CN115044960A - Rotary oscillation high-temperature furnace - Google Patents
Rotary oscillation high-temperature furnace Download PDFInfo
- Publication number
- CN115044960A CN115044960A CN202210393947.8A CN202210393947A CN115044960A CN 115044960 A CN115044960 A CN 115044960A CN 202210393947 A CN202210393947 A CN 202210393947A CN 115044960 A CN115044960 A CN 115044960A
- Authority
- CN
- China
- Prior art keywords
- crucible
- hole
- support
- rod
- hearth
- 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.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/34—Silicates
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 the 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
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, and the high-temperature sintering furnace is required to be used for preparing almost all high-melting-point crystals, and the high-temperature sintering furnace is used for carrying out heat preservation operation at high temperature so as to synthesize or grow the crystals. 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 be disturbed due to uneven heat transfer of the hearth in the temperature rising and falling process, and the slight disturbance of the temperature can cause the dislocation of arrangement in the crystal growth process; on the other hand, when the crucible is kept warm, the raw materials in the crucible are static, and when various raw materials are contained, impurity phases are easy to crystallize due to nonuniform local raw material mixing, so that the quality of crystals is influenced.
Disclosure of Invention
The invention provides a rotary oscillation high-temperature furnace, aiming at solving the technical problems that the heat transfer of the existing high-temperature furnace is unstable and the product is easy to crystallize out of 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 bolt 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 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 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 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 hearth 2, and 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 uniformly distributed and fixed in the crucible support 3 is 4-10;
furthermore, a groove 15 with an oval section is arranged in the crucible support 3, and the ceramic crucible 6 is fixed in the groove 15, so that the taking and placing are facilitated due to the oval shape. After the ceramic crucible 6 is placed in the recess 15, the cavity portion is filled with a heat-resistant material and fixed.
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 in the center of a hearth of the rotary oscillation high-temperature furnace, and the rotary and oscillating processes and the sintering process are independent. The rotary oscillation high-temperature furnace is characterized in that the hollow sleeve and the supporting rod are connected and fixed together through the bolt, the supporting rod is driven to rotate through the belt when the rotary motor works, and the crucible support is driven to rotate due to the fixing effect of the bolt, so that the crucible is driven to rotate around the axis of the crucible support 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 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 + XRD spectrogram of red phosphor;
FIG. 7 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 + Excitation spectrum of red phosphor;
FIG. 8 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 + Emission spectrogram of red phosphor;
FIG. 9 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 + 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 photograph of red fluorescent powder.
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 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 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:
pressing BaY 4 Si 3 O 13 :Eu 3+ Accurately weighing 0.9867 g of BaCO 3 1.8516 g of 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, 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;
secondly, transferring the mixed raw materials into a ceramic crucible 6, and putting the ceramic crucible into an oven to keep the temperature of the ceramic crucible at 100 ℃ for 40 min; fully volatilizing the isopropanol and residual moisture;
thirdly, after the crucible opening is covered with a cover and is tightly sealed, fixing the crucible in a crucible groove of a crucible support 3 of the rotary oscillation high-temperature furnace;
fourthly, sintering according to the following temperature control program:
(1) 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 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 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 reduced from 1350 ℃ to room temperature at the speed of 7 ℃/min, and only the crucible support 3 rotates at the rotating speed of 5r/min while the temperature is reduced;
v, V,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:
pressing BaY 4 Si 3 O 13 :Eu 3+ Accurately weighing 0.9867 g of BaCO 3 1.8516 g of 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;
secondly, the mixed raw materials are moved into a ceramic crucible 6 and put into an oven to be kept for 40min at the temperature of 100 ℃; fully volatilizing the isopropanol and residual moisture;
thirdly, covering the crucible with a cover and placing the crucible in a furnace chamber in normal high temperature without rotation and oscillation;
fourthly, sintering 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 120 min;
(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 3 h;
(5) the temperature in the hearth 2 is reduced to the room temperature from 1350 ℃ at the speed of 7 ℃/min;
fifthly, 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 cleaning the productThen the mixture was dried in an oven at 100 ℃ for 4 hours to obtain BaY as a control 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, compared with a standard PDF card, BaY prepared by utilizing a rotary oscillation high-temperature furnace 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 intensity of the excitation peak of the red phosphor is obviously increased, and the Eu is enabled to be driven by the rotating and oscillating device 3+ More easily enter the internal sites of the crystal lattice to make 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 measured, and the obtained emission spectrum is shown in fig. 8, and as can be seen from fig. 8, BaY prepared in this example 1 4 Si 3 O 13 :Eu 3+ The peak value of the emission spectrum 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.
The 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:
wherein (x) i ，y i ) Is the standard daylight color coordinate, the numerical 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 phosphor was increased to 93.12%, indicating that the rotary oscillating device also promoted the luminous purity of red light.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The scanning electron micrograph of the red phosphor is shown in fig. 10, and as can be seen from fig. 10, the sample crystal grain surface is smooth and full, the fusion degree is good, the particle diameter is between 3 and 10 μm, the particle size requirement of the red phosphor for the white light LED can be met, and the red phosphor 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 color coordinates 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 at the ratio Y in 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 requirement of red light emission of the commercial red fluorescent powder is met.
BaY prepared in example 1 4 Si 3 O 13 :Eu 3+ The fluorescence attenuation curve and the fitting result of the red phosphor are shown in FIG. 12, and the fluorescence attenuation curve is fitted by formula 2 and Eu is calculated by formula 3 3+ Fluorescence lifetime tau ave . After fitting R 2 0.9968 is close to 1, indicating that the fitting 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.
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, which 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 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 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 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 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 the 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 hearth (2), and the ceramic crucible (6) is uniformly fixed in the crucible support (3); a heating device is arranged in the hearth (2).
2. The rotary oscillation high-temperature furnace according to claim 1, characterized in that the number of the ceramic crucibles (6) uniformly distributed and fixed in the crucible support (3) is 4-10.
3. A rotary oscillating high-temperature furnace according to claim 1, characterized in that the susceptor (3) is provided with a groove (15) having an elliptical cross-section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210393947.8A CN115044960B (en) | 2022-04-14 | 2022-04-14 | Rotary oscillation high-temperature furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210393947.8A CN115044960B (en) | 2022-04-14 | 2022-04-14 | Rotary oscillation high-temperature furnace |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115044960A true CN115044960A (en) | 2022-09-13 |
| CN115044960B CN115044960B (en) | 2023-01-31 |
Family
ID=83157273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210393947.8A Active CN115044960B (en) | 2022-04-14 | 2022-04-14 | Rotary oscillation high-temperature furnace |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115044960B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115873707A (en) * | 2022-12-29 | 2023-03-31 | 北京大学第三医院（北京大学第三临床医学院） | Cell harvesting system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005075689A (en) * | 2003-09-01 | 2005-03-24 | Nikon Corp | Apparatus and method for producing calcium fluoride single crystal |
| CN104729294A (en) * | 2015-03-20 | 2015-06-24 | 重庆科技学院 | Ultrasonic vibration activation assisted microwave sintering furnace |
| CN206247848U (en) * | 2016-11-30 | 2017-06-13 | 江西省汉氏贵金属有限公司 | The lift noble metal smelting furnace of rotatable crucible |
| CN109867433A (en) * | 2019-03-27 | 2019-06-11 | 中国建筑材料科学研究总院有限公司 | A kind of glass ingredient high frequency zone system and method |
| CN111410958A (en) * | 2020-05-21 | 2020-07-14 | 哈尔滨工业大学 | Method for preparing red fluorescent powder by using L iF as fluxing agent |
-
2022
- 2022-04-14 CN CN202210393947.8A patent/CN115044960B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005075689A (en) * | 2003-09-01 | 2005-03-24 | Nikon Corp | Apparatus and method for producing calcium fluoride single crystal |
| CN104729294A (en) * | 2015-03-20 | 2015-06-24 | 重庆科技学院 | Ultrasonic vibration activation assisted microwave sintering furnace |
| CN206247848U (en) * | 2016-11-30 | 2017-06-13 | 江西省汉氏贵金属有限公司 | The lift noble metal smelting furnace of rotatable crucible |
| CN109867433A (en) * | 2019-03-27 | 2019-06-11 | 中国建筑材料科学研究总院有限公司 | A kind of glass ingredient high frequency zone system and method |
| CN111410958A (en) * | 2020-05-21 | 2020-07-14 | 哈尔滨工业大学 | Method for preparing red fluorescent powder by using L iF as fluxing agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115873707A (en) * | 2022-12-29 | 2023-03-31 | 北京大学第三医院（北京大学第三临床医学院） | Cell harvesting system |
| CN115873707B (en) * | 2022-12-29 | 2023-11-24 | 北京大学第三医院（北京大学第三临床医学院） | Cell harvesting system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115044960B (en) | 2023-01-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100389504C (en) | YAG chip-type white-light light-emitting-diode and its packing method | |
| CN115044960B (en) | Rotary oscillation high-temperature furnace | |
| RU2215070C2 (en) | Device for production of monocrystal (versions), method of production of monocrystal (versions) and monocrystal (versions) | |
| CN1934029A (en) | Oxynitride powder and method for producing same | |
| CN109477239A (en) | Quartz glass crucibles and its manufacturing method and used quartz glass crucibles monocrystalline silicon manufacturing method | |
| CN107353899A (en) | A kind of Mn4+Doped fluoride monocrystalline red light material and preparation method and application | |
| CN108753296A (en) | A kind of red emitting material and its preparation method and application that can be excited by near ultraviolet or blue chip | |
| CN114736682B (en) | BaY prepared by using rotary oscillation high-temperature furnace 4 Si 3 O 13 :Eu 3+ Method for preparing red fluorescent powder | |
| US6905636B2 (en) | Method for the production of europium activated yttrium gadolinium borate phosphor particles | |
| CN111019648A (en) | Molten salt method preparation method of oxysalt or oxynitride fluorescent powder | |
| CN114032091A (en) | Ternary metal halide with ultrahigh fluorescence efficiency and preparation method thereof | |
| CN107163938A (en) | A kind of Ho doping bismuth silicate green emitting phosphor and preparation method thereof | |
| CN103469298A (en) | Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace | |
| EP1574602A1 (en) | Process for producing single crystal of compound semiconductor and crystal growing apparatus | |
| CN108467196A (en) | A kind of RGB light full-inorganic perovskite quantum dot and cellular glass composite luminescent material and preparation method thereof | |
| CN108485658A (en) | The manufacturing method of fluorophor | |
| CN108456516A (en) | The manufacturing method of fluorophor | |
| CN103469306A (en) | Method for growing Ce: YAG monocrystal fluorescent material | |
| CN114316957B (en) | Blue light excited red fluorescent material and preparation method and application thereof | |
| CN108893780A (en) | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof | |
| JP4092387B2 (en) | GaAs single crystal, manufacturing method thereof, and manufacturing apparatus thereof | |
| CN105552198B (en) | One kind uses MxSr1‑xTiO3：Eu2+, Mn2+The high colour gamut white light LEDs implementation method of blue light fluorescent powder | |
| CN1283628C (en) | 8- hydroxy quinoline bryhtening blue light and preparation method | |
| CN106497557A (en) | A kind of short wavelength silicate green fluorescent powder of efficient stable and preparation method and application | |
| CN106876541B (en) | A kind of LED encapsulation method uniformly coated based on fluorescent powder |
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 |