CN104762081B - A kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material - Google Patents
A kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material Download PDFInfo
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Abstract
Present document relates to a kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, by being mixed into pore creating material in the feed then aged, compressing, the step such as dry, calcine, finally giving macropore Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material, can have important using value as noctilucence carrier material in fields such as noctilucence catalysis, biomarkers, and preparation method is easy to operate, raw material is easy to get, production efficiency high.
Description
Technical field
The present invention relates to a kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, belongs to inorganic non-gold
Category Material Field.
Background technology
Long after glow luminous material abbreviation long-afterglow material, the light-storing and emitting material that is otherwise known as, Noctilucent material, which is substantially
It is a kind of embedded photoluminescent material, he is that a class absorbs the energy stores of extraneous light radiation in it can fall into, such as visible ray, ultraviolet light,
The irradiation of X-ray etc., is then lentamente discharged these energy at normal temperatures in the form of visible ray, and is exciting stopping
May continue to afterwards send the material of light, people typically excite stop after continuous illumination more than 1 hour be called long afterglow.
Porous ceramics be a kind of there is the ceramic material for communicating with each other or closing pore in a large number through artificial synthesized, internal,
Pore structure with certain size and quantity, usual porosity are larger, and pore structure is present as useful structure.Porous is made pottery
The species of porcelain is various, and various ceramic materials can prepare porous ceramics by appropriate technique, draw by aggregate material
It is divided into：Aluminosilicate material, diatomaceous material, corundum and Buddha's warrior attendant sand material etc.；It is divided into by the big I of aperture size：Micro-
Hole pottery (aperture<2nm), mesoporous pottery (2nm<Aperture<50nm), macropore pottery (aperture>50nm).
But, the research of porous long-afterglow material but seldom has been reported that.Porous long-afterglow material can not only play porous
Density of material is little, porosity is high, specific surface area is big, the permeability to gas and selective penetrated property preferable the advantages of, also have length
The unique energy storage luminescent properties of afterglowing material.Yang Xuefeng etc. is with Determination of Polyoxyethylene Non-ionic Surfactants（PEO）Close for template
Mesoporous SrAl is become2O4：Eu, Dy long-afterglow material, but the method complex process, cycle are long, and the difficulty of synthesis becomes than larger
Power is relatively low.Lu Qingshan is prepared using mesoporous material SBA-15 as inorganic reaction thing by high-temperature solid phase reaction method
Zn2SiO4：Mn2+And Y2SiO5：Eu3+Material, but all avalanches of bi-material duct, do not have mesoscopic structure.
The present invention is different from above-mentioned report, it is proposed that one kind prepares macropore Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material
New technology, macropore Sr according to the present invention2MgSi2O7：Eu2+,Dy3+The size of long-afterglow material is 100 ~ 300nm, this kind of material
And preparation method is showed no open report, and the features such as this preparation method is easy to operate, raw material is easy to get, production efficiency is high.Greatly
Hole Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material can have in fields such as noctilucence catalysis, biomarkers as noctilucence carrier material
There is important using value.
Content of the invention
A kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, concrete content of the invention are as follows：
1st, according to mol ratio SrO：MgO：SiO2：B2O3：Eu2O3：Dy2O3= 2：1：2：0.05~0.15：0.001~0.01：
0.01 ~ 0.1 carries out weighing, dispensing, be mixed after obtain compound A, be subsequently adding pore creating material, after being mixed, obtain compound B, add
Binding agent is mixed to form compound C；By compound C good seal, 12-24h is aged, will be compressing for the compound B after ageing；Pressure
Piece dries 5 ~ 6h at 70 ~ 80 DEG C, is then calcined, obtains macropore Sr after sample along with the furnace cooling2MgSi2O7：Eu2+,Dy3+Long
Afterglowing material.
2nd, the operation that is mixed of compound A, B can be mixed using ceramic mortar underhand polish, 1 ~ 2h of milling time or employing
Dry ball milling is mixed, and ball-milling medium adopts rigid silica ball, material：Mass ratio=1 of ball：3 ~ 4, Ball-milling Time is 1 ~ 2h；Mixed
Close material C to be mixed using mechanical agitation, be mixed 15 ~ 30min of time.
3rd, the initial particle size of all solid feeds and pore creating material is respectively less than 200 mesh.
4th, pore creating material adopt ammonium carbonate, ammonium oxalate, ammonium nitrate one kind therein, addition account for compound A mass 10 ~
50wt%.
5th, binding agent for volume fraction 4vol% methylated cellulose aqueous solution, addition account for compound B mass 10 ~
15wt%.
6th, compressing pressure is 5 ~ 12Mpa, and the dwell time is 30s.
7th, obtained by molding compressing tablet be 1 ~ 5cm of diameter, the disk of 0.2 ~ 0.5cm of thickness or grow 5 ~ 15cm, wide 1 ~ 2cm, high 1 ~ 2cm
Rectangular sheet.
8th, calcinating system：Room temperature ~ 650 DEG C, heating rate are 3 DEG C/min, 650 DEG C of insulation 1h；650 ~ 1000 DEG C, heat up
Speed is 3 DEG C/min；1000 DEG C ~ highest calcining heat, heating rate are 2 DEG C/min, and highest calcining heat is 1200 ~ 1350 DEG C
Between arbitrary temp, highest calcining heat be incubated 1 ~ 2h；It is passed through hydrogen and reducing atmosphere is kept, hydrogen flowing quantity is controlled to 1 ~ 2L/
min.
Description of the drawings
Fig. 1 is the macropore Sr prepared by 1 technique of embodiment2MgSi2O7：Eu2+,Dy3+The XRD of long-afterglow material.
Fig. 2 is the macropore Sr prepared by 1 technique of embodiment2MgSi2O7：Eu2+,Dy3+The SEM figure of long-afterglow material.
Fig. 3 is the macropore Sr prepared by 1 technique of embodiment2MgSi2O7：Eu2+,Dy3+The fluorescent emission of long-afterglow material
Figure.
Fig. 4 is the macropore Sr prepared by 1 technique of embodiment2MgSi2O7：Eu2+,Dy3+The decay of afterglow of long-afterglow material is bent
Line chart.
Specific embodiment
The present invention is described in detail with reference to embodiments, and the present invention is not limited by these manufacture examples.
Example 1
According to mol ratio SrO：MgO：SiO2：B2O3：Eu2O3：Dy2O3= 2：1：2：0.1：0.005：0.05 carry out weighing,
Compound A is obtained after dispensing, ceramic mortar grinding batch mixing 1h, the ammonium carbonate of 20wt% of compound A mass is subsequently adding as making
Hole agent, obtains compound B after ceramic mortar grinding batch mixing 1h, and the volume fraction for adding the 11wt% of compound B mass is 4vol%
Methylated cellulose aqueous solution as binding agent, stir mixing 20min forms compound C；By compound C good seal, it is aged
24h, the compound C after ageing is pressed into diameter 2cm, the disk of thick 0.3cm, and compressing pressure is 12Mpa, during pressurize
Between be 30s；Compressing tablet dries 5h at 75 DEG C, is then calcined, and obtains macropore Sr after sample along with the furnace cooling2MgSi2O7：Eu2+,
Dy3+Long-afterglow material.The initial particle size of all solid feeds and pore creating material is respectively less than 200 mesh as mentioned above；Calcine as mentioned above
System is：Room temperature ~ 650 DEG C, heating rate are 3 DEG C/min, 650 DEG C of insulation 1h；650 ~ 1000 DEG C, heating rate be 3 DEG C/
min；1000 DEG C ~ 1200 DEG C, heating rate is 2 DEG C/min, 1200 DEG C of insulation 2h；It is passed through hydrogen and keeps reducing atmosphere, hydrogen stream
Amount is controlled to 2L/min.
Example 2
According to mol ratio SrO：MgO：SiO2：B2O3：Eu2O3：Dy2O3= 2：1：2：0.06：0.008：0.07 carry out weighing,
Compound A is obtained after the dry-mixed 1h of dispensing, ball milling, the starch of 30wt% of compound A mass is subsequently adding as pore creating material, ball milling
Compound B is obtained after dry-mixed 1h, and the volume fraction for adding the 13wt% of compound B mass is the methylated cellulose aqueous solution of 4vol%
Used as binding agent, stir mixing 30min forms compound C；By compound C good seal, 24h is aged, by the compound C after ageing
Diameter 2cm is pressed into, the disk of thick 0.3cm, compressing pressure are 12Mpa, the dwell time is 30s；Compressing tablet is at 75 DEG C
5h is dry, is then calcined, after sample along with the furnace cooling, obtain macropore Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material.As above institute
The initial particle size for stating all solid feeds and pore creating material is respectively less than 200 mesh；Calcinating system is as mentioned above：Room temperature ~ 650 DEG C, rise
Warm speed is 3 DEG C/min, 650 DEG C of insulation 1h；650 ~ 1000 DEG C, heating rate is 3 DEG C/min；1000 DEG C ~ 1250 DEG C, heat up
Speed is 2 DEG C/min, 1250 DEG C of insulation 2h,；It is passed through hydrogen and reducing atmosphere is kept, hydrogen flowing quantity is controlled to 2L/min.
Example 3
According to mol ratio SrO：MgO：SiO2：B2O3：Eu2O3：Dy2O3= 2：1：2：0.06：0.01：0.05 carry out weighing,
Compound A is obtained after the dry-mixed 2h of dispensing, ball milling, 40wt% pore creating material ammonium oxalate, the ball milling for being subsequently adding compound A mass is dry-mixed
Compound B is obtained after 2h, and the volume fraction for adding the 13wt% of compound B mass is the methylated cellulose aqueous solution conduct of 4vol%
Binding agent, stir mixing 30min form compound C；By compound C good seal, 24h is aged, the compound C after ageing is suppressed
Growth 5cm, wide 1cm, the rectangular sheet of high 1cm, compressing pressure are 12Mpa, and the dwell time is 30s；Compressing tablet is at 75 DEG C
5h is dry, is then calcined, after sample along with the furnace cooling, obtain macropore Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material.As above institute
The initial particle size for stating all solid feeds and pore creating material is respectively less than 200 mesh；Calcinating system is as mentioned above：Room temperature ~ 650 DEG C, rise
Warm speed is 3 DEG C/min, 650 DEG C of insulation 1h；650 ~ 1000 DEG C, heating rate is 3 DEG C/min；1000 DEG C ~ 1300 DEG C, heat up
Speed is 2 DEG C/min, 1300 DEG C of insulation 1h；It is passed through hydrogen and reducing atmosphere is kept, hydrogen flowing quantity is controlled to 2L/min.
Claims (5)
1. a kind of macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, it is characterised in that：According to mol ratio SrO：
MgO：SiO2：B2O3：Eu2O3：Dy2O3= 2：1：2：0.05~0.15：0.001~0.01：0.01 ~ 0.1 carries out weighing, dispensing, mixed
Compound A is obtained afterwards all, be subsequently adding pore creating material, obtain compound B after being mixed, add binding agent to be mixed to form compound C；Will
Compound C good seal, is aged 12-24h, compressing for the compound B after ageing, compressing pressure is 5 ~ 12Mpa, is protected
The pressure time be 30s, obtained by molding compressing tablet be 1 ~ 5cm of diameter, the disk of 0.2 ~ 0.5cm of thickness or grow 5 ~ 15cm, wide 1 ~ 2cm, high by 1 ~
The rectangular sheet of 2cm；Compressing tablet dries 5 ~ 6h at 70 ~ 80 DEG C, is then calcined, obtains macropore after sample along with the furnace cooling
Sr2MgSi2O7：Eu2+,Dy3+Long-afterglow material；The operation that is mixed of compound A, B can be mixed using ceramic mortar underhand polish,
1 ~ 2h of milling time is mixed using dry ball milling, and ball-milling medium adopts rigid silica ball, material：Mass ratio=1 of ball：3~
4, Ball-milling Time is 1 ~ 2h；Compound C is mixed using mechanical agitation, and be mixed 15 ~ 30min of time.
2. a kind of as claimed in claim 1, macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, its feature exist
In：The initial particle size of all solid feeds and pore creating material is respectively less than 200 mesh.
3. a kind of as claimed in claim 1, macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, its feature exist
In：Pore creating material adopts ammonium carbonate, ammonium oxalate, ammonium nitrate one kind therein, and addition accounts for 10 ~ 50wt% of compound A mass.
4. a kind of as claimed in claim 1, macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, its feature exist
In：Binding agent accounts for 10 ~ 15wt% of compound B mass for the methylated cellulose aqueous solution of 4 vol% of volume fraction, addition.
5. a kind of as claimed in claim 1, macropore Sr2MgSi2O7：Eu2+,Dy3+The preparation method of long-afterglow material, its feature exist
In：Calcinating system：Room temperature ~ 650 DEG C, heating rate are 3 DEG C/min, 650 DEG C of insulation 1h；650 ~ 1000 DEG C, heating rate is 3
℃/min；1000 DEG C ~ highest calcining heat, heating rate are 2 DEG C/min, and highest calcining heat is appointing between 1200 ~ 1350 DEG C
Meaning temperature, highest calcining heat are incubated 1 ~ 2h；It is passed through hydrogen and reducing atmosphere is kept, hydrogen flowing quantity is controlled to 1 ~ 2L/min.
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