CN106747398B - Preparation method of copper-doped magnesium aluminate tunable luminescent material - Google Patents
Preparation method of copper-doped magnesium aluminate tunable luminescent material Download PDFInfo
- Publication number
- CN106747398B CN106747398B CN201611108063.4A CN201611108063A CN106747398B CN 106747398 B CN106747398 B CN 106747398B CN 201611108063 A CN201611108063 A CN 201611108063A CN 106747398 B CN106747398 B CN 106747398B
- Authority
- CN
- China
- Prior art keywords
- magnesium aluminate
- copper
- luminescent material
- solution
- tunable
- 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.)
- Active
Links
Images
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
- C04B35/44—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 aluminates
- C04B35/443—Magnesium aluminate spinel
-
- 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
- C04B35/624—Sol-gel processing
-
- 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
-
- 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
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
-
- 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)
- Dispersion Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a preparation method of a copper-doped magnesium aluminate tunable luminescent material, belonging to the technical field of luminescent material preparation. The invention adopts an improved sol-gel preparation process, namely a sol-gel micro-area complexation method, and uses Mg (NO)3)2·6H2O、Cu(NO3)2·3H2O、Al(NO3)3·9H2O and C2H2O4·2H2And preparing wet gel from O, drying, calcining, ball-milling, blank-making, molding and sintering at high temperature to obtain the spinel type copper-doped magnesium aluminate tunable luminescent material. The emission peak intensities of 470nm (blue region) and 720nm (red region) of the copper-doped magnesium aluminate tunable luminescent material prepared by the method can be adjusted by the doping amount of copper under the excitation condition of ultraviolet light (280 nm); the intrinsic magnesium aluminate luminescence is mainly in a red light region, while the copper-doped magnesium aluminate can appropriately enhance 470nm and appropriately weaken 720nm emission peak intensity, so that the two peak intensities are close to each other, and the blue light and the red light are tuned. Therefore, the spinel type copper-doped magnesium aluminate ceramic material is a novel potential material for preparing a visible light band tunable solid-state laser device.
Description
Technical Field
The invention relates to a copper-doped magnesium aluminate tunable luminescent material and an improved preparation method thereof, belonging to the technical field of luminescent material preparation.
Background
The magnesium aluminate ceramic has good physical properties and chemical properties, such as good chemical stability, wear resistance, corrosion resistance, small thermal expansion coefficient and good insulating property, and simultaneously has good mechanical properties, thermal vibration stability, slag resistance and the like. Can be applied to the fields of refractory materials, optical materials, catalysts, humidity-sensitive sensors and the like.
Among the magnesium aluminate ceramic preparation methods, the sol-gel method is a relatively common preparation method. The traditional sol-gel method is a method for preparing magnesium aluminate by carrying out solution, sol, gel, drying, heat treatment and other process procedures on organic or inorganic compounds. The starting materials for the process are generally pureThe metal and the alcohol or the metal alkoxide are based on the hydrolysis of the metal alkoxide in the same point of the sol-gel reaction process, and deionized water is required to be introduced into the reaction system to realize the step, so that the control of the water adding speed has a crucial influence on the sol-gel process and the particle size of formed powder, and finally the performance of the magnesium aluminate ceramic is influenced. In addition to this, this method has the following disadvantages: the raw materials are expensive, the preparation process is complex, the sol-gelation process and the powder particle size are difficult to effectively control, and a large amount of organic matters or other metal salt anions (such as Cl)-) The presence of (a) makes it difficult to completely remove the wet gel during the drying, calcining stage, etc.
Disclosure of Invention
The invention aims to provide a preparation method of a copper-doped magnesium aluminate tunable luminescent material, which uses Mg (NO) as a raw material3)2·6H2O、Cu(NO3)2·3H2O、Al(NO3)3·9H2O and C2H2O4·2H2O is taken as a raw material, wet gel is prepared by adopting a sol-gel micro-area complexation method, and the wet gel is dried, calcined, ball-milled, blank-made, molded and sintered at high temperature to obtain Cu y Mg1- y Al2O4（0.1% ≤yLess than or equal to 1.0 percent) of tunable luminescent material; the emission peak intensities of 470nm (blue region) and 720nm (red region) of the tunable luminescent material of the copper-doped magnesium aluminate prepared by the invention can be adjusted by the doping amount of copper under the excitation condition of ultraviolet light (280 nm); the intrinsic magnesium aluminate luminescence is mainly in a red light region, while the copper-doped magnesium aluminate can properly enhance 470nm and properly weaken the emission peak intensity of 720nm, so that the two peak intensities are close to each other, and the tuning of blue light and red light is realized; therefore, the spinel type copper-doped magnesium aluminate ceramic material is a novel potential material for preparing a visible light band tunable solid-state laser device.
The preparation method of the copper-doped magnesium aluminate tunable luminescent material specifically comprises the following steps:
(1) adopts a novel sol-gel micro-area complexation method,with Mg (NO)3)2·6H2O、Cu(NO3)2·3H2O and Al (NO)3)3·9H2Dissolving O in anhydrous alcohol to obtain solution A, and dissolving C in anhydrous alcohol2H2O4·2H2Dissolving O in absolute ethyl alcohol and adding a dispersing agent to obtain a solution B, atomizing the solution B, adding the atomized solution B into the solution A, uniformly mixing to obtain a solution C, stirring the solution C at room temperature to enable the solution C to fully react, heating to enable the ethanol to evaporate to obtain wet gel, drying the obtained wet gel overnight to obtain a precursor, wherein C is2H2O4·2H2The molar ratio of O to total metal ions is 1.0-1.2;
(2) placing the precursor in a furnace for roasting, cooling along with the furnace, and ball-milling for 1-2 hours to obtain copper-doped magnesium aluminate powder;
(3) then the powder is subjected to blank making, molding and high-temperature sintering to obtain the copper-doped magnesium aluminate ceramic tunable luminescent material, wherein the expression of the luminescent material is Cu y Mg y1-Al2O4Whereiny=0.1%~1.0%。
Preferably, in step (1) of the present invention, solution B is added to solution A in atomized form and completed within 30 minutes, and is fully complexed in the micro-domains.
Preferably, the dispersant is ethylene glycol, and the using amount of the ethylene glycol is 0.4-0.6 ml per 100ml of reaction liquid.
Preferably, in the step (1), the reaction time is 4-6 hours, and the solvent ethanol is stirred for 1-3 hours under the condition of evaporation at 70-80 ℃.
Preferably, the roasting temperature in the step (2) of the invention is 700-900 ℃, and the roasting time is 4-6 hours.
Preferably, the blank making in the step (3) of the invention is to slowly pressurize to 10-30 Mpa on a tablet press, unload after 1-2 minutes of pressure maintaining, and demould to obtain a cake-shaped blank.
Preferably, the high-temperature sintering temperature in the step (3) is 1400-1600 ℃, and the sintering time is 4-6 hours.
The principle of the invention is as follows:
(1) the invention improves the defects of the common sol-gel method, and prepares the spinel copper-doped magnesium aluminate tunable luminescent material by using the improved sol-gel preparation process, namely a sol-gel micro-area complexation method; adopts nitrate compound and solvent which are cheap and easy to obtain, Mg (NO)3)2·6H2O、Cu(NO3)2·3H2O and Al (NO)3)3·9H2And O. The method has the advantages that firstly, because the boiling point of the ethanol is low, the ethanol can be quickly volatilized when the wet gel is dried at 120 ℃ to form small honeycomb-shaped xerogel, and the solvent is dried more thoroughly; II, C2H2O4·2H2O has simple structure, the main chain only has two carbon atoms, and C is calcined at 700-900 DEG C2H2O4·2H2O and nitrate ions can be completely changed into gas to be discharged without residue, and in addition, the formed small honeycomb shape is also beneficial to C2H2O4·2H2Removing O and nitrate ions; thirdly, the process is simple and reliable.
(2) By C2H2O4·2H2O is used as a micro-area complexing agent, and a certain amount of C2H2O4·2H2Dissolving O in absolute ethyl alcohol, then adding a proper amount of dispersing agent-ethylene glycol, atomizing, adding into the solution A, and completing within 30 minutes, which is the key point of the sol-gel microcell complexation method; under magnetic stirring, C2H2O4·2H2The method can more effectively control the particle size of formed particles, so that the particle size of the prepared split body is more uniform and fine, and the atomic-level uniform mixing is favorably achieved.
The invention has the beneficial effects that:
(1) the method can more effectively control the particle size of the formed particles, so that the prepared split particles have more uniform and fine particle size and are beneficial to achieving atom-level uniform mixing.
(2) Under the excitation of 280nm ultraviolet light, the emission peak intensities of 470nm (blue light region) and 720nm (red light region) of the copper-doped magnesium aluminate tunable luminescent material prepared by the method can be properly adjusted, so that the two peak intensities are close to each other, and the tuning of blue light and red light is realized; in view of this, the spinel type copper-doped magnesium aluminate ceramic material prepared by the method is a novel potential material for preparing a visible light band tunable solid laser device.
(4) In the method, the magnesium aluminate material is doped with copper, and part of Mg vacancies are only replaced by Cu to form a solid solution, so that the optical performance of the magnesium aluminate material is adjusted.
Drawings
FIG. 1 is an XRD pattern of magnesium aluminate powder calcined at 900 deg.C with different copper doping concentrations;
FIG. 2 is an XRD pattern of magnesium aluminate ceramics sintered at 1500 ℃ for 5h with different copper doping concentrations;
FIG. 3 is an emission spectrum of magnesium aluminate ceramics sintered at 1500 ℃ for 5h with different copper doping concentrations.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, but the scope of the invention is not limited thereto.
Example 1
Cu of the present example y Mg y1-Al2O4（y= 0.1%) ceramic was prepared by the following steps:
(1) according to (A)n Mg+n Cu）:n AlMolar ratio of = 1: 2 2.5614g of Mg (NO) were weighed out3)2·6H2O、0.0024g Cu(NO3)2·3H2O and 7.5026g Al (NO)3)3·9H2Dissolving the three into 60ml of absolute ethyl alcohol to obtain solution A; weighing C2H2O4·2H2O dissolved in 40ml of absolute ethanol (C)2H2O4·2H2The molar ratio of O to the total metal ions is 1.0), 0.6mL of dispersant (ethylene glycol) is added, and the mixture is stirred and mixed uniformly to obtain solution B; by atomisationAtomizing the solution B, adding the atomized solution B into the solution A, finishing the atomization in 30 minutes, and uniformly mixing to obtain a solution C; stirring the solution C at room temperature for 5h, stirring at the constant temperature of 80 ℃ for 2h, evaporating ethanol to obtain light blue wet gel, and drying the wet gel at 120 ℃ overnight to obtain honeycomb-shaped small fluffy xerogel, namely a precursor.
(2) And (2) placing the precursor of the magnesium aluminate obtained in the step (1) in a box-type resistance furnace, roasting for 5h at 900 ℃, cooling to room temperature along with the furnace, taking out, and then placing in a ball mill for ball milling for 1 h to obtain the magnesium aluminate powder with the copper content of 0.1%.
(3) Pouring a proper amount of magnesium aluminate powder obtained in the step (2) into a mould, slowly pressurizing to 30Mpa on a tablet press, maintaining the pressure for 1min, unloading and demoulding to obtain a cake-shaped blank; sintering the cake-shaped blank at 1500 ℃ for 5h to obtain the magnesium aluminate ceramic.
Under the same preparation conditions, respectively takingy=0%，y=0.3%，y=0.5%，y=1.0%, different magnesium aluminate ceramics were prepared.
FIG. 1 is an XRD diagram of magnesium aluminate powder with different copper doping concentrations calcined at 900 ℃, and it can be seen from FIG. 1 that the copper-doped magnesium aluminate powder forms a single-phase spinel structure after being calcined at 900 ℃, and the powder has narrow half-height width cross and higher crystallinity.
FIG. 2 is an XRD diagram of magnesium aluminate ceramics with different copper doping concentrations sintered at 1500 ℃ for 5h, and as can be seen from FIG. 2, the copper-doped magnesium aluminate ceramics prepared by calcining, ball milling, blank making, molding and high-temperature sintering the powder have very high crystallinity, are single spinel phases and have very high purity.
FIG. 3 is an emission spectrum of magnesium aluminate ceramic sintered at 1500 ℃ for 5h with different copper doping concentrations, and it can be seen from FIG. 3 that as the Cu doping concentration increases gradually, the 470nm (blue region) emission peak intensity increases first and then decreases, reaching a maximum value when the Cu doping amount is 0.5%, and Cu is doped with MgAl2O4The intensity of the 470nm emission peak of the ceramic is saturated; cu doped MgAl2O4The emission peak of the ceramic 720nm (red area) is linearly reduced along with the increase of the Cu doping amount.
Example 2
Cu of the present example y Mg y1-Al2O4（y= 0.3%) ceramic was prepared by the following steps:
(1) according to (A)n Mg+n Cu）:n AlMolar ratio of = 1: 2 2.5563g of Mg (NO) were weighed out3)2·6H2O、0.0072g Cu(NO3)2·3H2O and 7.5026g Al (NO)3)3·9H2Dissolving the three into 60ml of absolute ethyl alcohol to obtain solution A;
weighing C2H2O4·2H2O dissolved in 40ml of absolute ethanol (C)2H2O4·2H2The molar ratio of O to the total metal ions is 1.0), 0.6mL of dispersant (ethylene glycol) is added, and the mixture is stirred and mixed uniformly to obtain solution B; atomizing the solution B by using an atomizer, adding the atomized solution B into the solution A, finishing the atomization within 30 minutes, and uniformly mixing to obtain a solution C; stirring the solution C at room temperature for 5h, stirring at a constant temperature of 75 ℃ for 1.5h, evaporating ethanol to obtain light blue wet gel, and drying the wet gel at 120 ℃ overnight to obtain honeycomb-shaped small fluffy xerogel, namely a precursor.
(2) And (2) placing the precursor of the magnesium aluminate obtained in the step (1) into a box-type resistance furnace, roasting for 6h at 700 ℃, cooling to room temperature along with the furnace, taking out, and then placing into a ball mill for ball milling for 1 h to obtain magnesium aluminate powder with the copper content of 0.3%.
(3) Pouring a proper amount of magnesium aluminate powder obtained in the step (2) into a mould, slowly pressurizing to 30Mpa on a tablet press, maintaining the pressure for 1min, unloading and demoulding to obtain a cake-shaped blank; sintering the cake-shaped blank at 1400 ℃ for 6h to obtain the magnesium aluminate ceramic.
Example 3
Cu of the present example y Mg y1-Al2O4（y= 0.5%) ceramic was prepared by the following steps:
(1) according to (A)n Mg+n Cu）:n AlMolar ratio of = 1: 2 2.5512g of Mg (NO) were weighed out3)2·6H2O、0.0121g Cu(NO3)2·3H2O and 7.5026g Al (NO)3)3·9H2Dissolving the three into 60ml of absolute ethyl alcohol to obtain solution A; weighing C2H2O4·2H2O dissolved in 40ml of absolute ethanol (C)2H2O4·2H2The molar ratio of O to the total metal ions is 1.1, 0.6mL of dispersant (ethylene glycol) is added, and the mixture is stirred and mixed uniformly to obtain solution B; atomizing the solution B by using an atomizer, adding the atomized solution B into the solution A, finishing the atomization within 30 minutes, and uniformly mixing to obtain a solution C; stirring the solution C at room temperature for 6h, stirring at the constant temperature of 80 ℃ for 2h, evaporating ethanol to obtain light blue wet gel, and drying the wet gel at 120 ℃ overnight to obtain honeycomb-shaped small fluffy xerogel, namely a precursor.
(2) And (2) placing the precursor of the magnesium aluminate obtained in the step (1) in a box-type resistance furnace, roasting for 6h at 800 ℃, cooling to room temperature along with the furnace, taking out, and then placing in a ball mill for ball milling for 1 h to obtain the magnesium aluminate powder with the copper content of 0.5%.
(3) Pouring a proper amount of magnesium aluminate powder obtained in the step (2) into a mould, slowly pressurizing to 10Mpa on a tablet press, maintaining the pressure for 2min, unloading and demoulding to obtain a cake-shaped blank; respectively sintering the cake-shaped green bodies at 1600 ℃ for 4h to obtain the magnesium aluminate ceramics.
Example 4
Cu of the present example y Mg y1-Al2O4（y= 1.0%) ceramic was prepared by the following steps:
(1) according to (A)n Mg+n Cu）:n AlMolar ratio of = 1: 2 2.5384g of Mg (NO) were weighed out3)2·6H2O、0.0242g Cu(NO3)2·3H2O and 7.5026g Al (NO)3)3·9H2Dissolving the three into 60ml of absolute ethyl alcohol to obtain solution A; weighing C2H2O4·2H2O dissolved in 40ml of absolute ethanol (C)2H2O4·2H2The molar ratio of O to the total metal ions is 1.2), 0.6mL of dispersant (ethylene glycol) is added, and the mixture is stirred and mixed uniformly to obtain solution B; atomizing the solution B by using an atomizer, adding the atomized solution B into the solution A, finishing the atomization within 30 minutes, and uniformly mixing to obtain a solution C; stirring the solution C at room temperature for 4h, stirring at constant temperature of 70 ℃ for 3h, evaporating ethanol to obtain light blue wet gel, and drying the wet gel at 120 ℃ overnight to obtain honeycomb-shaped small fluffy xerogel, namely a precursor.
(2) And (2) placing the precursor of the magnesium aluminate obtained in the step (1) into a box-type resistance furnace, roasting for 5h at 850 ℃, cooling to room temperature along with the furnace, taking out, and then placing into a ball mill for ball milling for 1 h to obtain the magnesium aluminate powder with the copper content of 1.0%.
(3) Pouring a proper amount of magnesium aluminate powder obtained in the step (2) into a mould, slowly pressurizing to 20Mpa on a tablet press, maintaining the pressure for 1min, unloading and demoulding to obtain a cake-shaped blank; and (3) trial sintering the cake-shaped blank at 1600 ℃ for 5h to obtain the magnesium aluminate ceramic.
In conclusion, the preparation method provided by the invention is used for preparing the high-purity and high-crystallinity copper-doped magnesium aluminate ceramic material with the spinel structure, and the improvement method provided by the invention is effective. In addition, under the excitation of 280nm ultraviolet light, the emission peak intensities of 470nm (blue light region) and 720nm (red light region) can be artificially and properly adjusted, so that the two peak intensities are close to each other, and the tuning of blue light and red light is realized. In view of this, the spinel type copper-doped magnesium aluminate ceramic material is a novel potential material for preparing a visible light band tunable solid-state laser device.
Claims (5)
1. A preparation method of a copper-doped magnesium aluminate tunable luminescent material is characterized by comprising the following steps:
(1) by sol-gel micro-area complexation with Mg (NO)3)2·6H2O、Cu(NO3)2·3H2O and Al (NO)3)3·9H2O is taken as raw material and dissolved in water according to the proportionAdding water and ethanol to obtain solution A, adding C2H2O4·2H2Dissolving O in absolute ethyl alcohol and adding a dispersing agent to obtain a solution B, atomizing the solution B, adding the atomized solution B into the solution A, uniformly mixing to obtain a solution C, stirring the solution C at room temperature to enable the solution C to fully react, heating to enable the ethanol to evaporate to obtain wet gel, drying the obtained wet gel overnight to obtain a precursor, wherein C is2H2O4·2H2The molar ratio of O to total metal ions is 1.0-1.2;
(2) placing the precursor in a furnace for roasting, cooling along with the furnace, and ball-milling for 1-2 hours to obtain copper-doped magnesium aluminate powder; the roasting temperature is 700-900 ℃, and the roasting time is 4-6 hours;
(3) then the powder is subjected to blank making, molding and high-temperature sintering to obtain the copper-doped magnesium aluminate ceramic tunable luminescent material, wherein the expression of the luminescent material is CuyMg1-yAl2O4Wherein y is 0.1% -1.0%; the high-temperature sintering temperature is 1400-1600 ℃, and the sintering time is 4-6 hours.
2. The method for preparing the tunable copper-doped magnesium aluminate luminescent material according to claim 1, wherein the tunable copper-doped magnesium aluminate luminescent material comprises the following steps: in step (1), solution B was added to solution A in atomized form and completed in 30 minutes, with full complexation in the micro-domains.
3. The method for preparing the tunable copper-doped magnesium aluminate luminescent material according to claim 1, wherein the tunable copper-doped magnesium aluminate luminescent material comprises the following steps: the dispersing agent is ethylene glycol, and the using amount of the ethylene glycol is 0.4-0.6 ml added in each 100ml of reaction liquid.
4. The method for preparing the tunable copper-doped magnesium aluminate luminescent material according to claim 1, wherein the tunable copper-doped magnesium aluminate luminescent material comprises the following steps: the reaction time in the step (1) is 4-6 hours, and the solvent ethanol is stirred for 1-3 hours under the condition of evaporation at 70-80 ℃.
5. The method for preparing the tunable luminescent material of copper-doped magnesium aluminate according to claim 1, wherein: and (4) slowly pressurizing to 10-30 Mpa on a tablet press, maintaining the pressure for 1-2 minutes, unloading and demolding to obtain a cake-shaped blank body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611108063.4A CN106747398B (en) | 2016-12-06 | 2016-12-06 | Preparation method of copper-doped magnesium aluminate tunable luminescent material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611108063.4A CN106747398B (en) | 2016-12-06 | 2016-12-06 | Preparation method of copper-doped magnesium aluminate tunable luminescent material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106747398A CN106747398A (en) | 2017-05-31 |
| CN106747398B true CN106747398B (en) | 2020-08-25 |
Family
ID=58878159
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611108063.4A Active CN106747398B (en) | 2016-12-06 | 2016-12-06 | Preparation method of copper-doped magnesium aluminate tunable luminescent material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106747398B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328634A (en) * | 2018-03-16 | 2018-07-27 | 昆明理工大学 | A kind of copper load zinc aluminate nano-powder and preparation method thereof |
| CN113121208A (en) * | 2019-12-30 | 2021-07-16 | 深圳市绎立锐光科技开发有限公司 | Preparation method of fluorescent ceramic and fluorescent ceramic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124180A (en) * | 2005-01-19 | 2008-02-13 | 默克专利股份公司 | Method for producing mixed oxides by way of spray pyrolysis |
| CN104556166A (en) * | 2014-12-09 | 2015-04-29 | 东北大学 | Method for preparing MgO.Al2O3 superfine powder by sol-gel process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE60118514T2 (en) * | 2001-01-24 | 2006-08-24 | Tas, Ahmet Cüneyt, Prof. Dr. | Process for the preparation of crystalline phosphor powder at low temperature |
-
2016
- 2016-12-06 CN CN201611108063.4A patent/CN106747398B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124180A (en) * | 2005-01-19 | 2008-02-13 | 默克专利股份公司 | Method for producing mixed oxides by way of spray pyrolysis |
| CN104556166A (en) * | 2014-12-09 | 2015-04-29 | 东北大学 | Method for preparing MgO.Al2O3 superfine powder by sol-gel process |
Non-Patent Citations (3)
| Title |
|---|
| 尖晶石型M Al2O4 ( M= Ni、Mg )纳米粉体的溶胶凝胶法制备及表征;韦秀华等;《中南民族大学学报(自然科学版)》;20060331;第8-11页 * |
| 尖晶石型复合氧化物MgxCu1-xAl2O4上苯酚甲醇烷基化制备邻甲酚;于庆勇;《精细石油化工》;20090331;第12-14页 * |
| 工艺参数对微区沉淀法制备纳米MgAl2O4 粉体的影响;李逵等;《稀有金属材料与工程》;20070831;第84-86页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106747398A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lee et al. | Preparation of Portland cement components by poly (vinyl alcohol) solution polymerization | |
| Jiao et al. | Low temperature synthesis of YAG: Ce phosphors by LiF assisted sol–gel combustion method | |
| Lv et al. | Synthesis of nano-sized and highly sinterable Nd: YAG powders by the urea homogeneous precipitation method | |
| CN107151029A (en) | A kind of sol gel synthesis preparation technology of tetra phase barium titanate powder | |
| KR101074152B1 (en) | The method for synthesizing nano-sized yttria power using pva at the low temperature | |
| CN106747398B (en) | Preparation method of copper-doped magnesium aluminate tunable luminescent material | |
| CN104761251B (en) | A kind of reaction sintering method preparing magnesium aluminate spinel | |
| CN111848153A (en) | Microwave dielectric ceramic, preparation method of microwave dielectric ceramic and communication device | |
| CN108530057A (en) | Sol-gel method application and preparation is in the morphology controllable CaTiO of energy storage3The method of ceramics | |
| Naderi-Beni et al. | Development of a new sol-gel route for the preparation of aluminum oxynitride nano-powders | |
| US11345642B2 (en) | Method for preparing alumina-based solid solution ceramic powder by using aluminum oxygen combustion synthesis water mist process | |
| Lu et al. | Novel phenomenon on valence unvariation of doping ion in Yb: YAG transparent ceramics using MgO additives | |
| CN101831292A (en) | Strontium aluminate luminous material and controllable synthesis method thereof | |
| TWI647179B (en) | Method for producing magnesium silicate fine particles | |
| Ji et al. | Dielectric properties of Ba0. 5Sr0. 5TiO3–MgO composites synthesized by a citrate gel in situ process | |
| Monros et al. | Effects of ZrO 2 precursors on the synthesis of V-ZrSiO 4 solid solutions by the sol-gel method | |
| CN103864423B (en) | A kind of preparation method of microwave dielectric ceramic materials | |
| Wang et al. | Synthesis of nanocrystalline ytterbium-doped yttria by citrate-gel combustion method and fabrication of ceramic materials | |
| Ge et al. | Influence of combustion reagent and microwave drying method on the characteristics of nano-sized Nd 3+: YAG powders synthesized by the gel combustion method | |
| CN113788677B (en) | High-entropy sesqui-rare earth sulfide ceramic material and preparation method and application thereof | |
| CN101935527A (en) | Preparation method of yttrium aluminium garnet nanometre green fluorescent powder | |
| CN104671274A (en) | Preparation method of CuAlO<2> powder | |
| Hreniak et al. | Luminescence properties of Tb-doped yttrium disilicate prepared by the sol–gel method | |
| Yu et al. | Synthesis and characterization of Zn 2 SiO 4: Mn 2+ nanocrystals and tuning of phase by controlling of silica shell thickness | |
| JPH01122964A (en) | Zirconia stabilized by yttrium and its production |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |