CN115044960B - Rotary oscillation high-temperature furnace - Google Patents

Rotary oscillation high-temperature furnace Download PDF

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CN115044960B
CN115044960B CN202210393947.8A CN202210393947A CN115044960B CN 115044960 B CN115044960 B CN 115044960B CN 202210393947 A CN202210393947 A CN 202210393947A CN 115044960 B CN115044960 B CN 115044960B
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hole
support
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vibrating
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CN115044960A (en
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朱崇强
刘景祥
杨雪
杨春晖
雷作涛
郝树伟
宋梁成
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Harbin Institute of Technology
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    • C30CRYSTAL GROWTH
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    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00Single-crystal growth directly from the solid state
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    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/02Production of homogeneous polycrystalline material with defined structure directly from the solid state
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/34Silicates

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Abstract

A rotary oscillation high-temperature furnace relates to a high-temperature furnace. The rotary oscillation high-temperature furnace comprises a support frame, a hearth, a crucible holder, a hollow sleeve, a crucible, a support rod, a rotary disk, a bolt, a belt pulley, a rotary motor, a belt, a lifting platform, a vibrating rod and a vibrating motor; the crucible support is fixed with a hollow sleeve below the crucible support, and the hollow sleeve is connected with a support rod with a belt pulley through a bolt; the rotating motor can drive the supporting rod to rotate through a belt; the vibrating rod bottom mounting is on lift platform, and the distance that the top held in the palm the bottom with the crucible is adjusted through lift platform, and vibrating motor and vibrating rod fixed connection can hold in the palm the vibration transmission for the crucible. The rotary oscillation high-temperature furnace can avoid lattice dislocation caused by heat transfer of a hearth of the sintering furnace, can also avoid impurity phase caused by static sintering, improves the uniformity and quality of crystal products, and can be used in the field of high-temperature synthesis.

Description

Rotary oscillation high-temperature furnace
Technical Field
The present invention relates to a high temperature furnace.
Background
The high-temperature sintering furnace plays a great role in a method for preparing crystals on a large scale, almost all high-melting point crystals are prepared by using the high-temperature sintering furnace, and the crystals are synthesized or grown by carrying out heat preservation operation at high temperature. However, when the existing high-temperature sintering furnace works, the crucible is placed at the bottom of the hearth and is fixed, the temperature in the crucible is easy to disturb due to uneven heat transfer of the hearth in the temperature rising and reducing process, and the slight disturbance of the temperature can cause the dislocation of arrangement in the crystal growth process; on the other hand, the raw materials in the crucible are static during heat preservation, and when various raw materials are contained, impurity phases are easy to crystallize due to nonuniform mixing of local raw materials, so that the quality of crystals is influenced.
Disclosure of Invention
The invention provides a rotary oscillation high-temperature furnace, which aims to solve the technical problems that the heat transfer of the existing high-temperature furnace is unstable and the product is easy to crystallize to generate impure phases.
The rotary oscillation high-temperature furnace comprises a support frame 1, a hearth 2, a crucible support 3, a hollow sleeve 4, a support rod 5, a ceramic crucible 6, a rotary disk 7, a plug pin 8, a belt pulley 9, a rotary motor 10, a belt 11, a lifting platform 12, a vibrating rod 13 and a vibrating motor 14;
the support frame 1 comprises an upper platform 1-1 and a lower platform 1-2; the upper-layer platform 1-1 is provided with a first through hole 1-3 and a mounting hole 1-4; the lower platform 1-2 is provided with a second through hole 1-5;
a third hole is arranged below the hearth 2;
a fourth hole is arranged in the center of the rotating disc 7; the rotating disc 7 is arranged on the lower platform 1-2;
the axes of the third hole, the first through hole 1-3, the second through hole 1-5 and the fourth hole are on the same straight line;
the support rod 5 is a hollow cylindrical ceramic tube, and the lower end of the support rod 5 is fixed on the rotating disk 7; the upper end of the support rod 5 is inserted into the hearth 2 through the first through hole 1-3 and the third through hole;
the hollow sleeve 4 is fixed below the crucible support 3 and is of an integrated structure; the hollow sleeve 4 is sleeved outside the support rod 5, the lower end of the hollow sleeve 4 extends out of the hearth 2, the lower end of the hollow sleeve 4 is provided with a bolt 8, and the bolt 8 is used for controlling the connection and the fixation of the hollow sleeve 4 and the support rod 5;
the rotary motor 10 is arranged on the upper-layer platform 1-1, a belt pulley 9 is fixed outside the support rod 5 positioned between the upper-layer platform 1-1 and the lower-layer platform 1-2, and the belt pulley 9 is connected with the rotary motor 10 through a belt 11;
the vibrating rod 13 is of a solid structure, the bottom end of the vibrating rod 13 is fixed on the lifting platform 12, the vibrating rod 13 is inserted into the cavity of the supporting rod 5 through the second through holes 1-5 and the fourth through hole, the distance between the top end of the vibrating rod 13 and the bottom of the crucible holder is adjusted through the lifting platform 12, and the vibrating motor 14 is arranged on the lifting platform 12 and is fixedly connected with the vibrating rod 13;
the crucible support 3 is cylindrical, the crucible support 3 is positioned at the central position of the furnace chamber 2, and the ceramic crucibles 6 are uniformly fixed in the crucible support 3;
a heating device is arranged in the hearth 2.
Furthermore, the number of the ceramic crucibles 6 which are uniformly distributed and fixed in the crucible support 3 is 4-10;
furthermore, a groove 15 with an oval cross section is arranged in the crucible support 3, the ceramic crucible 6 is fixed in the groove 15, and the oval shape is convenient for taking and placing. After the ceramic crucible 6 is placed in the recess 15, the cavity portion is filled and fixed with a heat-resistant material.
The rotary oscillation high-temperature furnace is improved on the basis of the existing high-temperature sintering furnace, a rotary and oscillating device is additionally arranged at the center of a hearth of the rotary oscillation high-temperature furnace, and the rotary and oscillating processes are independent from the sintering process. According to the rotary oscillation high-temperature furnace, the hollow sleeve and the supporting rod are connected and fixed together through the bolt, when the rotary motor works, the supporting rod is driven to rotate through the belt, and the crucible holder also rotates under the fixing action of the bolt, so that the crucible is driven to rotate around the axis of the crucible holder at the central position of the furnace body, the uniform heat transfer is promoted, and the rotating speed can be adjusted by controlling the power of the motor. Extract the bolt to on rising the top that makes the vibrating arm with lift platform pushes up crucible and holds in the palm the end, the vibrating motor during operation, will vibrate direct transmission and give the bracing piece, the vibration of bracing piece holds in the palm the transmission through crucible and gives raw materials in crucible and the crucible, realizes sintering process in the powder dynamization, promotes the crystallization process, and oscillation frequency also can be adjusted according to motor frequency. The rotary oscillation high-temperature furnace can avoid dislocation in crystals caused by heat transfer of the hearth of the high-temperature sintering furnace, can also avoid impurity phases caused by static sintering, and can improve the uniformity of crystal products. The rotary oscillation high-temperature furnace is used for high-temperature sintering synthesis, so that elements can be mixed more uniformly, better doping in molecular lattices is achieved, and the quality of synthetic substances is improved.
Drawings
FIG. 1 is a schematic view of the structure of a rotary oscillation high temperature furnace of the present invention;
FIG. 2 is a schematic view showing the connection of a crucible holder 3, a hollow sleeve 4, a support rod 5 and a vibrating rod 13;
FIG. 3 is a schematic structural view of the supporting frame 1;
FIG. 4 is a schematic top view of the interior of the furnace 2;
FIG. 5 is a schematic view of the construction of the susceptor 3 and the ceramic crucible 6;
FIG. 6 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3 + XRD spectrogram of red phosphor;
FIG. 7 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3 + An excitation spectrum of the red phosphor;
FIG. 8 shows BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3 + Emission spectrogram of red phosphor;
FIG. 9 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3 + A CIE color coordinate diagram of the red fluorescent powder and a photograph taken by an ultraviolet analyzer;
FIG. 10 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Scanning electron microscope photographs of the red phosphor.
FIG. 11 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and commercial Y 2 O 2 S:Eu 3+ A color coordinate comparison chart of the red fluorescent powder;
FIG. 12 is BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Fluorescence attenuation curve of red fluorescent powder and fitting result chart.
In fig. 1-5, 1 is a support frame, 1-1 is an upper platform, 1-2 is a lower platform, 1-3 is a first through hole, 1-4 is a mounting hole, and 1-5 is a second through hole 1-5;2 is furnace, 3 is crucible holds in the palm, 4 is the cavity sleeve pipe, 5 is the bracing piece, 6 is ceramic crucible, 7 is the carousel, 8 is the bolt, 9 is the belt pulley, 10 is the rotating electrical machines, 11 is the belt, 12 is lift platform, 13 is the vibrating arm, 14 is vibrating motor, 15 is the cell body, 16 is the crucible lid.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: (see fig. 1-5) the rotary oscillation high-temperature furnace of the embodiment 1 is composed of a support frame 1, a furnace chamber 2, a crucible holder 3, a hollow sleeve 4, a support rod 5, a ceramic crucible 6, a rotary disk 7, a plug pin 8, a belt pulley 9, a rotary motor 10, a belt 11, a lifting platform 12, a vibrating rod 13 and a vibrating motor 14; the support frame 1 comprises an upper platform 1-1 and a lower platform 1-2; the upper-layer platform 1-1 is provided with a first through hole 1-3 and a mounting hole 1-4; the lower platform 1-2 is provided with a second through hole 1-5; a third hole is arranged below the hearth 2; a fourth hole is arranged in the center of the rotating disc 7; the rotating disc 7 is arranged on the lower platform 1-2; the axes of the third hole, the first through hole 1-3, the second through hole 1-5 and the fourth hole are on the same straight line; the support rod 5 is a hollow cylindrical ceramic tube, and the lower end of the support rod 5 is fixed on the rotating disc 7; the upper end of the support rod 5 is inserted into the hearth 2 through the first through hole 1-3 and the third through hole; the hollow sleeve 4 is fixed below the crucible support 3 and is of an integrated structure; the hollow sleeve 4 is sleeved outside the support rod 5, the lower end of the hollow sleeve 4 extends out of the hearth 2, the lower end of the hollow sleeve 4 is provided with a bolt 8, and the bolt 8 is used for controlling the connection, fixation and disconnection of the hollow sleeve 4 and the support rod 5; the rotary motor 10 is arranged on the upper-layer platform 1-1, a belt pulley 9 is fixed outside the support rod 5 positioned between the upper-layer platform 1-1 and the lower-layer platform 1-2, and the belt pulley 9 is connected with the rotary motor 10 through a belt 11; the vibrating rod 13 is of a solid structure, the bottom end of the vibrating rod 13 is fixed on the lifting platform 12, the vibrating rod 13 is inserted into the cavity of the supporting rod 5 through the second through holes 1-5 and the fourth hole, the distance between the top end of the vibrating rod 13 and the bottom of the crucible holder is adjusted through the lifting platform 12, and the vibrating motor 14 is arranged on the lifting platform 12 and is fixedly connected with the vibrating rod 13; the crucible support 3 is cylindrical, the crucible support 3 is positioned at the central position of the hearth 2, 4 grooves 15 with oval sections are uniformly distributed in the crucible support 3, and 4 ceramic crucibles 6 are fixed in the grooves 15; a heating device is arranged in the hearth 2.
BaY preparation Using Rotary Oscillating high-temperature furnace of example 1 4 Si 3 O 13 :Eu 3+ The method of the red fluorescent powder comprises the following steps:
1. according to BaY 4 Si 3 O 13 :Eu 3+ Accurately weighing 0.9867 g of BaCO according to the stoichiometric ratio 3 1.8516 g Y 2 O 3 0.9012 g of SiO 2 0.6335 g Eu 2 O 3 (Eu 3+ The doping amount is 18 percent); then 0.0185 g of fluxing agent Li is weighed 2 CO 3 (ii) a Adding all the weighed raw materials into an agate mortar, adding 3.5mL of isopropanol, stirring uniformly to form a paste, and grinding for 30min to uniformly mix raw material particles; drying to obtain a mixed raw material; wherein BaCO 3 、Y 2 O 3 、SiO 2 、Eu 2 O 3 、Li 2 CO 3 The purity of (A) is 4N;
2. transferring the mixed raw materials into a ceramic crucible 6, and placing the ceramic crucible into an oven to keep the temperature of the ceramic crucible at 100 ℃ for 40min; fully volatilizing the isopropanol and residual moisture;
3. after the upper cover of the crucible opening cover is tightly sealed, the crucible is fixed in a crucible groove of a crucible support 3 of the rotary oscillation high-temperature furnace;
4. sintering was carried out according to the following temperature control program:
(1) The hollow sleeve 4 is fixedly connected with the support rod 5 through a bolt 8; the distance between the top end of the vibrating rod 13 and the bottom of the crucible support is adjusted to 10mm through the lifting platform 12; the temperature in the hearth 2 is heated from room temperature to 800 ℃ at the speed of 6.5 ℃/min, and only the crucible holder 3 is rotated at the rotating speed of 5r/min while the temperature is raised;
(2) The hollow sleeve 4 is separated from the support rod 5 through the bolt 8; the distance between the top end of the vibrating rod 13 and the bottom of the crucible support is adjusted to be 0mm through the lifting platform 12; keeping the temperature in the hearth 2 at 800 ℃ for 120min, and only enabling the crucible holder 3 to vibrate at the vibration frequency of 1Hz while keeping the temperature;
(3) The hollow sleeve 4 is connected and fixed with the support rod 5 through a bolt 8; the distance between the top end of the vibrating rod 13 and the bottom of the crucible support is adjusted to 10mm through the lifting platform 12; the temperature in the hearth 2 is increased from 800 ℃ to 1350 ℃ at the speed of 4.5 ℃/min, and only the crucible support 3 rotates at the rotating speed of 4r/min while the temperature is increased;
(4) The hollow sleeve 4 is separated from the support rod 5 through the bolt 8; the distance between the top end of the vibrating rod 13 and the bottom of the crucible support is adjusted to be 0mm through the lifting platform 12; the temperature in the hearth 2 is kept at 1350 ℃ for 3h, and only the crucible holder 3 is vibrated at the vibration frequency of 1Hz while the temperature is kept;
(5) The hollow sleeve 4 is fixedly connected with the support rod 5 through a bolt 8; the distance between the top end of the vibrating rod 13 and the bottom of the crucible support is adjusted to 10mm through the lifting platform 12; the temperature in the hearth 2 is reduced from 1350 ℃ to room temperature at the speed of 7 ℃/min, and only the crucible support 3 is rotated at the rotating speed of 5r/min while the temperature is reduced;
5. taking the product out of the rotary oscillation high-temperature furnace, grinding the product to 300 meshes, washing the product twice by using deionized water, washing the product once by using isopropanol, and finally drying the product for 4 hours in an oven with the temperature of 100 ℃ to obtain BaY 4 Si 3 O 13 :Eu 3+ And (4) red fluorescent powder.
And (3) comparison test: a common high-temperature furnace without rotation and oscillation is used for a comparison test, and the method comprises the following steps:
1. according to BaY 4 Si 3 O 13 :Eu 3+ Accurately weighing 0.9867 g of BaCO according to the stoichiometric ratio 3 1.8516 g Y 2 O 3 0.9012 g of SiO 2 0.6335 g Eu 2 O 3 (ii) a Then 0.0185 g of fluxing agent Li is weighed 2 CO 3 (ii) a Adding the mixture into an agate mortar, adding 3.5mL of isopropanol, uniformly stirring to form a paste, and grinding for 30min to uniformly mix raw material particles; drying to obtain a mixed raw material; wherein BaCO 3 、Y 2 O 3 、SiO 2 、Eu 2 O 3 、Li 2 CO 3 The purity of (A) is 4N;
2. transferring the mixed raw materials into a ceramic crucible 6, and placing the ceramic crucible into an oven to keep the temperature of the ceramic crucible at 100 ℃ for 40min; fully volatilizing the isopropanol and residual moisture;
3. covering the crucible with a cover and placing the crucible in a furnace chamber in normal high temperature without rotation and oscillation;
4. sintering was carried out according to the following temperature control program:
(1) The temperature in the hearth 2 is increased from room temperature to 800 ℃ at the speed of 6.5 ℃/min;
(2) Keeping the temperature in the hearth 2 at 800 ℃ for 120min;
(3) The temperature in the hearth 2 is increased from 800 ℃ to 1350 ℃ at the speed of 4.5 ℃/min;
(4) Keeping the temperature in the hearth 2 at 1350 ℃ for 3h;
(5) The temperature in the hearth 2 is reduced from 1350 ℃ to room temperature at the speed of 7 ℃/min;
5. taking the product out of the rotary oscillation high-temperature furnace, grinding the product to 300 meshes, washing the product twice by using deionized water, washing the product once by using isopropanol, and finally drying the product for 4 hours in an oven with the temperature of 100 ℃ to obtain comparative BaY 4 Si 3 O 13 :Eu 3+ And (4) red fluorescent powder.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ XRD test is carried out on the red fluorescent powder, the obtained XRD spectrogram is shown in figure 6, and as can be seen from figure 6, baY prepared by using a rotary oscillation high-temperature furnace is compared with a standard PDF card 4 Si 3 O 13 :Eu 3+ The red fluorescent powder can be well matched with a standard card, particularly the position of a characteristic peak at 25-30 degrees can be well matched with the peak intensity, and the fact that Eu can be promoted by additionally arranging rotation and oscillation during sintering is shown 3+ Better enter the inside of crystal lattice and the prepared crystal has less impurity content.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ The red phosphors are subjected to excitation spectrum test, the obtained excitation spectrum is shown in fig. 7, and the excitation peak positions of the two red phosphors are not obviously changed per se, but the peak intensities are changed. BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The excitation peak intensity of the red fluorescent powder is obviously increased, which also indicates that the rotating and oscillating device causes Eu to be in 3+ More easily enter the internal sites of the crystal lattice to ensure that Eu 3+ The near ultraviolet and blue light can be absorbed more.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ The emission spectrum of the red phosphor is shown in fig. 8, and as can be seen from fig. 8, the BaY prepared in example 1 is shown in fig. 8 4 Si 3 O 13 :Eu 3+ The emission spectrum peak value of the red fluorescent powder is integrally higher than that of BaY prepared by a contrast test 4 Si 3 O 13 :Eu 3+ The red phosphor, consistent with the excitation spectrum results, also shows that the rotating and oscillating device promotes Eu 3+ And the light enters the internal sites of the crystal lattice, so that the luminous intensity of red light is improved.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ Red phosphor and BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ The emission spectrum data of the red fluorescent powder is led into CIE-1931 chromaticity diagram software, and a CIE color coordinate diagram obtained by calculation is shown in FIG. 9 and can directly reflect the luminous color of a sample. BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ Red phosphor having CIE color coordinates (0.619, 0.347), baY prepared in example 1 4 Si 3 O 13 :Eu 3+ The color coordinates of the red fluorescent powder are (0.644, 0.345), and it can be obviously seen that the red light purity of the sample is obviously improved by the rotating and oscillating device.
BaY prepared in example 1 was observed by taking a photograph with an ultraviolet analyzer 4 Si 3 O 13 :Eu 3+ Red phosphor vs. BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ The red light purity of the red fluorescent powder is obviously increased. The luminous purity was calculated by equation 1:
Figure RE-GDA0003797161620000061
wherein (x) i ,y i ) Is the standard daylight color coordinate, the value is (0.31, 0.316),
(x d ,y d ) For the color coordinate of 613nm, the color coordinate (x) of 613nm is obtained by looking up the table d ,y d ) Is (0.67, 0.32);
and (x, y) preparing red fluorescent powder CIE color coordinates.
Calculated BaY prepared by comparative experiment 4 Si 3 O 13 :Eu 3+ The luminous purity of the red fluorescent powder is 86.25 percent; baY prepared in example 1 4 Si 3 O 13 :Eu 3+ The luminous purity of the red fluorescent powder is improved to 93.12 percent, which shows that the rotary oscillation device also promotes the luminous purity of red light.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The scanning electron microscope photograph of the red fluorescent powder is shown in fig. 10, and as can be seen from fig. 10, the crystal grain surface of the sample is smooth and full, the fusion degree is good, the particle diameter is between 3 and 10 mu m, the requirement of the red fluorescent powder particle size for the white light LED can be met, and the red fluorescent powder can be firmly coated on the surface of an ultraviolet/blue light chip.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The red phosphor has a color coordinate of (0.644, 0.345), which is compared to commercial Y 2 O 2 S:Eu 3+ The red phosphor color coordinates (0.631, 0.350) were compared and found to lie in the ratio Y at the CIE color coordinate position as shown in FIG. 11 2 O 2 S:Eu 3+ The red fluorescent powder is in a redder area, and the red light emitting requirement of the commercial red fluorescent powder is met.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The fluorescence decay curve and the fitting result of the red phosphor are shown in FIG. 12, the fluorescence decay curve is fitted by formula 2, and Eu is calculated by formula 3 3+ Fluorescence lifetime tau ave . After fitting R 2 The value of 0.9968 is close to 1, which shows that the fitting effect is good and the result is reliable. Calculating tau from the fluorescence lifetime as the elapsed time required for the time when the luminous intensity at the excitation time gradually decays to 1/e of the luminous intensity at the excitation time ave The value is 1.59ms, which is beneficial to continuously maintaining stable luminescence.
Figure RE-GDA0003797161620000062
Figure RE-GDA0003797161620000071
As can be seen from comparison between the embodiment 1 and the comparative test, the rotary oscillation high-temperature furnace of the embodiment can promote uniform distribution and doping of elements in the product, and is beneficial to improving the product quality.

Claims (3)

1. A rotary oscillation high-temperature furnace is characterized by comprising a support frame (1), a hearth (2), a crucible support (3), a hollow sleeve (4), a support rod (5), a ceramic crucible (6), a rotating disc (7), a bolt (8), a belt pulley (9), a rotating motor (10), a belt (11), a lifting platform (12), a vibrating rod (13) and a vibrating motor (14); wherein the support frame (1) comprises an upper layer platform (1-1) and a lower layer platform (1-2); the upper layer platform (1-1) is provided with a first through hole (1-3) and a mounting hole (1-4); the lower platform (1-2) is provided with a second through hole (1-5); a third hole is arranged below the hearth (2); a fourth hole is formed in the center of the rotating disc (7); the rotating disc (7) is arranged on the lower-layer platform (1-2); the axes of the third hole, the first through hole (1-3), the second through hole (1-5) and the fourth hole are on the same straight line; the support rod (5) is a hollow cylindrical ceramic tube, and the lower end of the support rod (5) is fixed on the rotating disc (7); the upper end of the supporting rod (5) is inserted into the hearth (2) through the first through hole (1-3) and the third through hole; the hollow sleeve (4) is fixed below the crucible support (3) and is of an integrated structure; the hollow sleeve (4) is sleeved outside the supporting rod (5), the lower end of the hollow sleeve (4) extends out of the hearth (2), the lower end of the hollow sleeve (4) is provided with a bolt (8), and the bolt (8) is used for controlling the connection and fixation and disconnection of the hollow sleeve (4) and the supporting rod (5); the rotary motor (10) is arranged on the upper-layer platform (1-1), a belt pulley (9) is fixed outside the supporting rod (5) between the upper-layer platform (1-1) and the lower-layer platform (1-2), and the belt pulley (9) is connected with the rotary motor (10) through a belt (11); the vibrating rod (13) is of a solid structure, the bottom end of the vibrating rod (13) is fixed on the lifting platform (12), the vibrating rod (13) is inserted into a cavity of the supporting rod (5) through the second through hole (1-5) and the fourth hole, the distance between the top end of the vibrating rod (13) and the bottom of the crucible support is adjusted through the lifting platform (12), and the vibrating motor (14) is arranged on the lifting platform (12) and is fixedly connected with the vibrating rod (13); the crucible support (3) is cylindrical, the crucible support (3) is positioned at the central position of the furnace chamber (2), and the ceramic crucible (6) is uniformly fixed in the crucible support (3); a heating device is arranged in the hearth (2).
2. A rotary oscillating high-temperature furnace according to claim 1, characterized in that the number of ceramic crucibles (6) uniformly distributed and fixed in the crucible holder (3) is 4-10.
3. A rotary oscillating high temperature furnace according to claim 1, characterized in that a groove (15) with an oval cross-section is provided in the crucible holder (3).
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