CN107523297A - Upper conversion emitting red light powder and preparation method thereof - Google Patents
Upper conversion emitting red light powder and preparation method thereof Download PDFInfo
- Publication number
- CN107523297A CN107523297A CN201710842612.9A CN201710842612A CN107523297A CN 107523297 A CN107523297 A CN 107523297A CN 201710842612 A CN201710842612 A CN 201710842612A CN 107523297 A CN107523297 A CN 107523297A
- Authority
- CN
- China
- Prior art keywords
- red light
- emitting red
- light powder
- solution
- upper conversion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7768—Chalcogenides with alkaline earth metals
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to emitting red light powder and preparation method thereof is changed in one kind.The specific chemical formula of this upconversion luminescent powder is ZrCa0.06YbyErzO2.06+1.5(y+z)。Adulterated by calcium ion, obtain presoma, and presoma is obtained through 1100 DEG C of high-temperature calcinations and ball-milling treatment and changes emitting red light powder on the rear-earth-doped oxidation zirconium of stable Tetragonal using liquid-phase coprecipitation.The luminescent powder has luminosity high, and particle diameter is small, the characteristics of chemistry and good mechanical stability, has huge practical value in infrared anti-false field, also has potential application value in terms of upper converting biological fluorescence labeling.
Description
Technical field
The present invention relates to a kind of infrared up-conversion luminous material and preparation method thereof, is related specifically to a kind of red in 980nm
Outer light, which excites down, can send upper conversion emitting red light powder of bright visible feux rouges and preparation method thereof.
Background technology
Luminous infrared up conversion is that a kind of anti-Stokes light that short-wavelength light is produced under the exciting of infrared light was launched
Journey.Due to having larger frequency displacement between transmitting light wave and excitation light wave, up-conversion luminescent material can apply to biological fluorescent labelling,
False proof, short wavelength's all solid state laser, optical-fibre communications, infrared acquisition, illumination and polychrome 3 D stereo such as show at the field.
The rear-earth-doped up-conversion luminescent material of efficient stable is prepared, key is to select suitable up-conversion luminescence matrix
Material, at present the up-conversion luminescence host material of most study can be divided into fluoride, sulfide, oxide and oxyfluoride
Deng.For oxide-base material, fluorine-containing and sulfur-containing compound preparation process is complex, and cost is higher, and
The two heat endurance and chemical stability are also relatively low compared with oxide, therefore some oxides can be as the reason of up-conversion luminescence
Think host material.
It is mostly rare earth oxide using oxide as the material of up-conversion luminescence matrix, including Y2O3, Lu2O3, Gd2O3.With
ZrO2Also had been reported for the up-conversion of matrix, relative to the rare earth oxide matrix of raw material costly, with ZrO2As upper
Conversion luminous host material feedstock cost is less expensive, and chemical stability is also preferable, therefore ZrO2It is a kind of even more ideal upper conversion
Host material.
ZrO2Phonon cut-off frequency be 470cm-1, the inelastic scattering effect to excitation state electronics is relatively low, is advantageous to light
The up-conversion luminescence of son.ZrO2As up-conversion luminescence host material, in up-conversion luminescence field also by numerous studies.Generally,
In order to ensure rare earth ion is completely into zirconia crystal lattice, crystal defect is reduced, it is necessary to which high-temperature calcination processing is carried out to sample.It is pure
Following reversible transition in high-temperature burning process be present in zirconium oxide,
Occur a part of tetragonal phase zirconium oxide to monocline phase in version in temperature-fall period.The problem of maximum is, this phase transformation
Process can cause the volumetric expansion of material generation 5%, and this phase transition process inevitably causes part ion coordination mode to change
Become, cause material up-conversion luminescence performance substantially to reduce, final using effect is had undesirable effect.
In order to ensure that zirconium oxide has higher up-conversion luminescence performance, good using effect is obtained, first has to solve
Technical problem be exactly：Up-conversion luminescent material using pure zirconia as matrix causes because matrix thing is not mutually single, unstable
Luminescent properties reduce and mechanical performance reduces.
The content of the invention
Luminescent properties are caused because matrix thing phase is not single for the up-conversion luminescent material using pure zirconia as matrix
The problem of unstable, the technical scheme of solution above-mentioned technical problem of the present invention are：Emitting red light powder is changed in one kind,
Characterized in that, emitting red light powder is changed on this as emitting red light powder, its chemical formula is changed on rear-earth-doped calcia-stabilised zirconia
For：ZrCa0.06YbyErzO2.06+1.5(y+z)。
Technical characteristic of the invention further is；
The upper host material for changing emitting red light powder is calcia-stabilised zirconia powder.
Its luminescent activator ion is Er3+。
0.05≤y≤0.075, 0.01≤z≤0.015。
Its luminous sensitizing agent ion is Yb3+。
Such a luminescent powder be using concentrated ammonia liquor as precipitating reagent obtain presoma, and by presoma by 1100 DEG C calcining 2h and
Ball-milling treatment and obtain.
It is ZrCa the invention also discloses emitting red light powder is changed on rear-earth-doped calcia-stabilised zirconia0.06YbyErzO2.06+1.5(y+z)
Preparation method, it comprises the following steps：
A) by rare earth oxide Er2O3、Yb2O3, respectively with concentrated nitric acid according to 1:7 mixed in molar ratio is simultaneously diluted with water, through 70~
Er (the NO that concentration is 0.01mol/L are prepared in 80 DEG C of water-bath dissolvings3)3Solution, and 0.2mol/L Yb (NO3)3The aqueous solution；
B) according to material ZrCa0.06YbyErzO2.06+1.5(y+z)In the relative amount of each component converse zirconyl nitrate, four water
Required quality and the step a) for closing calcium nitrate prepares the Er (NO that concentration is 0.01mol/L3)3And concentration is 0.2mol/L's
Yb(NO3)3Institute's expense of rare earth nitrate solution；Weigh 0.01mol（That is 2.33g）Zirconyl nitrate in beaker, according still further to
Zr:Ca:Yb:Er=1:0.06:y:Z mol ratio measures 0.01ymol Yb (NO respectively3)3The Er of solution and 0.01zmol
(NO3)3It is added in beaker, the calcium nitrate tetrahydrate for finally weighing 0.0006mol adds beaker, and 50mL is added into beaker
Deionized water, quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, makes Zr4+Ion concentration is 0.2mol/L；
C) under stirring, concentrated ammonia liquor is poured slowly into b) step resulting solution, stops adding when solution ph reaches 9~10
Enter ammoniacal liquor, and continue 10~20min of stirring；
D) Anhydrous potassium carbonate for weighing 0.0006mol is dissolved completely in 15mL deionized waters, and pours into the white of c) step acquisition
In color solution, continue 3~4h of stirring；
E) stop that products therefrom is carried out into filtering and washing after stirring, suction filtration process is washed with deionized 3~4 times first, then uses
Absolute ethyl alcohol be washed once, and filter cake finally is placed in into 120 DEG C of constant temperature blast drying oven drying.
F) the predecessor block that e) step is dried is fitted into alumina crucible, is put into Muffle furnace and calcines, heating rate
For 5K/min, calcining heat is 1100 DEG C, calcination time 2h, and room temperature is naturally cooled to stove after calcining stopping；
G) by the sample after calcining and zirconium oxide ball milling pearl according to 1：4 mass ratio mixing, adds deionized water wetting, with
600rad/min rotating speed continuous ball milling 1h in planetary ball mill, ball milling isolate abrading-ball and in constant temperature forced air dryings after terminating
Case, which is dried, can obtain conversion emitting red light powder powder on rear-earth-doped calcia-stabilised zirconia.
Wherein：0.05≤y≤0.075, 0.01≤z≤0.015.
The beneficial effects of the invention are as follows：
The present invention passes through Ca2+Ion pair rare earth ion Yb3+,Er3+The zirconium oxide of codope is stablized, and ensure that zirconium oxide
With single stable thing phase.The luminescent properties that emitting red light powder is changed on zirconium oxide after calcium stable are significantly improved.And
And the present invention has prepared single Tetragonal using the method for liquid phase coprecipitation, high-temperature calcination and ball milling and stable rare earth is mixed
Emitting red light powder is changed on miscellaneous calcia-stabilised zirconia, this luminescent powder has preparation process simple, and cost is lower, product luminance
The characteristics of degree is high, chemical property and good mechanical stability, and particle size is small, there is huge practical value in anti-counterfeit field,
Also there is potential using value in biological fluorescent labelling field.
Embodiment
Emitting red light powder is changed on the rear-earth-doped calcia-stabilised zirconia of the present invention, its chemical formula is：
ZrCa0.06YbyErzO2.06+1.5(y+z), 0.05≤y≤0.075,0.01≤z≤0.015,
Glow, be that emitting red light powder is changed on rear-earth-doped calcia-stabilised zirconia, its chemical formula is：
ZrCa0.06YbyErzO2.06+1.5(y+z)。
With reference to specific embodiment, the invention will be further described；
Embodiment one
ZrCa0.06Yb0.075Er0.015O2.195 Upper conversion emitting red light powder CSR (6)-I, preparation method comprise the following steps:
A) 7.88g Yb are weighed respectively2O3, 0.382g Er2O3It is added separately in the beaker that two capacity are 200mL, and point
Not Jia Ru 50mL deionized waters, according to Er2O3、Yb2O3, it is 1 with concentrated nitric acid mol ratio:7 measure concentrated nitric acid respectively is added to beaker
In with corresponding Er2O3、Yb2O3Mix, while with 70~80 DEG C of progress water-baths.Treat that above two rare earth oxide is complete
Being dissolved in dust technology turns into corresponding Yb (NO3)3Solution and Er (NO3)3Solution, deionized water is separately added into two kinds of solution
Each overall solution volume is set to be changed into 200mL, now Yb (NO3)3Molar concentration is 0.2mol/L, Er (NO3)3Concentration is
0.01mol/L。
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, 0.2mol/L Yb (NO are measured respectively3)3Solution 3.75
ML, 0.01mol/L Er (NO3)3Solution 15.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O is in beaker
In, liquid make-up cumulative volume is 50mL, and quickly stirring makes solution be changed into clarifying completely by magnetic stirring apparatus, now Zr4+It is dense
Spend for 0.2mol/L.
C) under stirring, concentrated ammonia liquor is poured slowly into b) step resulting solution, stopped when solution ph reaches 9
Ammoniacal liquor is added, now White Flocculus has occurred in solution, continues stirring 10~20 minutes.
D) solution that continuation agitating solution c) steps obtain weighs 0.0828g Anhydrous potassium carbonates and is dissolved in 15mL after 10 minutes
Deionized water, this solution of potassium carbonate is poured into, and continue 3~4h of stirring.
E) stopping that products therefrom is carried out into filtering and washing after stirring, suction filtration process is washed with deionized 3~4 times first,
It washed once again with absolute ethyl alcohol, filter cake be finally placed in 120 DEG C of constant temperature blast drying oven drying.
F) the predecessor block of drying is fitted into alumina crucible, is put into Muffle furnace and calcines, heating rate 5K/
Min, calcining heat are 1100 DEG C, calcination time 2h, are calcined after terminating with stove natural cooling.
G) by the sample after calcining and zirconium oxide ball milling pearl according to 1：4 mass ratio mixing, and deionized water wetting is added,
Ball milling 1h is continued in planetary ball mill with 600rad/min rotating speed, ball milling is isolated abrading-ball and done in constant temperature air blast after terminating
Dry case, which is dried, can obtain ZrCa0.06Yb0.075Er0.015O2.195 Upper conversion emitting red light powder CSR (6)-I.
At room temperature, 980nm laser excitation of the powder through 50mW can produce the visible bright feux rouges of naked eyes under light field.
Embodiment two
ZrCa0.06Yb0.075Er0.01O2.1875 Upper conversion emitting red light powder CSR (6)-II, preparation method comprise the following steps:
A) 7.88g Yb are weighed respectively2O3, 0.382g Er2O3It is added separately in the beaker that two capacity are 200mL, and point
Not Jia Ru 50mL deionized waters, according to Er2O3、Yb2O3, it is 1 with concentrated nitric acid mol ratio:7 measure concentrated nitric acid respectively is added to beaker
In with corresponding Er2O3、Yb2O3Mix, while with 70~80 DEG C of progress water-baths.Treat that above two rare earth oxide is complete
Being dissolved in dust technology turns into corresponding Yb (NO3)3Solution and Er (NO3)3Solution, deionized water is separately added into two kinds of solution
Each overall solution volume is set to be changed into 200mL, now Yb (NO3)3Molar concentration is 0.2mol/L, Er (NO3)3Concentration is
0.01mol/L。
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3It is molten
Liquid 3.75mL, 0.01mol/L Er (NO3)3Solution 10.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O
In beaker, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now
Zr4+Concentration is 0.2mol/L.
C) under stirring, concentrated ammonia liquor is poured slowly into b) step resulting solution, stopped when solution ph reaches 10
Ammoniacal liquor is added, now White Flocculus has occurred in solution, continues stirring 10~20 minutes.
D) solution that continuation agitating solution c) steps obtain weighs 0.0828g Anhydrous potassium carbonates and is dissolved in 15mL after 10 minutes
Deionized water, this solution of potassium carbonate is poured into, and continue 3~4h of stirring.
E) stopping that products therefrom is carried out into filtering and washing after stirring, suction filtration process is washed with deionized 3~4 times first,
It washed once again with absolute ethyl alcohol, filter cake be finally placed in 120 DEG C of constant temperature blast drying oven drying.
F) the predecessor block of drying is fitted into alumina crucible, is put into Muffle furnace and calcines, heating rate 5K/
Min, calcining heat are 1100 DEG C, calcination time 2h, are calcined after terminating with stove natural cooling.
G) by the sample after calcining and zirconium oxide ball milling pearl according to 1：4 mass ratio mixing, and deionized water wetting is added,
Ball milling 1h is continued in planetary ball mill with 600rad/min rotating speed, ball milling is isolated abrading-ball and done in constant temperature air blast after terminating
Dry case, which is dried, can obtain ZrCa0.06Yb0.075Er0.01O2.1875 Upper conversion emitting red light powder CSR (6)-II.
At room temperature, 980nm laser excitation of the powder through 50mW can produce the visible bright feux rouges of naked eyes under light field.
Embodiment three
ZrCa0.06Yb0.075Er0.012O2.1905Upper conversion emitting red light powder CSR (6)-III preparation method comprises the following steps:
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3Solution
3.75mL, 0.01mol/L Er (NO3)3Solution 10.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O in
In beaker, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now Zr4+
Concentration is 0.2mol/L.
Other steps and above-described embodiment two are identical, you can obtain ZrCa0.06Yb0.075Er0.012O2.1905Upper conversion emitting red light
Powder CSR (6)-III.At room temperature, the 980nm laser excitations through 50mW, the powder can produce macroscopic bright fresh under light field
Gorgeous feux rouges.
Example IV
ZrCa0.06Yb0.06Er0.01O2.165Upper conversion emitting red light powder CSR (6)-IV preparation method comprises the following steps:
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3Solution
3.0mL, 0.01mol/L Er (NO3)3Solution 10.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O is in burning
In cup, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now Zr4+It is dense
Spend for 0.2mol/L.
Other steps and above-described embodiment two are identical, you can obtain ZrCa0.06Yb0.06Er0.01O2.165Upper conversion emitting red light powder
CSR(6)-Ⅳ.At room temperature, the 980nm laser excitations through 50mW, the powder can produce macroscopic bright bright-coloured under light field
Feux rouges.
Embodiment five
ZrCa0.06Yb0.06Er0.015O2.1725Upper conversion emitting red light powder CSR (6)-V preparation method comprises the following steps:
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3Solution
3.0mL, 0.01mol/L Er (NO3)3Solution 15.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O is in burning
In cup, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now Zr4+It is dense
Spend for 0.2mol/L.
Other steps and above-described embodiment two are identical, you can obtain ZrCa0.06Yb0.06Er0.015O2.1725Upper conversion emitting red light
Powder CSR (6)-V.
At room temperature, the 980nm laser excitations through 50mW, the powder can produce macroscopic bright bright-coloured under light field
Feux rouges.
Embodiment six
ZrCa0.06Yb0.05Er0.01O2.15Upper conversion emitting red light powder CSR (6)-VI preparation method comprises the following steps:
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3Solution
2.5mL, 0.01mol/L Er (NO3)3Solution 10.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O is in burning
In cup, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now Zr4+It is dense
Spend for 0.2mol/L.
Other steps and above-described embodiment two are identical, you can obtain ZrCa0.06Yb0.05Er0.01O2.15Upper conversion emitting red light powder
CSR(6)-Ⅵ。
At room temperature, the 980nm laser excitations through 50mW, the powder can produce macroscopic bright bright-coloured under light field
Feux rouges.
Embodiment seven
ZrCa0.06Yb0.05Er0.015O2.1575Upper conversion emitting red light powder CSR (6)-VII preparation method comprises the following steps:
B) 2.33g ZrO (NO are weighed3)2In 100mL beakers, the Yb (NO of 0.2mol/L concentration are measured respectively3)3Solution
2.5mL, 0.01mol/L Er (NO3)3Solution 15.0mL is added in beaker, then weighs 0.1416g Ca (NO3)2•4H2O is in burning
In cup, liquid make-up cumulative volume is 50mL, and quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, now Zr4+It is dense
Spend for 0.2mol/L.
Other steps and above-described embodiment two are identical, you can obtain ZrCa0.06Yb0.05Er0.015O2.1575Upper conversion emitting red light
Powder CSR (6)-VII.
At room temperature, the 980nm laser excitations through 50mW, the powder can produce macroscopic bright bright-coloured under light field
Feux rouges.
In addition, by extracting the upper conversion emitting red light powder ZrCa in above-described embodiment0.06Yb0.075Er0.015O2.195Do XRD spectrums
Map analysis, find can determine to be single Tetragonal by the change of XDR diffraction peaks, this is also at room temperature through 50mW's
980nm laser excitations, the powder can produce the immediate cause of macroscopic bright bright-coloured feux rouges under light field.
The present invention passes through Ca2+Ion pair rare earth ion Yb3+,Er3+Or Yb3+,Ho3+The zirconium oxide of codope is stablized, and protects
Having demonstrate,proved zirconium oxide has single stable thing phase.The luminescent properties acquisition that emitting red light powder is changed on zirconium oxide after calcium stable is bright
It is aobvious to improve.And the present invention has prepared single Tetragonal and steady using the method for liquid phase coprecipitation, high-temperature calcination and ball milling
Emitting red light powder is changed on fixed rear-earth-doped calcia-stabilised zirconia, this luminescent powder has preparation process simple, and cost is lower,
The characteristics of product luminosity is high, and chemical stability is good, and particle size is small, there is huge practical value in anti-counterfeit field,
Also there is potential using value in biological fluorescent labelling field.
It the above is only the description to specific embodiment, the ratio provided in embodiment and percentage are all Doped ions and zirconium
The relative molar proportions and Relative mole percentage that ion feeds intake.Technology contents and technical characterstic have revealed that as above, but can be with
Understand, under the creative ideas of the present invention, those skilled in the art can make various changes and improve to above-mentioned preparation method,
Protection scope of the present invention is defined by claims.
Claims (8)
1. emitting red light powder is changed in one kind, it is characterised in that：Emitting red light powder is changed on this to aoxidize into rear-earth-doped calcium stable
Emitting red light powder is changed on zirconium, its chemical formula is：ZrCa0.06YbyErzO2.06+1.5(y+z)。
2. upper conversion emitting red light powder according to claim 1, it is characterised in that：The base of the upper conversion emitting red light powder
Material is calcia-stabilised zirconia powder.
3. upper conversion emitting red light powder according to claim 1, it is characterised in that：Its luminescent activator ion is Er3+。
4. the upper conversion emitting red light powder according to claims 1, it is characterised in that 0.05≤y≤0.075,0.01
≤z≤0.015。
5. upper conversion emitting red light powder according to claim 1, it is characterised in that：Its luminous sensitizing agent ion is Yb3+。
6. upper conversion emitting red light powder according to claim 1, it is characterised in that：It using concentrated ammonia liquor is heavy that such a luminescent powder, which is,
Shallow lake agent obtains presoma, and presoma is obtained by 1100 DEG C of calcining 2h and ball-milling treatment.
7. the preparation method of upper conversion emitting red light powder according to claim 1, it is characterised in that prepare step including following
Suddenly：
A) by rare earth oxide Er2O3、Yb2O3, respectively with concentrated nitric acid according to 1:7 mixed in molar ratio is simultaneously diluted with water, through 70~
Er (the NO that concentration is 0.01mol/L are prepared in 80 DEG C of water-bath dissolvings3)3Solution, and 0.2mol/L Yb (NO3)3The aqueous solution；
B) according to material ZrCa0.06YbyErzO2.06+1.5(y+z)In the relative amount of each component converse zirconyl nitrate, four water
Required quality and the step a) for closing calcium nitrate prepares the Er (NO that concentration is 0.01mol/L3)3And concentration is 0.2mol/L's
Yb(NO3)3Institute's expense of rare earth nitrate solution；Weigh 0.01mol（That is 2.33g）Zirconyl nitrate in beaker, according still further to
Zr:Ca:Yb:Er=1:0.06:y:Z mol ratio measures 0.01ymol Yb (NO respectively3)3The Er of solution and 0.01zmol
(NO3)3It is added in beaker, the calcium nitrate tetrahydrate for finally weighing 0.0006mol adds beaker, and 50mL is added into beaker
Deionized water, quickly being stirred by magnetic stirring apparatus makes solution be changed into clarifying completely, makes Zr4+Ion concentration is 0.2mol/L；
C) under stirring, concentrated ammonia liquor is poured slowly into b) step resulting solution, stopped when solution ph reaches 9~10
Ammoniacal liquor is added, and continues 10~20min of stirring；
D) Anhydrous potassium carbonate for weighing 0.0006mol is dissolved completely in 15mL deionized waters, and pours into the white of c) step acquisition
In color solution, continue 3~4h of stirring；
E) stop that products therefrom is carried out into filtering and washing after stirring, suction filtration process is washed with deionized 3~4 times first, then uses
Absolute ethyl alcohol be washed once, and filter cake finally is placed in into 120 DEG C of constant temperature blast drying oven drying；
F) the predecessor block that e) step is dried is fitted into alumina crucible, is put into Muffle furnace and calcines, heating rate is
5K/min, calcining heat are 1100 DEG C, calcination time 2h, and room temperature is naturally cooled to stove after calcining stopping；
G) by the sample after calcining and zirconium oxide ball milling pearl according to 1：4 mass ratio mixing, adds deionized water wetting, with
600rad/min rotating speed continuous ball milling 1h in planetary ball mill, ball milling isolate abrading-ball and in constant temperature forced air dryings after terminating
Case, which is dried, can must go up conversion emitting red light powder powder.
8. the preparation method of upper conversion emitting red light powder according to claim 7, it is characterised in that： 0.05≤y≤
0.075, 0.01≤z≤0.015。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710842612.9A CN107523297A (en) | 2017-09-18 | 2017-09-18 | Upper conversion emitting red light powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710842612.9A CN107523297A (en) | 2017-09-18 | 2017-09-18 | Upper conversion emitting red light powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107523297A true CN107523297A (en) | 2017-12-29 |
Family
ID=60736809
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710842612.9A Pending CN107523297A (en) | 2017-09-18 | 2017-09-18 | Upper conversion emitting red light powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107523297A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185975A (en) * | 2021-05-14 | 2021-07-30 | 中国科学院长春光学精密机械与物理研究所 | Oxide up-conversion luminescent material and preparation method thereof |
-
2017
- 2017-09-18 CN CN201710842612.9A patent/CN107523297A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 刘建本 等: "化学共沉淀法制备四方相ZrO2-CaO纳米粉", 《粉末冶金材料科学与工程》 * |
| 曹力力: "铈稳定氧化锆上转换材料的制备及其发光性能研究", 《中国优秀博硕士学文论文全文数据库（硕士）工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113185975A (en) * | 2021-05-14 | 2021-07-30 | 中国科学院长春光学精密机械与物理研究所 | Oxide up-conversion luminescent material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Montoya et al. | Synthesis and characterization of praseodymium-containing ZrSiO4 solid solutions from gels | |
| Kang et al. | A novel blue-light excitable Pr3+ doped (Sr, Ba) LaMgTaO6 phosphor for plant growth lighting | |
| Liu et al. | Eu3+ and Mn4+ co-doped BaLaMgNbO6 double perovskite phosphors for WLED application | |
| CN100506947C (en) | Method for low temperature synthesis of zinc magnesium silicate green florescent powder of regular particle shape | |
| CN103484118A (en) | Up-conversion luminescent material with yttria-stabilized zirconia as substrate and preparation method thereof | |
| CN107163941B (en) | Alkaline earth metal tungsten molybdate red fluorescent powder and preparation method thereof | |
| CN107523297A (en) | Upper conversion emitting red light powder and preparation method thereof | |
| CN109082272A (en) | A kind of red light fluorescent powder and preparation method thereof | |
| CN107686728A (en) | Upper conversion green emitting powder and preparation method thereof | |
| CN107523298B (en) | Yttrium cerium composite oxide based up-conversion luminescent material and preparation method thereof | |
| CN104845615B (en) | A kind of rare-earth doped beta phase Sr2SiO4Nano-powder and preparation method thereof | |
| CN105733576B (en) | Warm white LED double-perovskite type titanate red fluorescence powder and preparation method thereof | |
| CN102925142B (en) | Method for preparing ternary sulfide and quaternary sulfur oxide phosphor powder | |
| CN114316957B (en) | Blue light excited red fluorescent material and preparation method and application thereof | |
| CN108559504A (en) | A kind of high sensitivity fluorescence temperature-measurement material and preparation method thereof | |
| CN107573934A (en) | One kind mixes Mn4+Fluogermanic acid potassium red fluorescence powder preparation method | |
| CN104861973B (en) | Preparation method for green fluorescent powder applicable to white-light LED with lanthanum titanate serving as substrate and application of method | |
| CN109777422B (en) | Blue fluorescent powder suitable for purple light excitation, preparation method thereof and light-emitting device | |
| CN106968016B (en) | Preparation, performance and application of green luminescent material terbium lead polyborate | |
| CN102585815B (en) | Orange-red long path persistence luminescent material and preparation method thereof | |
| CN106010528A (en) | Bismuth-manganese-doped blue fluorescent powder and preparation method and application thereof | |
| CN107573936A (en) | A kind of zirconia solid solution base up-conversion luminescence powder material and preparation method thereof | |
| CN102061168A (en) | Method for improving luminosity of europium-doped yttrium oxide red fluorescent powder | |
| CN101265408B (en) | Samarium doping gadolinium aluminate base fluorescent powder body and preparation method thereof | |
| CN109762563A (en) | It is a kind of with β-potassium carbonate structure orthoborate fluorescent powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171229 |
|
| WD01 | Invention patent application deemed withdrawn after publication |