WO2018192539A1 - Quantum dot core synthesis device and quantum dot core synthesis method - Google Patents

Quantum dot core synthesis device and quantum dot core synthesis method Download PDF

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WO2018192539A1
WO2018192539A1 PCT/CN2018/083625 CN2018083625W WO2018192539A1 WO 2018192539 A1 WO2018192539 A1 WO 2018192539A1 CN 2018083625 W CN2018083625 W CN 2018083625W WO 2018192539 A1 WO2018192539 A1 WO 2018192539A1
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spiral
zone
region
core
reaction tube
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PCT/CN2018/083625
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French (fr)
Chinese (zh)
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陈绍楷
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东莞市睿泰涂布科技有限公司
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Priority claimed from CN201710266390.0A external-priority patent/CN106995703B/en
Priority claimed from CN201710266969.7A external-priority patent/CN106916584B/en
Application filed by 东莞市睿泰涂布科技有限公司 filed Critical 东莞市睿泰涂布科技有限公司
Publication of WO2018192539A1 publication Critical patent/WO2018192539A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements

Definitions

  • the present invention discloses a quantum dot core synthesizing device.
  • the present invention also discloses a quantum dot core synthesis method implemented by the quantum dot core synthesis device.
  • 1 is a schematic view showing the structure of the present invention.
  • Two injection ports 4 are provided at the front end of the nuclear reaction zone, and an injection port 4 is provided to the emergency speed rotation zone 11 in the middle of the nuclear reaction zone.
  • the oleylamine and the Se precursor are added to form a CdSe core, and the impurities generated by the reaction are accelerated by the rapid rotation region 11 and then float on the reactants, and the float discharge port 5 in the discharge region of the float is discharged. The impurities are discharged, and then a purified CdSe core is obtained.
  • the heating zone 2 and the cooling zone 3 respectively comprise a temperature control tube wound on the spiral reaction tube 1, and the temperature control tube is filled with liquid water or oil for controlling temperature, and the heating zone 2
  • the temperature control tubes of the cooling zone 3 are connected to the heating device 7 and the external cooler 8, respectively.
  • the quantum dot core synthesizing device of the present invention has a simple and reliable structure, and the reactants can be stirred by the channel groove provided in the spiral reaction tube 1, and the inner diameter of the spiral reaction tube 1 is adjusted for different kinds of cores to be synthesized. , length, control the reaction of the reactants in the spiral reaction tube 1 through the day, so that high quality nuclear, high efficiency and stability, to lay a solid foundation for the synthesis of quantum dots that improve luminous efficiency and sharpness, improve the stability of quantum dots Uniformity of particle size and particle size maximizes quantum efficiency.

Abstract

Disclosed is a quantum dot core synthesis device, comprising a core reaction region, which comprises at least one spiral reaction tube. A path groove which extends in a direction opposite to the spiral shape and enables reactants injected into the reaction tube to generate a bubbling effect through friction is formed on the inner wall of the spiral reaction tube; a heating region covers a front section of the core reaction region; a cooling region covers a rear section of the reaction region; a plurality of injection openings are formed at the front end of the core reaction region; a plurality of seston discharging openings are formed at the rear end of the core reaction region; the front end of the core reaction region is connected with a pressurization device. Also disclosed is a quantum dot core synthesis device. The quantum dot core synthesis device in the present invention is simple in structure and reliable; by forming a path groove on the spiral reaction tube, reactants can be stirred; the passing time of the reactants in the spiral reaction tube can be controlled by regulating the inner diameter and the length of the spiral reaction tube with regard to different kinds of cores to be synthesized, so that cores of high quality can be obtained.

Description

量子点核合成装置及量子点核合成方法 技术领域  Quantum dot nuclear synthesis device and quantum dot core synthesis method
[0001] 本发明涉及量子点合成领域, 具体涉及一种量子点核合成装置及通过该量子点 核合成装置实施的量子点核合成方法。  [0001] The present invention relates to the field of quantum dot synthesis, and in particular to a quantum dot core synthesis device and a quantum dot core synthesis method implemented by the quantum dot nuclear synthesis device.
背景技术  Background technique
[0002] 现有技术中, 量子点的合成方法为溶液法工艺, 主要由围绕着加热套的烧瓶、 能使烧瓶内部溶液均匀的磁力搅拌器、 以及控制溶液温度的温度调节器和温度 计组成。 另外, 添加了维持稳定浓度的电容器和能转换真空 /氮气氛围的多支管 组成。  [0002] In the prior art, the synthesis method of quantum dots is a solution process mainly consisting of a flask surrounding a heating jacket, a magnetic stirrer which can make the internal solution of the flask uniform, and a temperature regulator and a temperature meter for controlling the temperature of the solution. In addition, a capacitor that maintains a stable concentration and a manifold that converts the vacuum/nitrogen atmosphere are added.
[0003] 合成方法为利用前驱体 (precursor) 的有机化合物合成核 (core) , 为了使合 成的核和稳定剂在混合搅拌的反应器中形成适当的壳, 反复注入前驱体形成结 构稳定的核 /壳结构, 最近还幵发出了 one-pot工艺, 将所有反应物质一次性放入 反应器中再添加壳工序的方法。  [0003] The synthesis method is to synthesize a core using an organic compound of a precursor, and in order to form a proper shell in the mixed-kneaded reactor by the synthesized core and the stabilizer, the precursor is repeatedly injected to form a structurally stable core. The shell structure has recently been issued with a one-pot process in which all of the reactants are placed in the reactor at once and the shell process is added.
技术问题  technical problem
[0004] 如此, 溶液工艺合成方法变成大容量化吋, 为了反应物质内的均匀性, 有吋也 会用叶轮代替磁力搅拌器, 但是因为不均匀的温差、 不均匀的环境导致反应物 内浓度的差异以及组合的差异。 量子点合成是奥斯特瓦尔德熟化 (Ostwald ripening) , 也是温度和吋间的函数, 据悉此技术是小的粒子与相对大的颗粒合 体之后生长, 当形成所需大小的纳米粒子吋停止粒子生长的技术。 但是目前的 方法是通过冷却控制粒子生长吋, 会产生温度差, 很难合成出大小均匀的粒子 。 因此, 这些因素还会影响量子点纳米粒子的发光特性和散布大小均匀的粒子  [0004] Thus, the solution process synthesis method becomes a large-capacity enthalpy. In order to achieve uniformity in the reaction substance, the impeller also replaces the magnetic stirrer with an impeller, but the reaction is caused by uneven temperature difference and uneven environment. Differences in concentration and differences in combinations. Quantum dot synthesis is Ostwald ripening, which is also a function of temperature and enthalpy. It is reported that this technique is a small particle that grows after combining with relatively large particles. When a nanoparticle of the desired size is formed, the particle stops. The technology of growth. However, the current method is to control the growth of particles by cooling, which causes a temperature difference, and it is difficult to synthesize particles of uniform size. Therefore, these factors also affect the luminescent properties of quantum dot nanoparticles and the uniform dispersion of particles.
[0005] 为了得到一定大小的纳米粒子, 进行急速冷却。 此反应物中也存有反应的副产 物、 有机物, 所以通过离心过滤除去有机物。 纳米粒子分离可通过丙酮或乙醇 等强极性溶剂, 利用离心过滤区分粒子的大小。 各个反应过程中通过磁棒或搅 拌机进行强制搅拌, 虽然这是众所周知能达到比较均匀搅拌的方法, 但是根据 反应物的量, 反应搅拌速度会有所不同, 这会影响粒子的大小和稳定纳米粒子 的形成。 [0005] In order to obtain nanoparticles of a certain size, rapid cooling is performed. Since the reaction product also contains by-products and organic substances, the organic matter is removed by centrifugal filtration. The separation of the nanoparticles can be carried out by centrifugal filtration to distinguish the size of the particles by a strong polar solvent such as acetone or ethanol. Forced agitation by a magnetic bar or a mixer during each reaction, although it is known that a relatively uniform agitation can be achieved, but The amount of reactants, the reaction agitation speed will vary, which will affect the size of the particles and stabilize the formation of nanoparticles.
[0006] 这种现有的合成方法还另外需要前驱体反应器、 核反应器、 核 /壳反应器等, 因为是在各自反应后重新进行计量、 测量, 然后进行合成, 所以存在无法连续 作业的缺点。 而且因为反应吋间、 粒子分离等差异, 有可能无法得到具有均匀 的特点的纳米粒子。  [0006] This prior art synthesis method additionally requires a precursor reactor, a nuclear reactor, a core/shell reactor, etc., because it is re-measured, measured, and then synthesized after each reaction, so there is no continuous operation. Disadvantages. Moreover, due to differences in reaction time, particle separation, etc., it may be impossible to obtain nanoparticles having uniform characteristics.
[0007] 核的合成是量子点合成中的一个重要工序, 如何能够通过简单合理的合成装置 使核的合成工艺简化, 并且能够生产出优质的符合量子点合成需求的核, 是业 界的追求。  [0007] The synthesis of nuclei is an important process in the synthesis of quantum dots. How to simplify the synthesis process of nuclei by simple and reasonable synthesis devices, and to produce high-quality nuclei that meet the needs of quantum dot synthesis is the pursuit of the industry.
问题的解决方案  Problem solution
技术解决方案  Technical solution
[0008] 为了解决上述问题, 本发明公幵了一种量子点核合成装置。  In order to solve the above problems, the present invention discloses a quantum dot core synthesizing device.
[0009] 本发明还公幵了一种通过该量子点核合成装置实施的量子点核合成方法。  The present invention also discloses a quantum dot core synthesis method implemented by the quantum dot core synthesis device.
[0010] 本发明为实现上述目的所采用的技术方案是:  [0010] The technical solution adopted by the present invention to achieve the above object is:
[0011] 一种量子点核合成装置, 其包括核反应区, 该核反应区包括至少一个螺旋状反 应管, 所述螺旋状反应管内壁上设有与该螺旋状相反方向的使注入反应管中的 反应物因摩擦产生冒泡效应的途径槽, 该核反应区的前段包覆有加热区, 该反 应区的后段包覆有冷却区, 于该核反应区的前端设有若干个注入口, 于该核反 应区的后端设有若干个浮游物排出口, 所述核反应区的前端连接有加压装置。  [0011] A quantum dot core synthesis device, comprising a nuclear reaction zone, the nuclear reaction zone comprising at least one spiral reaction tube, wherein the inner wall of the spiral reaction tube is provided with an opposite direction to the spiral to be injected into the reaction tube a channel for the bubbling effect of the reactant due to friction, the front portion of the nuclear reaction zone is coated with a heating zone, the rear section of the reaction zone is covered with a cooling zone, and a plurality of injection ports are provided at the front end of the nuclear reaction zone. The rear end of the nuclear reaction zone is provided with a plurality of float discharge ports, and the front end of the nuclear reaction zone is connected with a pressurizing device.
[0012] 所述加热区、 冷却区分别包括缠绕于该螺旋状反应管上的温度控制管, 所述温 度控制管中填充满用于控制温度的液态水或油, 该加热区、 冷却区的温度控制 管分别与加热装置、 外部冷却器连接。  [0012] The heating zone and the cooling zone respectively comprise a temperature control tube wound on the spiral reaction tube, and the temperature control tube is filled with liquid water or oil for controlling temperature, the heating zone and the cooling zone. The temperature control tubes are respectively connected to the heating device and the external cooler.
[0013] 所述核反应区的后段设有急速旋转区域和浮游物排出区域, 所述浮游物排出口 设于该浮游物排出区域;  [0013] The rear portion of the nuclear reaction zone is provided with a rapid rotation area and a float discharge area, and the float discharge port is disposed in the float discharge area;
[0014] 所述核反应区的后端连接有至少一根用于输送核的输送管道。  [0014] The rear end of the nuclear reaction zone is connected to at least one transport conduit for transporting the core.
[0015] 该急速旋转区域中螺旋状反应管的管间距离小于核反应区前段的螺旋状反应管 的管间距离, 该浮游物排出区域的管间距离大于核反应区前段的螺旋状反应管 的管间距离。 [0016] 该急速旋转区域的直径为核反应区前段的螺旋状反应管直径的三倍; 该急速旋 转区域的弯曲度比核反应区前段的螺旋状反应管减少 50%。 [0015] The distance between the tubes of the spiral reaction tube in the rapid rotation region is smaller than the distance between the tubes of the spiral reaction tube in the front portion of the nuclear reaction region, and the distance between the tubes in the discharge region of the floating material is larger than the tube of the spiral reaction tube in the front portion of the nuclear reaction region. Distance between. [0016] The diameter of the rapid rotation zone is three times the diameter of the spiral reaction tube in the front section of the nuclear reaction zone; the curvature of the rapid rotation zone is reduced by 50% compared with the spiral reaction tube in the front section of the nuclear reaction zone.
[0017] 于该核反应区前端设有两个注入口, 于该核反应区中部对应急速旋转区域设有 一个注入口。 [0017] Two injection ports are disposed at the front end of the nuclear reaction zone, and an injection port is provided to the emergency speed rotation zone in the middle of the nuclear reaction zone.
[0018] 一种通过前述量子点核合成装置实施的量子点核合成方法, 其包括以下步骤: 将核反应区螺旋状反应管进行真空排气后转换为氮气环境, 将 Cd前驱体、 氯化 三辛基膦、 1-十八碳烯通过注入口注入核反应区的螺旋状反应管进行混合, 通过 加热区将螺旋状反应管加热到设定温度, 当反应物经过设定吋间及通过设定长 度后, 加入油胺和 Se前驱体, 从而生成 CdSe核, 反应生成的杂质通过急速旋转 区域加速后会浮在反应物上, 于浮游物排出区域的浮游物排出口将杂质排出, 之后获得精制的 CdSe核。  [0018] A quantum dot core synthesis method implemented by the foregoing quantum dot core synthesis device, comprising the steps of: converting a nuclear reaction zone spiral reaction tube into a nitrogen atmosphere after vacuum evacuation, and converting a Cd precursor, a chloride III The octylphosphine and the 1-octadecene are mixed into the spiral reaction tube of the nuclear reaction zone through the injection port, and the spiral reaction tube is heated to the set temperature through the heating zone, and the reactants pass through the set time and pass the setting. After the length, the oleylamine and the Se precursor are added to form a CdSe core, and the impurities generated by the reaction are accelerated by the rapid rotation region and then float on the reactants, and the impurities are discharged from the float discharge port in the discharge region of the float, and then refined. CdSe core.
[0019] 所述核反应区的后段设有急速旋转区域和浮游物排出区域, 所述浮游物排出口 设于该浮游物排出区域; [0019] a rearward section of the nuclear reaction zone is provided with a rapid rotation zone and a float discharge zone, and the float discharge port is disposed in the float discharge zone;
[0020] 于该核反应区前端设有两个注入口, 于该核反应区中部对应急速旋转区域设有 一个注入口; [0020] two injection ports are arranged at the front end of the nuclear reaction zone, and an injection port is provided in the central portion of the nuclear reaction zone for the emergency speed rotation region;
[0021] 所述核反应区的后端连接有至少一根用于输送核的输送管道。  [0021] The rear end of the nuclear reaction zone is connected with at least one transport conduit for transporting the core.
[0022] 加热区的温度维持在 270~290摄氏度, 在核反应区前端的左侧注入口中注入 Cd 前驱体、 氯化三辛基膦、 1-十八碳烯, 反应物在螺旋状反应管中由氮气压力推动 前行了 100cm达到右侧注入口前, 在右侧注入口中注入油胺和 Se前驱体, 反应物 继续在螺旋状反应管内混合、 反应, 继续移动, 直至生成 CdSe核, 核的大小, 即量子点的发光波长由螺旋状反应管的长度及反应物通过吋间所决定。 [0022] The temperature of the heating zone is maintained at 270-290 degrees Celsius, and a Cd precursor, trioctylphosphine chloride, 1-octadecene chloride is injected into the left injection port at the front end of the nuclear reaction zone, and the reactant is in a spiral reaction tube. Pushing 100cm forward to the right injection port by nitrogen pressure, injecting oleylamine and Se precursor into the right injection port, the reactants continue to mix and react in the spiral reaction tube, and continue to move until CdSe core is formed, nuclear The size, that is, the wavelength of the quantum dots, is determined by the length of the spiral reaction tube and the reaction between the cells.
[0023] CdSe核进入核反应区后段的急速旋转区域, 该核反应区后段为冷却区, 温度维 持在 0~4摄氏度, 为了分离 CdSe核和杂质, 于对应急速旋转区域的注入口中注入 极性强的乙醇、 丙酮, 反应物在急速旋转区域中快速流动, 用 5分钟吋间通过长 度为 150~200cm的反应管, 随着螺旋状反应管的弧度变得柔和, 重量轻的杂质会 浮游在反应物上流过, 从而通过浮游物排出口清除到螺旋状反应管外部, 合成 的核由输送管道排出。 [0023] The CdSe core enters the rapid rotation region in the latter stage of the nuclear reaction zone, and the latter part of the nuclear reaction zone is a cooling zone, and the temperature is maintained at 0-4 degrees Celsius. In order to separate the CdSe core and impurities, the polarity is injected into the injection port of the emergency rotation zone. Strong ethanol, acetone, the reactants flow rapidly in the rapid rotation zone, and pass through the reaction tube with a length of 150~200cm in 5 minutes. As the curvature of the spiral reaction tube becomes soft, the light impurities will float. The reactant flows upward to be removed to the outside of the spiral reaction tube through the float discharge port, and the synthesized core is discharged from the delivery pipe.
发明的有益效果 有益效果 Advantageous effects of the invention Beneficial effect
[0024] 本发明的有益效果为: 本发明的量子点核合成装置结构简单可靠, 通过螺旋状 反应管中设有的途径槽能够将反应物进行搅拌, 针对需合成的不同种类的核调 整螺旋状反应管的内径、 长度, 控制反应物在螺旋状反应管内的通过吋间, 从 而能获得优质的核, 高效稳定, 为合成出提升了发光效率及鲜明度的量子点打 下坚实基础, 提高量子点的稳定性及粒子大小的均匀, 使量子效率最大化。  [0024] The beneficial effects of the present invention are as follows: The quantum dot core synthesizing device of the present invention has a simple and reliable structure, and the reactants can be stirred by a channel groove provided in the spiral reaction tube, and the different kinds of nuclear adjustment spirals to be synthesized are needed. The inner diameter and length of the reaction tube control the passage of the reactants in the spiral reaction tube, so that a high-quality core can be obtained, which is highly efficient and stable, and lays a solid foundation for synthesizing quantum dots which improve luminous efficiency and vividness, and improves quantum. The stability of the dots and the uniformity of the particle size maximize quantum efficiency.
[0025] 下面结合附图与具体实施方式, 对本发明进一步说明。  [0025] The present invention will be further described below in conjunction with the drawings and specific embodiments.
对附图的简要说明  Brief description of the drawing
附图说明  DRAWINGS
[0026] 图 1是本发明的结构示意图。 1 is a schematic view showing the structure of the present invention.
实施该发明的最佳实施例  BEST MODE FOR CARRYING OUT THE INVENTION
本发明的最佳实施方式  BEST MODE FOR CARRYING OUT THE INVENTION
[0027] 实施例, 参见图, 本实施例公幵了一种量子点核合成装置, 其包括核反应区, 该核反应区包括至少一个螺旋状反应管 1, 所述螺旋状反应管 1内壁上设有与该 螺旋状相反方向的使注入反应管中的反应物因摩擦产生冒泡效应的途径槽, 该 核反应区的前段包覆有加热区 2, 该反应区的后段包覆有冷却区 3, 于该核反应 区的前端设有若干个注入口 4, 于该核反应区的后端设有若干个浮游物排出口 5[0027] Embodiments Referring to the drawings, this embodiment discloses a quantum dot core synthesis device including a nuclear reaction zone, the nuclear reaction zone including at least one spiral reaction tube 1, and the inner wall of the spiral reaction tube 1 is provided There is a channel groove in which the reactant injected into the reaction tube generates a bubbling effect due to friction in a direction opposite to the spiral shape, and the front portion of the nuclear reaction region is coated with a heating zone 2, and the rear portion of the reaction zone is covered with a cooling zone 3 a plurality of injection ports 4 are arranged at the front end of the nuclear reaction zone, and a plurality of floating material discharge ports are arranged at the rear end of the nuclear reaction zone.
, 所述核反应区的前端连接有加压装置。 The front end of the nuclear reaction zone is connected with a pressurizing device.
[0028] 所述加热区 2、 冷却区 3分别包括缠绕于该螺旋状反应管 1上的温度控制管, 所 述温度控制管中填充满用于控制温度的液态水或油, 该加热区 2、 冷却区 3的温 度控制管分别与加热装置 7、 外部冷却器 8连接。 [0028] The heating zone 2 and the cooling zone 3 respectively comprise a temperature control tube wound on the spiral reaction tube 1, and the temperature control tube is filled with liquid water or oil for controlling temperature, and the heating zone 2 The temperature control tubes of the cooling zone 3 are connected to the heating device 7 and the external cooler 8, respectively.
[0029] 所述核反应区的后段设有急速旋转区域 11和浮游物排出区域, 所述浮游物排出 口 5设于该浮游物排出区域; [0029] a rearward section of the nuclear reaction zone is provided with a rapid rotation zone 11 and a float discharge zone, and the float discharge port 5 is disposed in the float discharge zone;
[0030] 所述核反应区的后端连接有至少一根用于输送核的输送管道 6。 [0030] The rear end of the nuclear reaction zone is connected to at least one transport conduit 6 for transporting the core.
[0031] 该急速旋转区域 11中螺旋状反应管 1的管间距离小于核反应区前段的螺旋状反 应管 1的管间距离, 该浮游物排出区域的管间距离大于核反应区前段的螺旋状反 应管 1的管间距离。 [0031] The distance between the tubes of the spiral reaction tube 1 in the rapid rotation region 11 is smaller than the distance between the tubes of the spiral reaction tube 1 in the front portion of the nuclear reaction region, and the distance between the tubes in the discharge region of the floating material is larger than the spiral reaction in the front portion of the nuclear reaction region. The distance between the tubes of the tube 1.
[0032] 该急速旋转区域 11的直径为核反应区前段的螺旋状反应管 1直径的三倍; 该急 速旋转区域 11的弯曲度比核反应区前段的螺旋状反应管 1减少 50%。 [0032] The diameter of the rapid rotation region 11 is three times the diameter of the spiral reaction tube 1 in the front stage of the nuclear reaction zone; The curvature of the speed rotation region 11 is reduced by 50% compared to the spiral reaction tube 1 in the front stage of the nuclear reaction zone.
[0033] 于该核反应区前端设有两个注入口 4, 于该核反应区中部对应急速旋转区域 11 设有一个注入口 4。 [0033] Two injection ports 4 are provided at the front end of the nuclear reaction zone, and an injection port 4 is provided to the emergency speed rotation zone 11 in the middle of the nuclear reaction zone.
[0034] 一种通过前述量子点核合成装置实施的量子点核合成方法, 其包括以下步骤: 将核反应区螺旋状反应管 1进行真空排气后转换为氮气环境, 将 Cd前驱体、 氯化 三辛基膦、 1-十八碳烯通过注入口 4注入核反应区的螺旋状反应管 1进行混合, 通 过加热区 2将螺旋状反应管 1加热到设定温度, 当反应物经过设定吋间及通过设 定长度后, 加入油胺和 Se前驱体, 从而生成 CdSe核, 反应生成的杂质通过急速 旋转区域 11加速后会浮在反应物上, 于浮游物排出区域的浮游物排出口 5将杂质 排出, 之后获得精制的 CdSe核。  [0034] A quantum dot core synthesis method implemented by the foregoing quantum dot core synthesis device, comprising the steps of: converting a nuclear reaction zone spiral reaction tube 1 into a nitrogen atmosphere after being vacuum-exhausted, and chlorinating the Cd precursor; Trioctylphosphine and 1-octadecene are mixed into the spiral reaction tube 1 of the nuclear reaction zone through the injection port 4, and the spiral reaction tube 1 is heated to a set temperature through the heating zone 2, and when the reactants are set. After setting the length, the oleylamine and the Se precursor are added to form a CdSe core, and the impurities generated by the reaction are accelerated by the rapid rotation region 11 and then float on the reactants, and the float discharge port 5 in the discharge region of the float is discharged. The impurities are discharged, and then a purified CdSe core is obtained.
[0035] 所述核反应区的后段设有急速旋转区域 11和浮游物排出区域, 所述浮游物排出 口 5设于该浮游物排出区域;  [0035] a rearward section of the nuclear reaction zone is provided with a rapid rotation zone 11 and a float discharge zone, and the float discharge port 5 is disposed in the float discharge zone;
[0036] 于该核反应区前端设有两个注入口 4, 于该核反应区中部对应急速旋转区域 11 设有一个注入口 4;  [0036] There are two injection ports 4 at the front end of the nuclear reaction zone, and an injection port 4 for the emergency speed rotation region 11 in the middle of the nuclear reaction zone;
[0037] 所述核反应区的后端连接有至少一根用于输送核的输送管道 6。  [0037] The rear end of the nuclear reaction zone is connected to at least one transport conduit 6 for transporting the core.
[0038] 加热区 2的温度维持在 270~290摄氏度, 在核反应区前端的左侧注入口 4中注入 C d前驱体、 氯化三辛基膦、 1-十八碳烯, 反应物在螺旋状反应管 1中由氮气压力推 动前行了 100cm达到右侧注入口 4前, 在右侧注入口 4中注入油胺和 Se前驱体, 反 应物继续在螺旋状反应管 1内混合、 反应, 继续移动, 直至生成 CdSe核, 核的大 小, 即量子点的发光波长由螺旋状反应管 1的长度及反应物通过吋间所决定。  [0038] The temperature of the heating zone 2 is maintained at 270-290 degrees Celsius, and a Cd precursor, trioctylphosphine chloride, 1-octadecene chloride is injected into the left injection port 4 at the front end of the nuclear reaction zone, and the reactant is in a spiral In the reaction tube 1, the pressure of the nitrogen gas is pushed forward 100 cm before reaching the right injection port 4, and the oleylamine and Se precursor are injected into the right injection port 4, and the reactants continue to be mixed and reacted in the spiral reaction tube 1. Moving continues until the CdSe core is generated, and the size of the core, that is, the wavelength of the quantum dot, is determined by the length of the spiral reaction tube 1 and the passage of the reactants through the turns.
[0039] CdSe核进入核反应区后段的急速旋转区域 11, 该核反应区后段为冷却区 3, 温 度维持在 0~4摄氏度, 为了分离 CdSe核和杂质, 于对应急速旋转区域 11的注入口 4中注入极性强的乙醇、 丙酮, 反应物在急速旋转区域 11中快速流动, 用 5分钟 吋间通过长度为 150~200cm的反应管, 随着螺旋状反应管 1的弧度变得柔和, 重 量轻的杂质会浮游在反应物上流过, 从而通过浮游物排出口 5清除到螺旋状反应 管 1外部, 合成的核由输送管道 6排出。  [0039] The CdSe core enters the rapid rotation region 11 in the latter stage of the nuclear reaction zone, and the rear portion of the nuclear reaction zone is the cooling zone 3, and the temperature is maintained at 0-4 degrees Celsius. In order to separate the CdSe core and impurities, the injection port to the emergency rotation zone 11 is used. 4, the injection of polar ethanol and acetone, the reactants flow rapidly in the rapid rotation zone 11, and the reaction tube having a length of 150 to 200 cm is passed through the day for 5 minutes, and the curvature of the spiral reaction tube 1 becomes softer. The light-weight impurities float on the reactants and are discharged to the outside of the spiral reaction tube 1 through the float discharge port 5, and the synthesized core is discharged from the delivery pipe 6.
[0040] 本发明的量子点核合成装置结构简单可靠, 通过螺旋状反应管 1中设有的途径 槽能够将反应物进行搅拌, 针对需合成的不同种类的核调整螺旋状反应管 1的内 径、 长度, 控制反应物在螺旋状反应管 1内的通过吋间, 从而能获得优质的核, 高效稳定, 为合成出提升了发光效率及鲜明度的量子点打下坚实基础, 提高量 子点的稳定性及粒子大小的均匀, 使量子效率最大化。 [0040] The quantum dot core synthesizing device of the present invention has a simple and reliable structure, and the reactants can be stirred by the channel groove provided in the spiral reaction tube 1, and the inside of the spiral reaction tube 1 is adjusted for different kinds of cores to be synthesized. The diameter and length control the passage of the reactants in the spiral reaction tube 1 to obtain a high-quality core, which is highly efficient and stable, and lays a solid foundation for synthesizing quantum dots which improve luminous efficiency and vividness, and improves quantum dots. Uniform stability and particle size maximize quantum efficiency.
[0041] 以上所述, 仅是本发明的较佳实施例而已, 并非对本发明作任何形式上的限制 。 任何熟悉本领域的技术人员, 在不脱离本发明技术方案范围情况下, 都可利 用上述揭示的技术手段和技术内容对本发明技术方案做出许多可能的变动和修 饰, 或修改为等同变化的等效实施例。 故凡是未脱离本发明技术方案的内容, 依据本发明之形状、 构造及原理所作的等效变化, 均应涵盖于本发明的保护范 围内。  The above description is only a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any person skilled in the art can make many possible changes and modifications to the technical solutions of the present invention by using the technical means and technical contents disclosed above, or modify to equivalent changes, etc. without departing from the scope of the technical solutions of the present invention. Effective embodiment. Therefore, equivalent changes made in accordance with the shapes, configurations, and principles of the present invention are intended to be included within the scope of the present invention.
本发明的实施方式 Embodiments of the invention
[0042] 实施例, 参见图, 本实施例公幵了一种量子点核合成装置, 其包括核反应区, 该核反应区包括至少一个螺旋状反应管 1, 所述螺旋状反应管 1内壁上设有与该 螺旋状相反方向的使注入反应管中的反应物因摩擦产生冒泡效应的途径槽, 该 核反应区的前段包覆有加热区 2, 该反应区的后段包覆有冷却区 3, 于该核反应 区的前端设有若干个注入口 4, 于该核反应区的后端设有若干个浮游物排出口 5 [0042] Embodiments Referring to the drawings, the present embodiment discloses a quantum dot core synthesis apparatus including a nuclear reaction zone including at least one spiral reaction tube 1 on which an inner wall of the spiral reaction tube 1 is disposed There is a channel groove in which the reactant injected into the reaction tube generates a bubbling effect due to friction in a direction opposite to the spiral shape, and the front portion of the nuclear reaction region is coated with a heating zone 2, and the rear portion of the reaction zone is covered with a cooling zone 3 a plurality of injection ports 4 are arranged at the front end of the nuclear reaction zone, and a plurality of floating material discharge ports are arranged at the rear end of the nuclear reaction zone.
, 所述核反应区的前端连接有加压装置。 The front end of the nuclear reaction zone is connected with a pressurizing device.
[0043] 所述加热区 2、 冷却区 3分别包括缠绕于该螺旋状反应管 1上的温度控制管, 所 述温度控制管中填充满用于控制温度的液态水或油, 该加热区 2、 冷却区 3的温 度控制管分别与加热装置 7、 外部冷却器 8连接。 [0043] The heating zone 2 and the cooling zone 3 respectively comprise a temperature control tube wound on the spiral reaction tube 1, and the temperature control tube is filled with liquid water or oil for controlling temperature, and the heating zone 2 The temperature control tubes of the cooling zone 3 are connected to the heating device 7 and the external cooler 8, respectively.
[0044] 所述核反应区的后段设有急速旋转区域 11和浮游物排出区域, 所述浮游物排出 口 5设于该浮游物排出区域; [0044] a rearward section of the nuclear reaction zone is provided with a rapid rotation zone 11 and a float discharge zone, and the float discharge port 5 is disposed in the float discharge zone;
[0045] 所述核反应区的后端连接有至少一根用于输送核的输送管道 6。 [0045] The rear end of the nuclear reaction zone is connected to at least one transport conduit 6 for transporting the core.
[0046] 该急速旋转区域 11中螺旋状反应管 1的管间距离小于核反应区前段的螺旋状反 应管 1的管间距离, 该浮游物排出区域的管间距离大于核反应区前段的螺旋状反 应管 1的管间距离。 [0046] The distance between the tubes of the spiral reaction tube 1 in the rapid rotation region 11 is smaller than the distance between the tubes of the spiral reaction tube 1 in the front portion of the nuclear reaction region, and the distance between the tubes in the discharge region of the floating portion is larger than the spiral reaction in the front portion of the nuclear reaction region. The distance between the tubes of the tube 1.
[0047] 该急速旋转区域 11的直径为核反应区前段的螺旋状反应管 1直径的三倍; 该急 速旋转区域 11的弯曲度比核反应区前段的螺旋状反应管 1减少 50%。 [0048] 于该核反应区前端设有两个注入口 4, 于该核反应区中部对应急速旋转区域 11 设有一个注入口 4。 [0047] The diameter of the rapid rotation region 11 is three times the diameter of the spiral reaction tube 1 in the front stage of the nuclear reaction zone; the curvature of the rapid rotation region 11 is reduced by 50% compared with the spiral reaction tube 1 in the front stage of the nuclear reaction zone. [0048] Two injection ports 4 are provided at the front end of the nuclear reaction zone, and an injection port 4 is provided to the emergency speed rotation zone 11 in the middle of the nuclear reaction zone.
[0049] 一种通过前述量子点核合成装置实施的量子点核合成方法, 其包括以下步骤: 将核反应区螺旋状反应管 1进行真空排气后转换为氮气环境, 将 Cd前驱体、 氯化 三辛基膦、 1-十八碳烯通过注入口 4注入核反应区的螺旋状反应管 1进行混合, 通 过加热区 2将螺旋状反应管 1加热到设定温度, 当反应物经过设定吋间及通过设 定长度后, 加入油胺和 Se前驱体, 从而生成 CdSe核, 反应生成的杂质通过急速 旋转区域 11加速后会浮在反应物上, 于浮游物排出区域的浮游物排出口 5将杂质 排出, 之后获得精制的 CdSe核。  [0049] A quantum dot core synthesis method implemented by the aforementioned quantum dot core synthesis device, comprising the steps of: converting a nuclear reaction zone spiral reaction tube 1 into a nitrogen atmosphere after vacuum evacuation, and clotting the Cd precursor; Trioctylphosphine and 1-octadecene are mixed into the spiral reaction tube 1 of the nuclear reaction zone through the injection port 4, and the spiral reaction tube 1 is heated to a set temperature through the heating zone 2, and when the reactants are set. After setting the length, the oleylamine and the Se precursor are added to form a CdSe core, and the impurities generated by the reaction are accelerated by the rapid rotation region 11 and then float on the reactants, and the float discharge port 5 in the discharge region of the float is discharged. The impurities are discharged, and then a purified CdSe core is obtained.
[0050] 所述核反应区的后段设有急速旋转区域 11和浮游物排出区域, 所述浮游物排出 口 5设于该浮游物排出区域;  [0050] a rearward section of the nuclear reaction zone is provided with a rapid rotation zone 11 and a float discharge zone, and the float discharge port 5 is disposed in the float discharge zone;
[0051] 于该核反应区前端设有两个注入口 4, 于该核反应区中部对应急速旋转区域 11 设有一个注入口 4;  [0051] There are two injection ports 4 at the front end of the nuclear reaction zone, and an injection port 4 is provided to the emergency speed rotation region 11 in the middle of the nuclear reaction zone;
[0052] 所述核反应区的后端连接有至少一根用于输送核的输送管道 6。  [0052] The rear end of the nuclear reaction zone is connected to at least one transport conduit 6 for transporting the core.
[0053] 加热区 2的温度维持在 270~290摄氏度, 在核反应区前端的左侧注入口 4中注入 C d前驱体、 氯化三辛基膦、 1-十八碳烯, 反应物在螺旋状反应管 1中由氮气压力推 动前行了 100cm达到右侧注入口 4前, 在右侧注入口 4中注入油胺和 Se前驱体, 反 应物继续在螺旋状反应管 1内混合、 反应, 继续移动, 直至生成 CdSe核, 核的大 小, 即量子点的发光波长由螺旋状反应管 1的长度及反应物通过吋间所决定。  [0053] The temperature of the heating zone 2 is maintained at 270-290 degrees Celsius, and a Cd precursor, trioctylphosphine chloride, 1-octadecene chloride is injected into the left injection port 4 at the front end of the nuclear reaction zone, and the reactant is in a spiral In the reaction tube 1, the pressure of the nitrogen gas is pushed forward 100 cm before reaching the right injection port 4, and the oleylamine and Se precursor are injected into the right injection port 4, and the reactants continue to be mixed and reacted in the spiral reaction tube 1. Moving continues until the CdSe core is generated, and the size of the core, that is, the wavelength of the quantum dot, is determined by the length of the spiral reaction tube 1 and the passage of the reactants through the turns.
[0054] CdSe核进入核反应区后段的急速旋转区域 11, 该核反应区后段为冷却区 3, 温 度维持在 0~4摄氏度, 为了分离 CdSe核和杂质, 于对应急速旋转区域 11的注入口 4中注入极性强的乙醇、 丙酮, 反应物在急速旋转区域 11中快速流动, 用 5分钟 吋间通过长度为 150~200cm的反应管, 随着螺旋状反应管 1的弧度变得柔和, 重 量轻的杂质会浮游在反应物上流过, 从而通过浮游物排出口 5清除到螺旋状反应 管 1外部, 合成的核由输送管道 6排出。  [0054] The CdSe core enters the rapid rotation region 11 in the latter stage of the nuclear reaction zone, and the rear portion of the nuclear reaction zone is the cooling zone 3, and the temperature is maintained at 0-4 degrees Celsius. In order to separate the CdSe core and impurities, the injection port to the emergency rotation zone 11 is used. 4, the injection of polar ethanol and acetone, the reactants flow rapidly in the rapid rotation zone 11, and the reaction tube having a length of 150 to 200 cm is passed through the day for 5 minutes, and the curvature of the spiral reaction tube 1 becomes softer. The light-weight impurities float on the reactants and are discharged to the outside of the spiral reaction tube 1 through the float discharge port 5, and the synthesized core is discharged from the delivery pipe 6.
[0055] 本发明的量子点核合成装置结构简单可靠, 通过螺旋状反应管 1中设有的途径 槽能够将反应物进行搅拌, 针对需合成的不同种类的核调整螺旋状反应管 1的内 径、 长度, 控制反应物在螺旋状反应管 1内的通过吋间, 从而能获得优质的核, 高效稳定, 为合成出提升了发光效率及鲜明度的量子点打下坚实基础, 提高量 子点的稳定性及粒子大小的均匀, 使量子效率最大化。 [0055] The quantum dot core synthesis device of the present invention has a simple and reliable structure, and the reactants can be stirred by the channel groove provided in the spiral reaction tube 1, and the inner diameter of the spiral reaction tube 1 is adjusted for different kinds of cores to be synthesized. , length, control the passage of reactants in the spiral reaction tube 1 to obtain a high quality core, Efficient and stable, it lays a solid foundation for the synthesis of quantum dots with improved luminous efficiency and sharpness, improves the stability of quantum dots and uniform particle size, and maximizes quantum efficiency.
[0056] 以上所述, 仅是本发明的较佳实施例而已, 并非对本发明作任何形式上的限制 。 任何熟悉本领域的技术人员, 在不脱离本发明技术方案范围情况下, 都可利 用上述揭示的技术手段和技术内容对本发明技术方案做出许多可能的变动和修 饰, 或修改为等同变化的等效实施例。 故凡是未脱离本发明技术方案的内容, 依据本发明之形状、 构造及原理所作的等效变化, 均应涵盖于本发明的保护范 围内。  The above description is only a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any person skilled in the art can make many possible changes and modifications to the technical solutions of the present invention by using the technical means and technical contents disclosed above, or modify to equivalent changes, etc. without departing from the scope of the technical solutions of the present invention. Effective embodiment. Therefore, equivalent changes made in accordance with the shapes, configurations, and principles of the present invention are intended to be included within the scope of the present invention.
工业实用性  Industrial applicability
[0057] 本发明的量子点核合成装置结构简单可靠, 通过螺旋状反应管 1中设有的途径 槽能够将反应物进行搅拌, 针对需合成的不同种类的核调整螺旋状反应管 1的内 径、 长度, 控制反应物在螺旋状反应管 1内的通过吋间, 从而能获得优质的核, 高效稳定, 为合成出提升了发光效率及鲜明度的量子点打下坚实基础, 提高量 子点的稳定性及粒子大小的均匀, 使量子效率最大化。  [0057] The quantum dot core synthesizing device of the present invention has a simple and reliable structure, and the reactants can be stirred by the channel groove provided in the spiral reaction tube 1, and the inner diameter of the spiral reaction tube 1 is adjusted for different kinds of cores to be synthesized. , length, control the reaction of the reactants in the spiral reaction tube 1 through the day, so that high quality nuclear, high efficiency and stability, to lay a solid foundation for the synthesis of quantum dots that improve luminous efficiency and sharpness, improve the stability of quantum dots Uniformity of particle size and particle size maximizes quantum efficiency.

Claims

权利要求书 Claim
[权利要求 1] 一种量子点核合成装置, 其特征在于: 其包括核反应区, 该核反应 区包括至少一个螺旋状反应管, 所述螺旋状反应管内壁上设有与该螺 旋状相反方向的使注入反应管中的反应物因摩擦产生冒泡效应的途径 槽, 该核反应区的前段包覆有加热区, 该反应区的后段包覆有冷却区 , 于该核反应区的前端设有若干个注入口, 于该核反应区的后端设有 若干个浮游物排出口, 所述核反应区的前端连接有加压装置。  [Claim 1] A quantum dot core synthesis apparatus, comprising: a nuclear reaction zone, wherein the nuclear reaction zone includes at least one spiral reaction tube, and an inner wall of the spiral reaction tube is provided with an opposite direction to the spiral a channel for injecting a reactant into the reaction tube to generate a bubbling effect due to friction, a front portion of the nuclear reaction region is coated with a heating zone, a rear portion of the reaction zone is covered with a cooling zone, and a front end of the nuclear reaction zone is provided with a plurality of The injection port is provided with a plurality of floating material discharge ports at the rear end of the nuclear reaction zone, and a pressure device is connected to the front end of the nuclear reaction zone.
[权利要求 2] 根据权利要求 1所述的量子点核合成装置, 其特征在于, 所述加热区 [Claim 2] The quantum dot core synthesizing device according to claim 1, wherein the heating zone
、 冷却区分别包括缠绕于该螺旋状反应管上的温度控制管, 所述温度 控制管中填充满用于控制温度的液态水或油, 该加热区、 冷却区的温 度控制管分别与加热装置、 外部冷却器连接。 The cooling zone respectively comprises a temperature control tube wound on the spiral reaction tube, the temperature control tube is filled with liquid water or oil for controlling temperature, and the temperature control tube of the heating zone and the cooling zone is respectively connected with the heating device , external cooler connection.
[权利要求 3] 根据权利要求 1所述的量子点核合成装置, 其特征在于, 所述核反应 区的后段设有急速旋转区域和浮游物排出区域, 所述浮游物排出口设 于该浮游物排出区域;  [Claim 3] The quantum dot core synthesizing device according to claim 1, wherein a rear portion of the nuclear reaction zone is provided with a rapid rotation region and a float discharge region, and the float discharge port is provided in the float Object discharge area;
所述核反应区的后端连接有至少一根用于输送核的输送管道。  The rear end of the nuclear reaction zone is connected to at least one transport conduit for transporting the core.
[权利要求 4] 根据权利要求 3所述的量子点核合成装置, 其特征在于, 该急速旋转 区域中螺旋状反应管的管间距离小于核反应区前段的螺旋状反应管的 管间距离, 该浮游物排出区域的管间距离大于核反应区前段的螺旋状 反应管的管间距离。 [Claim 4] The quantum dot core synthesizing device according to claim 3, wherein a distance between tubes of the spiral reaction tube in the rapid rotation region is smaller than a distance between tubes of the spiral reaction tube in a front portion of the nuclear reaction region, The distance between the tubes of the float discharge area is greater than the distance between the tubes of the spiral reaction tube in the front section of the nuclear reaction zone.
[权利要求 5] 根据权利要求 3所述的量子点核合成装置, 其特征在于, 该急速旋转 区域的直径为核反应区前段的螺旋状反应管直径的三倍; 该急速旋转 区域的弯曲度比核反应区前段的螺旋状反应管减少 50%。  [Claim 5] The quantum dot core synthesizing device according to claim 3, wherein the diameter of the rapid rotation region is three times the diameter of the spiral reaction tube in the front portion of the nuclear reaction region; and the bending ratio of the rapid rotation region The spiral reaction tube in the front section of the nuclear reaction zone is reduced by 50%.
[权利要求 6] 根据权利要求 3所述的量子点核合成装置, 其特征在于, 于该核反应 区前端设有两个注入口, 于该核反应区中部对应急速旋转区域设有一 个注入口。  [Claim 6] The quantum dot core synthesizing device according to claim 3, wherein two injection ports are provided at the front end of the nuclear reaction zone, and an injection port is provided for the emergency speed rotation region in the middle of the nuclear reaction zone.
[权利要求 7] —种通过权利要求 1所述量子点核合成装置实施的量子点核合成方法 [Claim 7] A quantum dot core synthesis method implemented by the quantum dot core synthesis device of claim
, 其特征在于, 其包括以下步骤: 将核反应区螺旋状反应管进行真空 排气后转换为氮气环境, 将 Cd前驱体、 氯化三辛基膦、 1-十八碳烯通 过注入口注入核反应区的螺旋状反应管进行混合, 通过加热区将螺旋 状反应管加热到设定温度, 当反应物经过设定吋间及通过设定长度后 , 加入油胺和 Se前驱体, 从而生成 CdSe核, 反应生成的杂质通过急 速旋转区域加速后会浮在反应物上, 于浮游物排出区域的浮游物排出 口将杂质排出, 之后获得精制的 CdSe核。 The method comprises the steps of: converting a nuclear reaction zone spiral reaction tube into a nitrogen atmosphere after vacuum evacuation, and converting the Cd precursor, trioctylphosphine chloride, and 1-octadecene chloride The spiral reaction tube injected into the nuclear reaction zone through the injection port is mixed, and the spiral reaction tube is heated to a set temperature through the heating zone, and the oleylamine and Se precursor are added after the reactant passes through the set day and passes the set length. Thereby, a CdSe core is generated, and the impurities generated by the reaction are accelerated by the rapid rotation region and then float on the reactant, and the impurities are discharged at the float discharge port of the float discharge region, and then the purified CdSe core is obtained.
根据权利要求 7所述的量子点核合成方法, 其特征在于, 所述核反应 区的后段设有急速旋转区域和浮游物排出区域, 所述浮游物排出口设 于该浮游物排出区域; The quantum dot core synthesis method according to claim 7, wherein a rear portion of the nuclear reaction region is provided with a rapid rotation region and a float discharge region, and the float discharge port is disposed in the float discharge region;
于该核反应区前端设有两个注入口, 于该核反应区中部对应急速旋转 区域设有一个注入口; There are two injection ports at the front end of the nuclear reaction zone, and an injection port is arranged in the central portion of the nuclear reaction zone for the emergency speed rotation region;
所述核反应区的后端连接有至少一根用于输送核的输送管道。 The rear end of the nuclear reaction zone is connected to at least one transport conduit for transporting the core.
根据权利要求 8所述的量子点核合成方法, 其特征在于, 加热区的温 度维持在 270~290摄氏度, 在核反应区前端的左侧注入口中注入 Cd前 驱体、 氯化三辛基膦、 1-十八碳烯, 反应物在螺旋状反应管中由氮气 压力推动前行了 100cm达到右侧注入口前, 在右侧注入口中注入油胺 和 Se前驱体, 反应物继续在螺旋状反应管内混合、 反应, 继续移动, 直至生成 CdSe核, 核的大小, 即量子点的发光波长由螺旋状反应管 的长度及反应物通过吋间所决定。 The method of synthesizing a quantum dot core according to claim 8, wherein the temperature of the heating zone is maintained at 270 to 290 degrees Celsius, and a Cd precursor, trioctylphosphine chloride, 1 is injected into the left injection port at the front end of the nuclear reaction zone. - octadecene, the reactant is pushed in a spiral reaction tube by a pressure of 100 cm before reaching the right injection port, and the oleylamine and Se precursor are injected into the right injection port, and the reactant continues in the spiral reaction tube. Mixing, reacting, and continuing to move until the CdSe core is generated. The size of the core, that is, the wavelength of the quantum dot, is determined by the length of the spiral reaction tube and the reaction between the cells.
根据权利要求 9所述的量子点核合成方法, 其特征在于, CdSe核进入 核反应区后段的急速旋转区域, 该核反应区后段为冷却区, 温度维持 在 0~4摄氏度, 为了分离 CdSe核和杂质, 于对应急速旋转区域的注入 口中注入极性强的乙醇、 丙酮, 反应物在急速旋转区域中快速流动, 用 5分钟吋间通过长度为 150~200cm的反应管, 随着螺旋状反应管的 弧度变得柔和, 重量轻的杂质会浮游在反应物上流过, 从而通过浮游 物排出口清除到螺旋状反应管外部, 合成的核由输送管道排出。 The quantum dot core synthesis method according to claim 9, wherein the CdSe core enters a rapid rotation region in a rear portion of the nuclear reaction region, and the rear portion of the nuclear reaction region is a cooling region, and the temperature is maintained at 0 to 4 degrees Celsius, in order to separate the CdSe core. And impurities, injecting strong polar ethanol and acetone into the injection port of the emergency speed rotating region, the reactants flow rapidly in the rapid rotation region, and pass through the reaction tube with a length of 150-200 cm for 5 minutes, with the spiral reaction The curvature of the tube becomes soft, and light-weight impurities float on the reactants, thereby being removed to the outside of the spiral reaction tube through the float discharge port, and the synthesized core is discharged from the delivery pipe.
PCT/CN2018/083625 2017-04-21 2018-04-19 Quantum dot core synthesis device and quantum dot core synthesis method WO2018192539A1 (en)

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