CN110357591A - A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof - Google Patents
A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof Download PDFInfo
- Publication number
- CN110357591A CN110357591A CN201910710219.3A CN201910710219A CN110357591A CN 110357591 A CN110357591 A CN 110357591A CN 201910710219 A CN201910710219 A CN 201910710219A CN 110357591 A CN110357591 A CN 110357591A
- Authority
- CN
- China
- Prior art keywords
- ion
- red light
- emitting red
- activated
- light fluorescence
- 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/10—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 aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- 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
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
- C09K11/641—Chalcogenides
- C09K11/643—Chalcogenides with alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3267—MnO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention provides ion-activated corundum phase emitting red light fluorescence ceramics of a kind of Mn4+ and preparation method thereof, chemical formula is (Al1‑x‑yMn4+ xM2+ y)2O3;M2+For Mg2+Ion or Ca2+The Mg of ion or arbitrary proportion2+And Ca2+Ion population.Above-mentioned emitting red light fluorescence ceramics the preparation method comprises the following steps: press (Al1‑x‑yMnxM2+ y)2O3Chemical composition weighs corresponding raw material, is uniformly mixed by modes such as batch mixer, barreling, ball millings, then in pure oxygen atmosphere, after 1200-1800 DEG C of temperature range heat preservation heat treatment 0.5-120 h, cooling down to obtain the final product.Bright red fluorescence transmitting is presented in the emitting red light fluorescence ceramics prepared using the method for the present invention under ultraviolet-blue violet light-blue light excitation, the emitting red light fluorescence ceramics have very high thermal conductivity, have the characteristics that at low cost, physicochemical stability is good, preparation controllability is high.
Description
Technical field
The present invention relates to a kind of preparation methods of fluorescent ceramic material, and in particular to a kind of Mn4+Ion-activated corundum is mutually red
Color luminous fluorescent ceramics and preparation method thereof.
Background technique
Fluorescence conversion type is still a kind of technology path of current white light LEDs mainstream, now commercial fluorescence conversion type white light
LED is that the Ce:YAG yellow fluorescent powder being scattered in pellosil by blue-light LED chip excitation is constituted.However, Ce:YAG fluorescent powder
Although light efficiency is very high (internal quantum efficiency up to 90% or more), lacks red color light component in its fluorescence spectrum, cause colour temperature higher, shows
Colour index is relatively low.
In recent years, Mn4+Ion-activated red light flourescent material causes scientific research and the very big concern of industrial circle, is improving LED
Room lighting color quality and plant light compensation lighting area have huge applications space, and existing commodity come out, such as K2SiF6:Mn4 +Deng.However, the material system moisture resistance can be poor, and need to have negatively environment and human body using HF acid in preparation process
It influences.
Currently, the Mn of scientific research personnel's exploitation4+Ion-activated emitting red light fluorescent material, majority are concentrated on Mn4+Ion
The perovskite fluoride system and oxide system of octahedral coordination structure, wherein the chemical constituent of oxide-base material has
To the trend for complicating development.
In addition the cost of material of emitting red light fluorescent material in the prior art is high, technology of preparing is complicated, physical and chemical performance not
It is ideal.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of Mn4+Ion-activated corundum phase emitting red light fluorescence pottery
Porcelain and preparation method thereof, this method solve existing Mn4+Ion-activated fluoride red light flourescent material physicochemical stability is undesirable,
And use during the preparation process to human body, the harmful HF of environment is sour the problems such as.
Specific technical solution is as follows:
A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics, chemical formula are (Al1-x-yMn4+ xM2+ y)2O3, wherein
0.000005≤x≤0.1,0 y≤0.3 ﹤, wherein M2+For Mg2+Ion or Ca2+The Mg of ion or arbitrary proportion2+And Ca2+Ion
Combination.
Preferably, the chemical formula (Al of the emitting red light fluorescence ceramics1-x-yMn4+ xM2+ y)2O3In, x=0.00025, y=
0.00025。
Preferably, the chemical formula (Al of the emitting red light fluorescence ceramics1-x-yMn4+ xM2+ y)2O3In, x=0.0005, y=
0.0005。
Above-mentioned Mn4+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, comprising the following steps:
S1. solid reaction process or wet chemical method are used, by chemical formula (Al1-x-yMn4+ xM2+ y)2O3, according to Mn4+Ion and M2
Any concentration ratio target doping concentration calculate, weigh needed for various raw materials Mass Calculation, weigh needed for various raw materials
Quality.
S2. raw material is uniformly mixed using wet ball grinding or dry method barreling, raw material incorporation time is 2-24h, more preferably former
Material incorporation time is 10h.
S3. uniformly mixed powder is passed through into uniaxial pressure-isostatic cool pressing or biscuit is made in slip-casting shaping process.
S4. biscuit is placed in oxidizing atmosphere sintering furnace and is sintered, 1200 DEG C -1800 DEG C of sintering range, in oxygen
Change and be sintered in atmosphere, soaking time is 0.5-120 h；Wherein preferred sintering temperature is 1500 DEG C or 1600 DEG C, preferably burns heat preservation
Time is 5h.
S5. Mn is obtained after cooling down4+Ion-activated corundum phase emitting red light fluorescence ceramics.
It further, is chemical formula (Al in the various raw materials of emitting red light fluorescence ceramics described in step S11-x-yMn4+ xM2 + y)2O3,
The raw material for providing Al is Al2O3、Al(OH)3、Al(NO3)3One of；
Mn is provided4+Raw material be MnO2、MnO、MnCO3、Mn(OH)2One of；
M is provided2+Raw material be MgO, Mg (OH)2, one of Mg (OH).
The Mn4+The amount of ion substance in every mole of fluorescence ceramics product is 0.000005-0.1mol, M2+Total object
The amount of the amount of matter substance in every mole of fluorescence ceramics product is 0-0.3mol.
Further, oxidizing atmosphere is non-current or flowing oxidizing atmosphere in step S4, can be pure oxygen or is higher than
The mixed gas of ambient oxygen partial pressure；The mixed gas be oxygen mix with air gas, oxygen and nitrogen mixed gas,
One of oxygen and other inert gas mixed gas.
The present invention uses Al2O3、Al(OH)3、Al(NO3)3、MnO2、MnO、MnCO3、Mn(OH)2、MgO、Mg(OH)2Or Mg
(OH) etc. it is initial feed, is uniformly mixed raw material using wet ball grinding or dry method barreling；Uniformly mixed powder is passed through into list
Biscuit is made in axis pressure-moulding process such as isostatic cool pressing or slip casting.Biscuit is placed in high-temperature atmosphere tube furnace, in oxygen atmosphere
Sintering, obtained Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics, it is red with what is become clear under ultraviolet~blue violet light excitation
Color fluorescent emission, and its wavelength of the fluorescence peak can be by changing M2+The type of ion is adjusted.
This excellent luminance matrix object phase of target lock-on corundum of the present invention, using simple and easy high-temperature solid phase reaction method,
It is aided with atmosphere heat treatment during solid phase reaction, to improve fluorescence efficiency and ceramic dense degree, while solid phase reaction temperature can be lowered
Degree.
Compared with prior art, the present invention its technological progress is significant.Mn of the invention4+Ion-activated corundum is mutually red
Luminous fluorescent ceramic preparation has preparation method simple, and raw material easily obtains, and material preparation cost is low, easy to operate, controllability
Height, chemical composition are suitble to the advantages that being mass produced entirely without murder by poisoning.Mn of the invention4+Ion-activated corundum phase emitting red light
Fluorescence ceramics have important application in the fields such as high-color development LED and plant light compensation illumination.
Detailed description of the invention
Fig. 1 is the (Al that embodiment 1 is prepared using ultraviolet specrophotometer0.9995Mn0.00025M2+ 0.00025)2O3It is red
The absorbance curve of color luminous fluorescent ceramics.The ceramics being prepared have stronger absorption within the scope of 250 ~ 500 nm.
Fig. 2 is using X-ray diffractometer to 1 gained (Al of embodiment0.9995Mn0.00025M2+ 0.00025)2O3Emitting red light fluorescence
The XRD test map that ceramics carry out, by being compared with standard card, it was demonstrated that the ceramics being prepared are α-Al2O3This single object
Phase.
Fig. 3 is using Fluorescence Spectrometer to 1 gained (Al of embodiment0.9995Mn0.00025M2+ 0.00025)2O3Emitting red light fluorescence
Fluorescence spectrum of the ceramics under the excitation of 405 nm blue lights, the centre of luminescence for the ceramics being prepared are 678 nm.
Fig. 4 is using Fluorescence Spectrometer to 1 gained (Al of embodiment0.9995Mn0.00025M2+ 0.00025)2O3Emitting red light fluorescence
Thermal conductivity measured by ceramics, at 25 DEG C, measured thermal conductivity is 26.27 W/ (mK).
Fig. 5 is the (Al that embodiment 2 is prepared using Fluorescence Spectrometer0.999Mn0.0005M2+ 0.0005)2O3Emitting red light
Fluorescence spectrum of the fluorescence ceramics under the excitation of 405 nm blue lights, the centre of luminescence for the ceramics being prepared are 678 nm.
Fig. 6 is the (Al that embodiment 3 is prepared using Fluorescence Spectrometer0.9995Mn0.00025M2+ 0.00025)2O3Emitting red light is glimmering
Fluorescence spectrum of the light ceramic under the excitation of 405 nm blue lights, the centre of luminescence for the ceramics being prepared are 678 nm.
Fig. 7 is the (Al that embodiment 4 is prepared using Fluorescence Spectrometer0.999Mn0.0005M2+ 0.0005)2O3Emitting red light
Fluorescence spectrum of the fluorescence ceramics under the excitation of 405nm blue light, the centre of luminescence for the ceramics being prepared are 678 nm.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Principles and features of the present invention are described in further detail below with reference to examples and drawings, example is only used
It invents, is not intended to limit the scope of the present invention in explaining.
Embodiment 1
Chemical formula (the Al of fluorescence ceramics described in the present embodiment1-x-yMn4+ xM2+ y)2O3In, x=0.00025, y=0.00025.
With Al2O3、MnO2It is raw material with MgO, weighs Al2O329.96 g, MnO20.03 g, MgO 0.01g.By Al2O3、
MnO2It is put into polytetrafluoroethylene (PTFE) ball grinder with MgO, agate ball and suitable alcohols is added, mix 10 by planetary ball mill
Hour.
After ball milling stops, uniformly mixed powder is pressed into plain embryo by uniaxial pressure-isostatic cool pressing.
Plain embryo is finally put into corundum tube furnace at 1600 DEG C the normal pressure in flowing pure oxygen atmosphere and is heat-treated 5 hours hairs
Raw solid phase reaction, rear furnace cooling obtain the manganese ion activated corundum phase emitting red light ceramics of tetravalence.
The absorption spectrum for the fluorescent material that the embodiment of the present invention 1 is prepared is tested using ultraviolet-visible spectrophotometer,
As shown in Figure 1, it can be seen that the fluorescent material has strong light absorption in 250~500 nm ranges.
Using x-ray powder diffraction instrument, gained phosphor material is mutually detected, testing result is statistics indicate that gained is glimmering
The object of luminescent material is mutually corundum, and XRD spectrum is as shown in Figure 2.By being compared with standard card, it was demonstrated that the ceramics being prepared are α-
Al2O3This single object phase.
Using Fluorescence Spectrometer, the fluorescent material that the test embodiment of the present invention 1 is prepared is under the excitation of 405 nm blue lights
Fluorescence spectrum, test results are shown in figure 3.The centre of luminescence for the ceramics being prepared is 678 nm.
The thermal conductivity for the ceramics being prepared is measured, test results are shown in figure 4.At 25 DEG C, surveyed
The thermal conductivity obtained is 26.27 W/ (mK).
From the figure 3, it may be seen that the manganese ion activated corundum phase emitting red light ceramics of tetravalence that the embodiment of the present invention 1 is prepared are in ultraviolet light
It can produce narrowband red emission under excitation, luminous peak position is in 678 nm.The sample is measured in Fluorescence Spectrometer using integrating sphere
Fluorescence quantum yield is 54%.
Embodiment 2
Chemical formula (the Al of fluorescence ceramics described in the present embodiment1-x-yMn4+ xM2+ y)2O3In, x=0.0005, y=0.0005.
With Al2O3、MnO2It is raw material with MgO, weighs Al respectively2O3 29.96 g、MnO20.02 g of 0.03 g, MgO.It will
Al2O3、MnO2It is put into polytetrafluoroethylene (PTFE) ball grinder with MgO, agate ball and suitable alcohols is added, it is mixed by planetary ball mill
Close 10 hours.
After ball milling stops, uniformly mixed powder is pressed into plain embryo by uniaxial pressure-isostatic cool pressing.
Finally plain embryo is put into corundum tube furnace at 1600 DEG C and is heat-treated 5 hours using oxygen stream normal pressure in atmosphere of taking offence
Reaction is undergone phase transition, rear furnace cooling obtains the manganese ion activated corundum phase emitting red light ceramics of tetravalence.
Using Fluorescence Spectrometer, the fluorescent material that the test embodiment of the present invention 2 is prepared is under the excitation of 405 nm blue lights
Fluorescence spectrum, test results are shown in figure 5.The centre of luminescence for the ceramics being prepared is 678 nm.
Embodiment 3
The method that embodiment 3 prepares fluorescent material is substantially the same manner as Example 1, only difference is that the temperature of heat treatment is 1500
℃。
Fluorescence Spectrometer is equally used, the fluorescent material that the test embodiment of the present invention 3 is prepared is in 405 nm ultraviolet lights
Fluorescence spectrum under excitation, test results are shown in figure 6, and the centre of luminescence for the ceramics being prepared is 678 nm, that is, obtains
The feux rouges of 678nm.
Embodiment 4
Chemical formula (the Al of fluorescence ceramics described in the present embodiment1-x-yMn4+ xM2+ y)2O3In, x=0.0005, y=0.0005.
With Al2O3、MnO2With Mg (OH)2For raw material, Al is weighed respectively2O3 29.96 g、MnO20.03 g, Mg (OH)2
0.02 g.By Al2O3、MnO2With Mg (OH)2It is put into polytetrafluoroethylene (PTFE) ball grinder, agate ball and suitable alcohols is added, pass through row
Planetary ball mill mixes 10 hours.
After ball milling stops, uniformly mixed powder is pressed into plain embryo by uniaxial pressure-isostatic cool pressing.
Finally plain embryo is put into corundum tube furnace at 1600 DEG C and is heat-treated 5 hours using oxygen stream normal pressure in atmosphere of taking offence
Reaction is undergone phase transition, rear furnace cooling obtains the manganese ion activated corundum phase emitting red light ceramics of tetravalence.
Fluorescence Spectrometer is equally used, the fluorescent material that the test embodiment of the present invention 4 is prepared swashs in 405 nm blue lights
The fluorescence spectrum given, test results are shown in figure 7, and the centre of luminescence for the ceramics being prepared is 678 nm, that is, obtains 678
The feux rouges of nm.
To sum up, this method has many advantages, such as that material preparation cost is low, preparation process is simple, is suitable for large-scale industrial production,
There is important application in the fields such as high color rendering index (CRI) LED and plant light compensation illumination.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (9)
1. a kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics, it is characterised in that: the emitting red light fluorescence ceramics
Chemical formula is (Al1-x-yMn4+ xM2+ y)2O3, wherein 0.000005≤x≤0.1,0 y≤0.3 ﹤, wherein M2+For Mg2+Ion or Ca2+
The Mg of ion or arbitrary proportion2+And Ca2+Ion population.
2. Mn according to claim 14+Ion-activated corundum phase emitting red light fluorescence ceramics, it is characterised in that: the red
Chemical formula (the Al of luminous fluorescent ceramics1-x-yMn4+ xM2+ y)2O3In, x=0.00025, y=0.00025.
3. Mn according to claim 14+Ion-activated corundum phase emitting red light fluorescence ceramics, it is characterised in that: the red
Chemical formula (the Al of luminous fluorescent ceramics1-x-yMn4+ xM2+ y)2O3In, x=0.0005, y=0.0005.
4. Mn as described in claim 14+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, which is characterized in that
The following steps are included:
S1. solid reaction process or wet chemical method are used, by chemical formula (Al1-x-yMn4+ xM2+ y)2O3It is various needed for calculating, weighing
The quality of raw material;
S2. raw material is uniformly mixed using wet ball grinding or dry method barreling, raw material incorporation time is 2-24h;
S3. uniformly mixed powder is passed through into uniaxial pressure-isostatic cool pressing or biscuit is made in slip-casting shaping process;
S4. biscuit is placed in oxidizing atmosphere sintering furnace and is sintered, 1200 DEG C -1800 DEG C of sintering range, in oxic gas
It is sintered in atmosphere, soaking time is 0.5-120 h；
S5. Mn is obtained after cooling down4+Ion-activated corundum phase emitting red light fluorescence ceramics.
5. Mn according to claim 34+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, feature exist
In: it is chemical formula (Al in the various raw materials of emitting red light fluorescence ceramics described in step S11-x-yMn4+ xM2+ y)2O3,
The raw material for providing Al is Al2O3、Al(OH)3、Al(NO3)3One of；
Mn is provided4+Raw material be MnO2、MnO、MnCO3、Mn(OH)2One of；
M is provided2+Raw material be MgO, Mg (OH)2, one of Mg (OH).
6. Mn according to claim 34+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, feature exist
In: raw material incorporation time described in step S2 is 10h.
7. Mn according to claim 34+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, feature exist
In: sintering temperature described in step S4 is 1500 DEG C or 1600 DEG C.
8. Mn according to claim 34+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, feature exist
In: soaking time described in step S4 is 5h.
9. Mn according to claim 34+The preparation method of ion-activated corundum phase emitting red light fluorescence ceramics, feature exist
In: oxidizing atmosphere is non-current or flowing oxidizing atmosphere in step S4, can be pure oxygen or is higher than ambient oxygen partial pressure
Mixed gas；The mixed gas is that oxygen mixes with air gas, oxygen and nitrogen mixed gas, oxygen and other inertia
One of gas mixing gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910710219.3A CN110357591A (en) | 2019-08-02 | 2019-08-02 | A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910710219.3A CN110357591A (en) | 2019-08-02 | 2019-08-02 | A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110357591A true CN110357591A (en) | 2019-10-22 |
Family
ID=68221830
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910710219.3A Pending CN110357591A (en) | 2019-08-02 | 2019-08-02 | A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110357591A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094120A (en) * | 2020-10-16 | 2020-12-18 | 贵州赛义光电科技有限公司 | Fluorescent ceramic with adjustable light emitting color and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010054708A1 (en) * | 2000-06-27 | 2001-12-27 | Sumitomo Chemical Company, Limited | Method of producing aluminate fluorescent substance, a fluorescent substance and a diode containing a fluorescent substance |
| CN101402857A (en) * | 2008-10-29 | 2009-04-08 | 华南理工大学 | Red luminous material for LED and producing process thereof |
| US20110101275A1 (en) * | 2004-06-10 | 2011-05-05 | Gundula Roth | Luminescent material |
| CN103333686A (en) * | 2013-07-03 | 2013-10-02 | 惠州学院 | Manganese (IV) doped red phosphor and preparation method thereof |
| CN104531144A (en) * | 2014-12-14 | 2015-04-22 | 中国科学院福建物质结构研究所 | CaMg<2>Al<16>O<27>:Mn <4+> red fluorescent powder and preparation technology thereof |
| CN108503352A (en) * | 2018-03-27 | 2018-09-07 | 中国科学院上海硅酸盐研究所 | A kind of garnet-base red fluorescence ceramic material and preparation method thereof |
-
2019
- 2019-08-02 CN CN201910710219.3A patent/CN110357591A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010054708A1 (en) * | 2000-06-27 | 2001-12-27 | Sumitomo Chemical Company, Limited | Method of producing aluminate fluorescent substance, a fluorescent substance and a diode containing a fluorescent substance |
| US20110101275A1 (en) * | 2004-06-10 | 2011-05-05 | Gundula Roth | Luminescent material |
| CN101402857A (en) * | 2008-10-29 | 2009-04-08 | 华南理工大学 | Red luminous material for LED and producing process thereof |
| CN103333686A (en) * | 2013-07-03 | 2013-10-02 | 惠州学院 | Manganese (IV) doped red phosphor and preparation method thereof |
| CN104531144A (en) * | 2014-12-14 | 2015-04-22 | 中国科学院福建物质结构研究所 | CaMg<2>Al<16>O<27>:Mn <4+> red fluorescent powder and preparation technology thereof |
| CN108503352A (en) * | 2018-03-27 | 2018-09-07 | 中国科学院上海硅酸盐研究所 | A kind of garnet-base red fluorescence ceramic material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FEOFILOV,SP ET AL.: "Selective laser spectroscopy of RE3+ and Mn4+ in sol-gel technique produced Al2O3", 《JOURNAL OF LUMINESCENCE》 * |
| YUDONG XU ET AL.: "The role of co-dopants on the luminescent properties of α-Al2O3:Mn4+ and BaMgAl10O17:Mn4+", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094120A (en) * | 2020-10-16 | 2020-12-18 | 贵州赛义光电科技有限公司 | Fluorescent ceramic with adjustable light emitting color and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110857389B (en) | Near-infrared fluorescent powder and light-emitting device containing same | |
| CN110129051B (en) | La4Ca3Si6N14Crystal and fluorescent powder and preparation method | |
| CN111378445A (en) | Cr (chromium)3+Preparation and application method of doped near-infrared broad-spectrum luminescent material | |
| JP2021529240A (en) | Red light / near infrared light emitting material, its preparation method, and light emitting device | |
| CN116120928B (en) | Ultra-wideband emission near infrared fluorescent powder and preparation method thereof | |
| CN112342021A (en) | Near-infrared broadband emission luminescent material, preparation method thereof and luminescent device comprising material | |
| CN114590831B (en) | LaSi 2 N 3 O crystal and fluorescent powder and preparation method thereof | |
| CN116200194B (en) | Near infrared luminescent material, preparation method thereof and LED light source containing luminescent material | |
| CN112011332A (en) | Far-red fluorescent powder and light-emitting device comprising same | |
| CN106554777A (en) | A kind of colourity is with adjustable luminescent material of temperature and preparation method and application | |
| CN110357591A (en) | A kind of Mn4+Ion-activated corundum phase emitting red light fluorescence ceramics and preparation method thereof | |
| CN106544024B (en) | A kind of gallium aluminate fluorescent powder and preparation method thereof | |
| CN110591711B (en) | Gallate red fluorescent powder for white light LED and preparation method thereof | |
| CN104673287A (en) | Long-wavelength high-brightness nitride red fluorescent powder and preparation method thereof | |
| CN104232081B (en) | A kind of light converting function material and its preparation method and application | |
| CN106995702B (en) | A kind of gallium germanic acid alkali dark red light emitting material and preparation method thereof | |
| CN114437723B (en) | Near-infrared luminescent material, preparation method thereof and LED (light-emitting diode) luminescent device | |
| CN108863345A (en) | A kind of luminescence medium ceramic material and preparation method thereof | |
| CN112322292B (en) | Eu3+Doped fluorescent material and preparation method thereof | |
| CN110846035B (en) | Erbium ion activated fluorescent powder and preparation method thereof | |
| CN110846034B (en) | Dy 3+ Activated fluorescent powder and preparation method thereof | |
| CN106497557A (en) | A kind of short wavelength silicate green fluorescent powder of efficient stable and preparation method and application | |
| CN108410453B (en) | Europium-doped single-matrix white-light fluorescent material and preparation method and application thereof | |
| CN112159213A (en) | Zero-light-decay luminescent ceramic and preparation method thereof | |
| CN105860973B (en) | A kind of magnesium Indium phosphate red or green emitting phosphor and its preparation |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191022 |