354 zirconium(IV) silicide Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical class [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/671—Chalcogenides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
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Abstract
The invention discloses a kind of blue-green multicomponent light storage ceramic materials and preparation method thereof.The materials chemistry group becomes xMnO (1-0.5x) ZrO2·SiO2(x=0.003 ~ 0.15), using made from traditional high temperature solid-state method.It is characterized by X-ray powder diffraction instrument, the results showed that the XRD spectrum of the light storage ceramic material matches with standard diagram PDF#06-0266.Light storage ceramic material of the present invention can be observed to send out glaucous light after light-illuminating 15 minutes in dark, fluorescent lifetime is up to 8 ~ 12 hours.Excitation-emission spectroscopic assay shows there is emission peak near 486,529,542nm, consistent with observed blue green light.Mn2+And Zr4+For the common centre of luminescence of material, material preparation method is simple, at low cost, chemical property is stable and has excellent luminescent properties, the advanced luminescent material with good application prospect.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, in particular to a kind of blue-green multicomponent light storage ceramic material and
Preparation method.
Background technique
Light storage ceramic material is also known as long after glow luminous material, refers to that material is removing irradiation source（UV, VUV, X-ray, γ
Ray or other ionising radiations）Afterwards, visible light can be launched or near infrared light is up to a kind of material of 20 min or more.Due to length
Afterglow materials can store energy in illumination, can give off energy again after illumination, therefore it is also a kind of energy storage material.
In recent years, long after glow luminous material is widely used in due to its good luminescent properties and its with certain energy-storage function
In military affairs, fire-fighting, industrial agricultural production and daily life.Nowadays, some new luminescent materials include more than fluorescent material and length
Brightness luminescent material and new technology of preparing constantly are disclosed out.Patent of invention CN104073255A discloses a kind of zirconium silicate
Salt blue colour fluorescent powder, preparation method and application, material use Eu3+Adulterate A2ZrSi2O7（Wherein A is alkali metal）Part replaces A
It sets, can be used as fluorescent lamp or high-pressure mercury lamp phosphor, also can be used as photic color fluorescent anti-fake material；Chinese invention patent
CN107129801A discloses a kind of Li+Codope is come the method that improves silicate fluorescent powder long afterglow property, chemistry expression
Formula is Sr2MgSiO7:xEu2+yDy3+zLi+, Li+Doping increase Lacking oxygen, increase captured electronics, thus more than improving
The brightness time；Chinese invention patent CN1560189A discloses a kind of long lad phosphor Ba1-xMxAl2O4:aEu2+bRE3+Preparation
Method, wherein M is alkaline-earth metal Ca2+、Mg2+、Sr2+One of, RE3+For Dy3+、Nd3+One of, Eu2+And RE3+It is sharp
Agent living；Chinese invention patent CN107629789A discloses a kind of ZrO2Base Sm3+-Sn4+The long afterglow of codope, Sm3+-Sn4+Altogether
Adulterate ZrO2Make the Sm of script luminescent properties difference3+Single doping ZrO2Luminescent properties be greatly improved.Above-mentioned long afterglow
Luminescent material is all using rare earth ion or transition metal ions as the centre of luminescence.The oxide of silicon, zirconium of the invention is matrix material
Material, and the oxide for introducing suitable manganese improves the luminescent properties of material, using NaF as mineralizer, can both improve crystalline substance
Body crystallization degree, and material can be made to generate defect to improve the luminescent properties of material.Obtained light storage ceramic material tool
Have the advantages that good luminous performance, chemical property are stable, at low cost.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of blue-green multicomponent light storage ceramic material and
Preparation method.Prepared material, Mn2+And Zr4+For the common centre of luminescence of material, which has good
Chemical stability and thermal stability；Light storage ceramic material of the present invention can be observed to send out after light-illuminating 15 minutes in dark
Glaucous light, fluorescent lifetime are up to 8 ~ 12 hours.Excitation-emission spectroscopic assay shows there is transmitting near 486,529,542nm
Peak, it is consistent with observed blue green light.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of blue-green multicomponent light storage ceramic material, chemical composition are xMnO (1-0.5x) ZrO2·SiO2；Wherein x=
0.003~0.15。
Preparation method includes the following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with xMnO (1-0.5x) ZrO2·
SiO2(x=0.003 ~ 0.15) meter, weighs mineralizer NaF by mole for 30-70%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 600 ~
After the revolving speed of 1000 r/min is ground 2 ~ 4 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, in weak reducing atmosphere（H2With N2By volume 2 ~ 5:98 ~ 95 gas mixed
Body or CO gas）In, it is calcined 3-4 hours at 1100-1300 DEG C, blue-green multicomponent light storage ceramic material xMnO is made
(1-0.5x)ZrO2·SiO2 (x=0.003~0.15)。
The beneficial effects of the present invention are：
1）Material cost prepared by the present invention is lower, property is stable and luminescent properties are good；Pass through X-ray powder diffraction instrument
It is characterized, the results showed that the XRD spectrum of the light storage ceramic material matches with standard diagram PDF#06-0266；By heat
It releases spectrum test two energy level traps of material obtained and is divided into 0.75eV and 0.86eV, illustrate that energy level trap depth compares conjunction
It is suitable, excitation state electronics is preferably stored in particular corresponding to the defect trap energy of the 0.75eV of main peak, the afterglow property tribute to material
It offers bigger.
2）Light storage ceramic material of the present invention can be observed to send out glaucous light, hair after light-illuminating 15 minutes in dark
It is up to 8 ~ 12 hours between light time.Excitation-emission spectroscopic assay shows there is emission peak near 486,529,542nm, and observed
Blue green light is consistent.
Detailed description of the invention
Fig. 1 is 3 gained blue-green long persistence luminescent material 0.05MnO0.975ZrO of embodiment2·SiO2X-ray
Diffraction spectrogram；
Fig. 2 is 3 gained blue-green long persistence luminescent material 0.05MnO0.975ZrO of embodiment2·SiO2Excitation and transmitting
Spectrogram；
Fig. 3 is 3 gained blue-green long persistence luminescent material 0.05MnO0.975ZrO of embodiment2·SiO2Decay of afterglow it is bent
Line；
Fig. 4 is 3 gained blue-green long persistence luminescent material 0.05MnO0.975ZrO of embodiment2·SiO2Thermoluminescence set a song to music
Line.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
A kind of blue-green multicomponent light storage ceramic material, chemical composition 0.003MnO0.9985ZrO2·SiO2。
Preparation method includes the following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with 0.003MnO
0.9985ZrO2·SiO2Meter, weighs mineralizer NaF by 50 mol%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 800
After the revolving speed of r/min is ground 3 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, in weak reducing atmosphere（V(H2):V(N2)=2:98 mixed gas）In, in
It is calcined 3.5 hours at 1200 DEG C, blue-green multicomponent light storage ceramic material 0.003MnO0.9985ZrO is made2·SiO2。
Light storage ceramic material of the present invention can be observed to send out glaucous light after light-illuminating 15 minutes in dark, shine
Time is up to 8 hours.
Embodiment 2
A kind of blue-green multicomponent light storage ceramic material, chemical composition 0.15MnO0.925ZrO2·SiO2。
Preparation method includes the following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with 0.15MnO0.925ZrO2·
SiO2Meter, weighs mineralizer NaF by 30mol%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 1000
After the revolving speed of r/min is ground 2 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, in weak reducing atmosphere（V(H2):V(N2)=5:95 mixed gas）In, in
It is calcined 3 hours at 1300 DEG C, blue-green multicomponent light storage ceramic material 0.15MnO0.925ZrO is made2·SiO2。
Light storage ceramic material of the present invention can be observed to send out glaucous light after light-illuminating 15 minutes in dark, shine
Time is up to 10 hours.
Embodiment 3
A kind of blue-green multicomponent light storage ceramic material, chemical composition 0.05MnO0.975ZrO2·SiO2。
Preparation method includes the following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with 0.05MnO0.975ZrO2·
SiO2Meter, weighs mineralizer NaF by 40mol%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 1000
After the revolving speed of r/min is ground 2 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, in weak reducing atmosphere（V(H2):V(N2)=3:97 mixed gas）In, in
It is calcined 3 hours at 1300 DEG C, blue-green multicomponent light storage ceramic material 0.05MnO0.975ZrO is made2·SiO2。
Light storage ceramic material of the present invention can be observed to send out glaucous light after light-illuminating 15 minutes in dark, shine
Time is up to 12 hours.
Embodiment 4
A kind of blue-green multicomponent light storage ceramic material, chemical composition 0.10MnO0.95ZrO2·SiO2。
Preparation method includes the following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with 0.10MnO0.95ZrO2·
SiO2Meter, weighs mineralizer NaF by 70 mol%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 600r/
After the revolving speed of min is ground 4 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, is to be calcined 4 hours at 1300 DEG C in CO gas in weak reducing atmosphere, is made
Blue-green multicomponent light storage ceramic material 0.10MnO0.95ZrO2·SiO2。
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of blue-green multicomponent light storage ceramic material, it is characterised in that：The materials chemistry group becomes：xMnO·(1-
0.5x)ZrO2·SiO2；Wherein x=0.003 ~ 0.15.
2. a kind of method for preparing blue-green multicomponent light storage ceramic material as described in claim 1, it is characterised in that：Including
Following steps：
1）Raw material ZrOCl is stoichiometrically weighed respectively2·8H2O、SiO2、MnCO3, and with xMnO (1-0.5x) ZrO2·
SiO2Meter, weighs mineralizer NaF according to 30-70mol%；
2）The raw material weighed up are mixed and is placed in ball grinder and is added at dehydrated alcohol to the mid-height of tank, with 600 ~
After the revolving speed of 1000 r/min is ground 2 ~ 4 hours, mixture of raw material is taken out and is transferred in crucible after air-drying；
3）Crucible is placed in batch-type furnace, in weak reducing atmosphere, is calcined 3-4 hours at 1100-1300 DEG C, is made bluish-green
Color multicomponent light storage ceramic material xMnO (1-0.5x) ZrO2·SiO2；Wherein x=0.003 ~ 0.15.
3. the method for preparing blue-green multicomponent light storage ceramic material according to claim 2, it is characterised in that：Step 3）Described
Weak reducing atmosphere is H2With N2By volume 2 ~ 5：98 ~ 95 mixed gases or CO gas.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4767567A (en) * | 1984-04-14 | 1988-08-30 | Degussa Aktiengesellschaft | Process for producing luminous material based on manganese activated zinc silicate |
| CN1810921A (en) * | 2006-02-28 | 2006-08-02 | 华南理工大学 | Red long afterglow luminescent material and its prepn |
| CN104073255A (en) * | 2014-06-30 | 2014-10-01 | 苏州大学 | Zirconium silicate salt blue fluorescent powder, preparation method and application thereof |
| CN105969350A (en) * | 2016-06-03 | 2016-09-28 | 闽南师范大学 | Blue-green long-afterglow luminescent material and preparation method thereof |
| CN107325813A (en) * | 2017-06-21 | 2017-11-07 | 合肥工业大学 | A kind of blue-green fluorescent material and preparation method thereof |
| CN107474838A (en) * | 2017-08-02 | 2017-12-15 | 兰州大学 | A kind of blue-green long persistence luminescent material and preparation method thereof |
-
2018
- 2018-06-12 CN CN201810602568.9A patent/CN108892504B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4767567A (en) * | 1984-04-14 | 1988-08-30 | Degussa Aktiengesellschaft | Process for producing luminous material based on manganese activated zinc silicate |
| CN1810921A (en) * | 2006-02-28 | 2006-08-02 | 华南理工大学 | Red long afterglow luminescent material and its prepn |
| CN104073255A (en) * | 2014-06-30 | 2014-10-01 | 苏州大学 | Zirconium silicate salt blue fluorescent powder, preparation method and application thereof |
| CN105969350A (en) * | 2016-06-03 | 2016-09-28 | 闽南师范大学 | Blue-green long-afterglow luminescent material and preparation method thereof |
| CN107325813A (en) * | 2017-06-21 | 2017-11-07 | 合肥工业大学 | A kind of blue-green fluorescent material and preparation method thereof |
| CN107474838A (en) * | 2017-08-02 | 2017-12-15 | 兰州大学 | A kind of blue-green long persistence luminescent material and preparation method thereof |
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