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19 results about "Flux method" patented technology

Flux method is a method of crystal growth where the components of the desired substance are dissolved in a solvent (flux). The method is particularly suitable for crystals needing to be free from thermal strain. It takes place in a crucible made of highly stable, non-reactive material. For production of oxide crystals, metals such as platinum, tantalum, and niobium are common. Production of metallic crystals generally uses crucibles made from ceramics such as alumina, zirconia, and boron nitride. The crucibles and their contents are often isolated from the air for reaction, either by sealing them in a quartz ampoule or by using a furnace with atmosphere control. A saturated solution is prepared by keeping the constituents of the desired crystal and the flux at a temperature slightly above the saturation temperature long enough to form a complete solution. Then the crucible is cooled in order to allow the desired material to precipitate. Crystal formation can begin by spontaneous nucleation or may be encouraged by the use of a seed. As material precipitates out of the solution, the amount of solute in the flux decreases and the temperature at which the solution is saturated lowers. This process repeats itself as the furnace continues to cool until the solution reaches its melting point or the reaction is stopped artificially.

Fluorinated guanidinium borate nonlinear optical crystal, method for preparing the same, and use thereof

The application provides a fluorinated guanidinium borate nonlinear optical crystal and a preparation method and application thereof. The chemical formula of the crystal is [C(NH2)3]B6O9F, the molecular weight is 287.95, the crystal belongs to an orthorhombic system, the space group is Pnma, Pna 21, the cell parameter is a=7.8420(11) Å, b=15.1862(19) Å, c=8.5762(9) Å, α =90°, β =90°, γ =90°, the unit cell volume is 1021.3(2) ų, the crystal is grown by a high-temperature solution method or a flux method, the frequency doubling effect of the crystal is 0.4 times of that of KH2PO4 (KDP), the ultraviolet cutoff edge is 190 nm, the birefringence is large, the birefringence is 0.133 @ 1064 nm, and the deep ultraviolet phase matching capability is deep, the shortest matching wavelength is 196 nm, and the crystal can be applied to deep ultraviolet nonlinear optical crystals in a full solid-state laser.
Owner:XINJIANG TECH INST OF PHYSICS & CHEM CHINESE ACAD OF SCI

Method for improving thickness and quality uniformity of crystal growth, repair method, and crystal

The application discloses a method for improving the thickness and quality uniformity of crystal growth, a repairing method and a crystal. The method comprises the following steps: providing a growth system required for growing a group III nitride crystal by a flux method liquid phase epitaxy, forming a temperature gradient between a top layer part and a bottom layer part of a molten growth material, so as to form a closed circulation flow field of the molten growth material and a nitrogen source in the molten growth material; and in an initial stage of the growth of the group III nitride crystal, adjusting the temperature gradient to a positive temperature gradient, and then alternately switching the temperature gradient between the positive temperature gradient and a negative temperature gradient, so as to change the nitrogen source concentration distribution and the growth rate of different regions of a growth interface of the group III nitride crystal, until the growth interface of the group III nitride crystal presents as a flat surface. The method provided by the application is simple in operation and wide in application range, and can reduce the production cost and improve the yield of the crystal.
Owner:SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI

Compound arsenic silicon gallium strontium and arsenic silicon gallium strontium infrared nonlinear optical crystal, preparation method and application

The application relates to a compound arsenic-silicon-gallium-strontium and an infrared nonlinear optical crystal of arsenic-silicon-gallium-strontium, a preparation method and application, the compound has a molecular formula of SrGa3Si4As 11 , a molecular weight of 1233.26 g / mol, an asymmetric center, and is crystallized in a hexagonal crystal system P , a 63 space group, a cell parameter of a=b=9.2604(3) A, c=11.6484(5) A, Z=2, and V=865.08(7) A 3 , and is prepared into a crystal by using a high-temperature melt method, a chemical vapor phase transmission method or a flux method. The crystal has strong laser damage resistance, large nonlinear optical effect, wide infrared transmission range, and simultaneously has the advantages of large hardness, good mechanical property, not easy to break and deliquesce, easy to process and store and the like, and can be used for manufacturing infrared nonlinear optical devices.
Owner:XINJIANG TECH INST OF PHYSICS & CHEM CHINESE ACAD OF SCI

Flux recovery device and method for growing gallium nitride single crystal by flux method

The invention discloses a fluxing agent recovery device and method for growing gallium nitride single crystals through a fluxing agent method, and belongs to the technical field of crystal material preparation. The device comprises a high-pressure cavity which internally comprises a flow choking cover, a backflow cavity and a single crystal growth cavity from top to bottom in sequence; wherein the backflow cavity is of a double-cone flow guide structure; the top of the backflow cavity is covered with the flow choking cover. The pressure regulation and control system comprises a pressure oscillation gas circuit, a crystal growth gas circuit and a pressure controller; the pressure oscillation gas circuit is used for introducing inert gas into the high-pressure cavity; the crystal growth gas circuit is directly communicated to the single crystal growth cavity from the outside of the high-pressure cavity, the crystal growth gas circuit and the pressure oscillation gas circuit are both connected with the pressure controller, and the pressure controller is used for periodically adjusting the internal pressure of the high-pressure cavity and controlling gas introduction of the crystal growth gas circuit. The heating element is used for heating the backflow cavity and the single crystal growth cavity respectively; according to the invention, the grown crystal can be effectively separated from the fluxing agent, and recovery of the fluxing agent is realized.
Owner:XI AN JIAOTONG UNIV

Method for improving growth thickness and quality uniformity of crystal, repairing method and crystal

The invention discloses a method for improving crystal growth thickness and quality uniformity, a repairing method and a crystal. The method comprises the following steps: providing a growth system required by liquid phase epitaxy growth of the III-group nitride crystal by a fluxing agent method, and forming a temperature gradient between a top layer part and a bottom layer part of a molten growth raw material so as to form a closed circulation flow field of the molten growth raw material and a nitrogen source in the molten growth raw material; and at the initial stage of III-nitride crystal growth, adjusting the temperature gradient into a positive temperature gradient, and alternately switching the temperature gradient between the positive temperature gradient and a negative temperature gradient so as to change the nitrogen source concentration distribution and the growth rate of different areas of the growth interface of the III-nitride crystal, until the growth interface of the group III nitride crystal is a flat surface. The method provided by the invention is simple to operate and wide in application range, and can reduce the production cost and improve the crystal yield.
Owner:SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI

Self-adaptive temperature compensation method for growing gallium nitride single crystal by sodium fluxing agent method

The invention discloses a self-adaptive temperature compensation method for growing gallium nitride single crystals by a sodium fluxing agent method, and belongs to the technical field of semiconductor crystal growth. The method comprises the following steps: in an inert atmosphere, putting sodium, gallium, carbon and a seed crystal into a crucible together, putting the crucible into a high-pressure reaction kettle, vacuumizing, filling nitrogen, and heating to a preset temperature and pressure; a dynamic regulation and control temperature function is calculated, and a temperature regulation and control function T = a4t + b4 is established; self-adaptive compensation is started in the later growth period (larger than or equal to 120 h), and the temperature is adjusted according to the formula T = a4t + b4; according to the method, fluctuation and attenuation of the supersaturation degree are automatically corrected through temperature compensation, the stable growth time of the crystal can be prolonged to 200 h or above, the dislocation density is smaller than or equal to 5 * 10 < 5 > cm <-2 >, and the method is suitable for efficient preparation of the high-quality gallium nitride single crystal of 2 inches or above.
Owner:JIANGXI SCI & TECH NORMAL UNIV

Non-Archimedes mosaic lattice structure and compound material thereof

The invention belongs to the field of condensed physical and quantum materials, and discloses a non-Archimedes mosaic lattice structure and a compound material thereof. The lattice is a periodic network which is formed by closely arranging and splicing at least three different types of geometrical shapes (including triangles, quadrangles, pentagons and the like) in a two-dimensional plane in a common-edge or common-angle mode, and a traditional Archimedes lattice frame is broken through. The preparation of the single crystal from the compound A3M9X13 (such as Rb3V9Te13 and Cs3V9Te13) of the crystal lattice through a fluxing agent method is realized for the first time. Wherein Rb3V9Te13 belongs to an orthorhombic system and contains a distorted pentagonal unit; the Cs3V9Te13 belongs to a hexagonal crystal system, and the symmetry is higher. According to the structure, complex file blocking units such as pentagons are introduced, a unique platform is provided for exploring quantum singular matter states, and the compound has structure tunability.
Owner:SHANGHAI JIAOTONG UNIV

Crystal interface regulation and control device and method for sodium fluxing agent method gallium nitride single crystal growth

The invention discloses a crystal interface regulation and control device and method for sodium flux method gallium nitride single crystal growth, and belongs to the technical field of crystal material preparation.The device comprises a reaction kettle body, a crucible is arranged in the reaction kettle body, the inner wall of the crucible is of a step structure, a flow guide plate is arranged on the step, and a side wall heating unit is arranged on the side wall of the reaction kettle body; a bottom heating unit is arranged at the bottom, and the reaction kettle body and the bottom of the crucible are of an embedded step structure. The embedded inner and outer step design of the reaction kettle body and the bottom of the crucible hinders heat transfer of the bottom heating unit and the side wall heating unit at the bottom of the reaction kettle body, and the supersaturation degree of gallium nitride in alloy melt is maintained to be slightly higher than the two-dimensional critical nucleation supersaturation degree through the side wall heating unit. The bottom heating unit is used for carrying out temperature control on the contact surface of the crystal and the alloy melt to form periodic temperature change, so that periodic regulation and control are carried out on the gallium nitride supersaturation degree of a crystal growth interface, and the quality and yield of the gallium nitride single crystal are improved.
Owner:XI AN JIAOTONG UNIV

Zr-Ru-Si-based ternary superconducting single crystal material, preparation method and application thereof, and terminal product

The invention relates to the technical field of superconducting single crystal materials, and discloses a Zr-Ru-Si-based ternary superconducting single crystal material, the chemical general formula is ZrxRuySiz, x is equal to 1.8-2.2, y is equal to 2.5-3.5, and z is equal to 3.5-4.5. The superconducting single crystal material belongs to a typical ternary transition metal silicide system, and a Si element is introduced to participate in construction of a crystal skeleton, so that a stable silicide structure is formed; the crystal belongs to a monoclinic system C2 / c space group, and has unique spatial symmetry and a three-dimensional crystal skeleton; and the material has good crystallinity and high purity, and shows a superconducting transition behavior at the temperature of 5.4 K. The growth is carried out by adopting a fluxing agent method, the operation is simple and convenient, the cost is controllable, the method is suitable for large-scale exploration, and a foundation is laid for the development of other potential superconducting phases in a subsequent Zr-Ru-Si ternary system. The invention further discloses a preparation method and application of the Zr-Ru-Si-based ternary superconducting single crystal material and a terminal product.
Owner:BINZHOU WEIQIAO NATIONAL SCIENCE & TECHNOLOGY ADVANCED TECHNOLOGY RESEARCH INSTITUTE

Method for preparing rare earth aluminum-based intermetallic compound EuAl4 single crystal by Al fluxing agent method

The invention discloses a method for preparing a rare earth aluminum-based intermetallic compound EuAl4 single crystal by an Al fluxing agent method. The method comprises the following steps: A, cutting Al particles into small sizes in a glove box; after the Eu piece is subjected to oil removal treatment, the Eu piece is transferred into a glove box to be polished; b, weighing Al particles and Eu sheets in a glove box, and placing the Al particles and the Eu sheets in a No.1 alumina crucible; c, placing a No.1 alumina crucible in a quartz tube, and placing a filter screen above the crucible; d.2, quartz wool is placed in a No.2 alumina crucible, and the No.2 alumina crucible is placed in a quartz tube with an opening facing downwards; e, placing quartz wool above a No.2 alumina crucible, and then placing a quartz column; f, locking the quartz tube by using a tube sealing buckle and then transferring the quartz tube out of the glove box; g, performing vacuum sealing on the quartz tube by using a vacuum tube sealing machine; h, cutting the sealed quartz tube to the upper part of the quartz column by sharp-nose pliers, and putting the quartz tube into a No.3 alumina crucible; i, heating and cooling the No.3 alumina crucible in a box-type furnace; j, after cooling, the quartz tube is turned over and subjected to heat preservation; taking out the quartz tube, centrifuging, opening and cleaning to obtain a final product.
Owner:ZHEJIANG INSTITUTE OF OPTOELECTRONICS

Intrinsic superlattice single crystal material and preparation method thereof

The invention discloses an intrinsic superlattice single crystal material and a preparation method thereof, and belongs to the technical field of single crystal growth. The chemical formula of the single crystal is BaLaMnSb4, and the crystal structure of the single crystal is formed by alternately stacking BaMnSb2 layers and LaSb2 layers in an intrinsic superlattice form in the direction perpendicular to the layers. The novel magnetic topological material BaLaMnSb4 single crystal with the intrinsic superlattice is grown by utilizing a self-fluxing agent method, the single crystal has an intrinsic superlattice structure formed by alternating BaMnSb2 and LaSb2, and the single crystal is high in quality, few in defect and large in size, and is an ideal research platform for the magnetic topological material.
Owner:HEFEI INSTITUTE OF PHYSICAL SCIENCE CHINESE ACADEMY OF SCIENCES

Application of Rb4Li2TiOGe4O12 single crystal in preparation of direct X-ray detector

The invention discloses an application of an Rb4Li2TiOGe4O12 single crystal in preparation of a direct type X-ray detector. According to the preparation method, Rb4Li2TiOGe4O12 single crystals are obtained through growth by a fluxing agent method, then the Rb4Li2TiOGe4O12 single crystals are cut in the normal direction of the upper surface and the lower surface of a wafer by taking the 001 crystal orientation or the 100 crystal orientation of the Rb4Li2TiOGe4O12 single crystals as the normal direction to form the wafer, positive and negative electrodes are formed on the upper surface and the lower surface of the wafer in a sputtering deposition mode, and preparation of the direct type X-ray detector is completed. The preparation process is simple, universal and low in cost, the direct type X-ray detector prepared by taking the Rb4Li2TiOGe4O12 wafer as the raw material can have high detection sensitivity and ultralow detection limit by selecting the proper cutting direction, and meanwhile, the source of the direct type X-ray detector material is widened.
Owner:TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI

Growth method of high-temperature phase lanthanum borosilicate crystal and use

The present disclosure provides a growth method of a high-temperature phase lanthanum borosilicate crystal, where the high-temperature phase lanthanum borosilicate crystal is a β-La1-yLnyBSiO5 crystal prepared by a high-temperature flux method; a composite flux system is (La1-yLny)BO3—LiMoO4—SiO2—B2O3, and (La1-yLny)BO3, LiMoO4, SiO2, and B2O3 in the system have molar percentages of x1, x2, x3, and x4, respectively; 0<x1<0.3, 0.7≤x2<1, 0<x3<0.3, x1+x2+x3=1, x1:x4=2:1 to 4:1. In the present disclosure, a difficulty is overcome in the crystal growth of β-LaBSiO5 due to phase transition. The crystal is an optical function material that does not undergo the phase transition during annealing and can exist stably at room temperature. The crystal is widely used in laser, terahertz, and other fields.
Owner:FUZHOU UNIV

Flux for growing SrB4O7 crystal and application thereof

The invention relates to the technical field of crystal growth, in particular to a fluxing agent for growing SrB4O7 crystals and application of the fluxing agent. According to the invention, by introducing a specific fluxing agent system composed of one or two of Li2O and Sr2V2O7, the growth mode of the SrB4O7 crystal is changed from the traditional melt method growth to the fluxing agent method growth. The fluxing agent is effectively introduced, so that the actual growth temperature of the crystal is greatly reduced. Meanwhile, the fluxing agent system enhances the capability of resisting external tiny temperature disturbance of the melt, so that the crystal growth process can be stably carried out in a wider and easier-to-control temperature range, the harsh requirement on the temperature control precision is greatly reduced, and the stability and repeatability of the process are improved.
Owner:TIANJIN UNIVERSITY OF TECHNOLOGY

Device and method for batch growth of doped gallium nitride single crystals by flux method

The invention discloses a device and a method for batch growth of doped gallium nitride single crystals by a flux method, and belongs to the technical field of crystal material preparation, the device comprises a reaction kettle, a cylindrical groove used for placing a cylindrical central heating unit is formed in the bottom of the reaction kettle, and an annular lining used for containing raw material melt is arranged in the reaction kettle; the annular lining is an annular cavity formed by an inner circular lining wall and an outer circular lining wall, the inner circular lining wall of the annular lining is of a step structure, a seed crystal seat for placing a seed crystal is placed at the bottom of the annular lining, a flow guide cover is arranged outside the seed crystal, and a side wall heating unit is arranged on the outer side wall of the reaction kettle. Through annular two-section type center and outer wall heating control, the consistency of melt mass transfer among a plurality of single crystal sheets and the uniformity of crystal surface solute diffusion are realized, so that a plurality of gallium nitride single crystals with high quality and consistent performance are obtained.
Owner:XI AN JIAOTONG UNIV

Method for growing group 13 element nitride crystal layer, nitride semiconductor ingot, and sputtering target

A 13-group element nitride crystal layer is grown at a high growth rate to obtain a crystal layer having a large thickness. A 13-group element nitride crystal layer is grown on a base substrate including at least a seed layer. The base substrate is immersed in a melt solution including a flux, and a 13-group element nitride crystal layer is grown two-dimensionally on a nitrogen-polar surface of the seed layer by a flux method.
Owner:NGK INSULATORS LTD

Convection frequency difference regulation and control device for growing gallium nitride single crystal by flux method

The invention belongs to the technical field of crystal material preparation, and particularly relates to a convection frequency difference regulation and control device for growing gallium nitride single crystals by a flux method. Comprising a growth cavity, a reaction kettle body is arranged in the growth cavity, seed crystal and single crystal growth melt are arranged in the reaction kettle body, the bottom wall of the reaction kettle body is of a fan-shaped concave-convex structure, at least two ultrasonic convection driving units are evenly and symmetrically arranged on the bottom wall of the reaction kettle body, and each ultrasonic convection driving unit comprises at least two variable-amplitude bases which are evenly and symmetrically arranged in the radial direction of the fan-shaped concave-convex structure; the lower end of each variable-amplitude base is connected with a transmission rod, each transmission rod is connected with a piezoelectric transducer, and all the piezoelectric transducers are connected with an ultrasonic drive control source. According to the invention, the ultrasonic driving control source generates driving electric signals with different frequencies, and the variable amplitude seat applies ultrasonic waves with different frequencies to the reaction kettle body, so that single crystal growth melt forms a pressure difference in an area near the surface of a seed crystal, and the single crystal growth melt is driven to form controllable push-suction type ring convection.
Owner:XI AN JIAOTONG UNIV

Seed crystal inoculation monitoring device for growth of gallium nitride single crystal by flux method

The invention belongs to the technical field of crystal material preparation, and particularly relates to a seed crystal inoculation monitoring device for growth of a flux method gallium nitride single crystal. Comprising a reaction kettle body, the top of the reaction kettle body is provided with a packaging shell layer capable of moving up and down, a convex seed crystal is placed in the packaging shell layer, a convex part of the convex seed crystal penetrates out of the packaging shell layer and faces single crystal growth melt, a concave surface close to the convex part is covered with a coplanar electrode, and the coplanar electrode is located in the packaging shell layer. The coplanar electrode is used for measuring the capacitance change in the contact process of the inoculation area of the convex seed crystal and the single crystal growth melt, positioning the inoculation position of the convex seed crystal on the surface of the melt, measuring the capacitance change of the gallium nitride single crystal growing on the surface after the seed crystal is inoculated, and monitoring the crystallization process of the gallium nitride single crystal. According to the invention, the problem that the seed crystal inoculation process at the top is difficult to observe in the high-temperature and high-pressure closed reaction kettle body can be solved, the seed crystal inoculation position is accurately controlled, and the crystal epitaxial change in the inoculation process is monitored, so that high-quality crystal growth is realized.
Owner:XI AN JIAOTONG UNIV

Metal droplet collection and reflux system for growing nitride single crystal by flux method

The utility model provides a metal droplet collecting and reflowing system for growing nitride single crystals by a fluxing agent method, which is characterized in that a reaction chamber is arranged at the lower part of a furnace body, a reaction container is arranged in the reaction chamber, a heating component is arranged within a certain range from the reaction container, and an air blowing component is arranged at the lower end of the reaction container; the upper end of the reaction chamber is connected with a condenser through a lifting mechanism, a drainage component is arranged at the bottom of the condenser, and the tail end of the drainage component faces the reaction container; an adjusting bracket is arranged in the reaction chamber, a stirring mechanism is arranged on the adjusting bracket, and stirring blades of the stirring mechanism extend into the reaction container; the electric control system is connected with the lifting mechanism, the air blowing assembly, the adjusting support and the stirring mechanism and used for controlling the corresponding mechanisms to act. The device disclosed by the utility model better meets the actual requirements of single crystal growth, can adapt to large-scale and programmed commercialized production, and simultaneously meets the requirements of energy conservation, emission reduction, safety and stability.
Owner:SHANDONG UNIV