CN112110728A - Preparation method of yttrium aluminum garnet ceramic fluorescent film - Google Patents
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Abstract
The invention belongs to the field of material science, and relates to a preparation method of an yttrium aluminum garnet ceramic fluorescent film‑Pillared rare earth layered compound (Y)1‑x‑yGdxMy)2(OH)5NO3·nH2And O (x is more than or equal to 0 and less than or equal to 1, y is more than 0 and less than or equal to 0.1) to obtain a pillared product, stirring and stripping the pillared product in a formamide solution until the solution generates a Tyndall effect, and then performing centrifugal separation on the solution to obtain the ultrathin rare earth nanosheet. The nano-sheet is coated on the surface of the alumina substrate by spin coating, and a proper sintering method is adopted,the rare earth doped yttrium aluminum garnet transparent ceramic film is successfully prepared. The method is simple and easy to implement, provides a new method for synthesizing the garnet-structure ceramic, can realize the luminescence of different colors by regulating and controlling the types and doping amounts of the doped rare earth ions, constructs films with different optical functions, realizes the application in different directions, and has extremely high application prospect.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a preparation method of an yttrium aluminum garnet ceramic fluorescent film.
Background
The yttrium aluminum garnet structure (YAG) has excellent application prospect as a functional material due to good permeability and a series of excellent physical properties in visible light and infrared light regions, and Y in the structure3+The effective radius is similar to most rare earth ions, and the rare earth ions can be easily substituted for the effective radius to realize the luminescence of different colors, thereby becoming an important solid laser matrix material. The main method of the existing YAG transparent ceramic is to prepare YAG powder, and then to form the transparent ceramic by molding and sintering. The method has high sintering temperature (about 1900 ℃), high requirements on sintering equipment (such as vacuum sintering), difficult molding of fine and complex shapes and high cost.
General formula Ln2(OH)5NO3·nH2The 251-phase rare earth layered compound of O has excellent intercalation property and strippability because anions between layers are not coordinated with the laminate in a free state, and the rare earth nanosheet formed by stripping is mainly applied to the preparation of the fluorescent film. Different colors of luminescence can be realized by doping different rare earth ions into the layered compound, so that different luminescent films are formed.
Disclosure of Invention
The invention provides a method for preparing a YAG fluorescent ceramic film, which adopts Dodecyl Sulfonate (DS)-) Pillared rare earth layered compound (Y)1-x-yGdxMy)2(OH)5NO3·nH2O (x is more than or equal to 0 and less than or equal to 1, Y is more than 0 and less than or equal to 0.1) to obtain a pillared product, and the pillared product (Y)1-x-yGdxMy)2(OH)5DS·nH2And stirring and stripping the O in a formamide solution until the solution generates a Tyndall effect, and then performing centrifugal separation on the solution to obtain the ultrathin rare earth nanosheet. The nano-sheet is coated on the surface of the alumina substrate in a spin mode, and a proper sintering method is adopted to successfully synthesize (Y)1-x-yGdxMy)3Al5O12:(0≤x≤1，0＜y≤0.1)(YAG)，M＝Eu3+,Ce3+,Tb3+,Dy3+,Ho3+,Tm3+,Yb3+，Pr3+,Cr3+,Mn4+A ceramic membrane.
The technical scheme of the invention is as follows:
a preparation method of an yttrium aluminum garnet ceramic fluorescent film comprises the following steps:
step 1: weighing rare earth layered compound (Y) according to the molar ratio of 1: 1-501-x-yGdxMy)2(OH)5NO3·nH2O, wherein x is more than or equal to 0 and less than or equal to 1, y is more than 0 and less than or equal to 0.1, and M is Eu3+,Ce3+,Tb3+,Dy3+,Ho3+,Tm3+,Yb3+，Pr3+,Cr3+,Mn4+Measuring sodium dodecyl sulfate as one of the raw materials; after fully stirring, pouring the mixed solution into a hydrothermal inner container, and carrying out hydrothermal reaction for 1-72 h at 100-300 ℃ to ensure that the DS is obtained-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)1-x-yGdxMy)2(OH)5DS·nH2O; adding the pillared product into a formamide solution with the mass fraction of 50% -100% according to the proportion of 0.14g: 5-100 mL, stirring the mixed solution for 1-20 days, and stripping until the solution has an obvious Tyndall effect; centrifugally separating the solution, and dispersing the precipitate in alcohol to obtain a nano-flaky rare earth layered compound;
step 2: spin-coating the nano-sheet rare earth layered compound obtained in the step 1 on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a sample with the coating thickness of 50 nm-1 mu m; if the doped ion M is Eu3+、Dy3+、Ho3+、Tm3+、Yb3+、Pr3+、Cr3+、Mn4+Calcining under an oxygen atmosphere; if the doping ion M is Ce3+Or Tb3+Then, calcining in a reducing atmosphere; the calcination temperature is 1000-1500 ℃, and the sintering time is 2-100 h.
Further, a rare earth layered compound (Y) is preferable1-x-yGdxMy)2(OH)5NO3·nH2The molar ratio of O to sodium dodecyl sulfate is 1: 3-20.
Further, the hydrothermal reaction time is preferably 12 to 24 hours.
Further, it is preferable that the ratio of the pillared product to the formamide solution is 0.14g:20 to 30 mL.
Further, the nanosheet-shaped rare earth layered compound obtained in the step 1 is preferably spin-coated on the surface of the sapphire substrate subjected to hydrophilic treatment to obtain the yttrium aluminum garnet transparent ceramic fluorescent film.
Further, the reducing atmosphere is a hydrogen-argon mixed atmosphere.
The invention has the beneficial effects that: the (YAG) (Y) is successfully synthesized by a method of spin-coating a rare earth nano-sheet on the surface of sapphire and sintering1-x-yGdx)3Al5O12:MyX is more than or equal to 0 and less than or equal to 1, and y is more than 0 and less than or equal to 0.1, thereby effectively reducing the sintering temperature and the difficulty of forming complex shapes and providing a new method for synthesizing garnet structure ceramics.
Drawings
FIG. 1 is a schematic flow chart of all the examples of the invention for preparing YAG ceramic fluorescent films.
FIG. 2 is an XRD spectrum of YAG ceramic fluorescent films prepared in examples 1-5 of the present invention.
FIG. 3 is an XRD spectrum of YAG ceramic fluorescent films prepared in examples 6-7 of the present invention.
FIG. 4 is an XRD pattern of a YAG ceramic block made in accordance with a comparative example of the present invention.
Detailed Description
The following detailed description of the embodiments of the invention refers to the accompanying drawings.
The chemical reagents used in the examples of the present invention are analytical grade products.
Example 1(M ═ Eu)3+,x＝0,y＝0.05,T＝1000℃)
Weighing rare earth layered compound (Y)0.95Eu0.05)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:5) are weighed and stirred fully, the mixed solution is poured into a hydrothermal liner, and the hydrothermal reaction is carried out for 12 hours at the temperature of 120 ℃, so that the DS is obtained-Fully replace rare earth layerNO in the form of a compound3 -To obtain a pillared product (Y)0.95Eu0.05)2(OH)5DS·nH2And O. The pillared product is added into formamide solution (the proportion is 0.14g:20mL), and the mixed solution is stirred for 10 days for stripping until the solution has obvious Tyndall effect. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin-coating a certain amount of nano-sheets on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a film with the thickness of 60nm, and sintering the film for 20 hours at 1000 ℃ in an oxygen atmosphere to obtain YAG, Eu3+The XRD pattern of the fluorescent ceramic film is shown in figure 2(a), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Example 2(M ═ Dy)3+,x＝0.2,y＝0.01T＝1200℃)
Weighing rare earth layered compound (Y)0.79Gd0.2Dy0.01)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:12) are weighed and stirred fully, the mixed solution is poured into a hydrothermal liner, and hydrothermal reaction is carried out for 18 hours at 160 ℃, so that DS is obtained-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)0.79Gd0.2Dy0.01)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (0.14 g:25mL) and the mixture was stirred for 5 days to strip off until a significant Tyndall effect was observed. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin-coating a certain amount of nano-sheets on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a film with the thickness of 100nm, and sintering the film for 2 hours at 1200 ℃ in an oxygen atmosphere to obtain YAG (yttrium aluminum garnet): Dy3+The XRD pattern of the fluorescent ceramic film is shown in figure 2(b), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Example 3(M ═ Ce)3+,x＝0.5,y＝0.05,T＝1500℃)
Weighing rare earth layered compound (Y)0.45Gd0.5Ce0.05)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:10) are weighed and stirred fully, the mixed solution is poured into a hydrothermal inner container, and hydrothermal reaction is carried out for 16 hours at 140 ℃ so as to lead DS-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)0.45Gd0.5Ce0.05)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (0.14 g:28mL) and the mixture was stirred for 7 days to strip off until a significant Tyndall effect was observed. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin-coating a certain amount of nano-sheets on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a film with the thickness of 180nm, and sintering the film for 4 hours at 1500 ℃ in a reducing atmosphere to obtain YAG (yttrium aluminum garnet): Ce3+The XRD pattern of the fluorescent ceramic film is shown in figure 2(c), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Example 4(M ═ Tb)3+,x＝0.9,y＝0.1,T＝1300℃)
Weighing rare earth lamellar compound (Gd)0.9Tb0.1)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:15) are weighed and subjected to hydrothermal reaction at 170 ℃ for 20 hours to obtain DS-Fully substituted NO in rare earth layered compound3 -Obtaining a pillared product (Gd)0.9Tb0.1)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (0.14 g:25mL) and the mixture was stirred for 5 days to strip off until a significant Tyndall effect was observed. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin-coating a certain amount of nano-sheets on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a film with the thickness of 500nm, and sintering the film for 5 hours at 1300 ℃ in a reducing atmosphere to obtain YAG, Tb3+The XRD pattern of the fluorescent ceramic film is shown in figure 2(d), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Example 5(M ═ Er)3+,x＝0.9,y＝0.1,T＝1500℃)
Weighing rare earth lamellar compound (Gd)0.9Er0.1)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:30) are weighed and stirred fully, the mixed solution is poured into a hydrothermal liner, and hydrothermal reaction is carried out for 26 hours at 250 ℃ to ensure that the DS-Fully substituted NO in rare earth layered compound3 -Obtaining a pillared product (Gd)0.9Er0.1)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (0.14 g:30mL) and the mixture was stirred for 9 days to strip off until a significant Tyndall effect appeared in the solution. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin-coating a certain amount of nano-sheets on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a film with the thickness of 750nm, and sintering the film for 12 hours at 1500 ℃ in an oxygen atmosphere to obtain YAG (yttrium aluminum garnet): Er3+The XRD pattern of the fluorescent ceramic film is shown in figure 2(e), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Example 6(M ═ Cr)3+,x＝0.2,y＝0.03,T＝1400℃)
Weighing rare earth layered compound (Y)0.77Gd0.2Cr0.03)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:15) are weighed and subjected to hydrothermal reaction at 170 ℃ for 20 hours to obtain DS-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)0.77Gd0.2Cr0.03)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (0.14 g:28mL) and the mixture was stirred for 6 days to strip off until a significant Tyndall effect was observed. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin coating a certain amount of nano-sheets on the surface of the sapphire substrate subjected to hydrophilic treatment to obtain a film with the thickness of 600nm, and sintering the film for 18 hours at 1400 ℃ in an oxygen atmosphere to obtain YAG (yttrium aluminum garnet): Cr3+The XRD pattern of the fluorescent transparent ceramic film is shown in figure 3(a), which proves that the fluorescent transparent ceramic film is successfully synthesizedYAG fluorescent ceramic film.
Example 7(M ═ Mn)4+,x＝0.3,y＝0.02,T＝1400℃)
Weighing rare earth layered compound (Y)0.68Gd0.3Mn0.02)2(OH)5NO3·nH2O and sodium dodecyl sulfate (1:24) are weighed and subjected to hydrothermal reaction at 260 ℃ for 24 hours to ensure that the DS is obtained-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)0.68Gd0.3Mn0.02)2(OH)5DS·nH2And O. The pillared product was added to a formamide solution (ratio 0.14g:32mL) and the mixture was stirred for 8 days to strip off until a significant Tyndall effect was observed. And (4) carrying out centrifugal separation on the solution, and dispersing the precipitate into alcohol to obtain the flaky rare earth layered compound. Finally, spin coating a certain amount of nano-sheets on the surface of the sapphire substrate subjected to hydrophilic treatment to obtain a film with the thickness of 500nm, and sintering the film for 19 hours at 1400 ℃ in an oxygen atmosphere to obtain YAG (yttrium aluminum garnet)/Mn4+The XRD pattern of the fluorescent ceramic film is shown in figure 3(b), which proves that the YAG fluorescent ceramic film is successfully synthesized.
Comparative example
Weighing Y2O3And Al2O3Fully grinding powder with the molar ratio of 3:5, firstly calcining for 4 hours at 1400 ℃ in an oxygen atmosphere, then tabletting the mixed powder under 300Mpa, and calcining the pressed tablets for 8 hours at 1800 ℃ in the air to finally obtain the YAG ceramic chip. The XRD pattern of this ceramic wafer is shown in fig. 4, which is the same as the XRD pattern of all samples in the examples of the present invention. Proves that the YAG M with good crystallinity can be obtained by the synthesis mode introduced by the inventionyThe fluorescent ceramic thin film of (1).
Claims (6)
1. A preparation method of an yttrium aluminum garnet ceramic fluorescent film is characterized by comprising the following steps:
step 1: weighing rare earth layered compound (Y) according to the molar ratio of 1: 1-501-x-yGdxMy)2(OH)5NO3·nH2O, wherein x is more than or equal to 0 and less than or equal to 1, y is more than 0 and less than or equal to 0.1, and M is Eu3+,Ce3+,Tb3+,Dy3+,Ho3+,Tm3+,Yb3+，Pr3+,Cr3+,Mn4+Measuring sodium dodecyl sulfate as one of the raw materials; after fully stirring, pouring the mixed solution into a hydrothermal inner container, and carrying out hydrothermal reaction for 1-72 h at 100-300 ℃ to ensure that the DS is obtained-Fully substituted NO in rare earth layered compound3 -To obtain a pillared product (Y)1-x-yGdxMy)2(OH)5DS·nH2O; adding the pillared product into a formamide solution with the mass fraction of 50-100% according to the proportion of 0.14g: 5-100 mL, stirring the mixed solution for 1-20 days, and stripping until the solution has an obvious Tyndall effect; centrifugally separating the solution, and dispersing the precipitate in alcohol to obtain a nano-flaky rare earth layered compound;
step 2: spin-coating the nano-sheet rare earth layered compound obtained in the step 1 on the surface of the alumina substrate subjected to hydrophilic treatment to obtain a sample with the coating thickness of 50 nm-1 mu m; if the doped ion M is Eu3+、Dy3+、Ho3+、Tm3+、Yb3+、Pr3+、Cr3+、Mn4+Calcining under an oxygen atmosphere; if the doping ion M is Ce3+Or Tb3+Then, calcining in a reducing atmosphere; the calcination temperature is 1000-1500 ℃, and the sintering time is 2-100 h.
2. The method of claim 1, wherein the rare earth layered compound (Y) is1-x-yGdxMy)2(OH)5NO3·nH2The molar ratio of O to sodium dodecyl sulfate is 1: 3-20.
3. The method of claim 1, wherein the hydrothermal reaction time is 12-24 hours.
4. The method of claim 1, wherein the ratio of the pillared product to the formamide solution is 0.14 g/20-30 mL.
5. The method of claim 1, wherein the nano-flake rare earth layered compound obtained in step 1 is spin-coated on the surface of the sapphire substrate treated with hydrophilicity to obtain the yttrium aluminum garnet transparent ceramic fluorescent film.
6. The method of claim 1, wherein the reducing atmosphere is a mixed atmosphere of hydrogen and argon.
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