WO2018192541A1 - 量子点前驱体合成装置及量子点前驱体合成方法 - Google Patents

量子点前驱体合成装置及量子点前驱体合成方法 Download PDF

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WO2018192541A1
WO2018192541A1 PCT/CN2018/083632 CN2018083632W WO2018192541A1 WO 2018192541 A1 WO2018192541 A1 WO 2018192541A1 CN 2018083632 W CN2018083632 W CN 2018083632W WO 2018192541 A1 WO2018192541 A1 WO 2018192541A1
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precursor
spiral
reaction tube
reaction
zone
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PCT/CN2018/083632
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English (en)
French (fr)
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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 CN201710266969.7A external-priority patent/CN106916584B/zh
Priority claimed from CN201710265873.9A external-priority patent/CN106914208B/zh
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 WO2018192541A1 publication Critical patent/WO2018192541A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements

Definitions

  • the present invention relates to the field of quantum dot synthesis, and in particular to a quantum dot precursor synthesis device and a quantum dot precursor synthesis method implemented by the quantum dot precursor synthesis device.
  • the synthesis method of quantum dots is a solution process, which mainly consists of a flask surrounding a heating jacket, a magnetic stirrer which can make the solution inside the flask uniform, and a temperature regulator and a thermometer for controlling the temperature of the solution.
  • a capacitor that maintains a stable concentration and a manifold that can convert a vacuum/nitrogen atmosphere are added.
  • 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 stirred reactor by the synthesized core and the stabilizer, the precursor is repeatedly injected to form a structurally stable core/shell structure.
  • a one-pot process has been developed, in which all the reactants are placed in the reactor at one time and the shell process is added.
  • Quantum dot synthesis is Ostwald ripening (Ostwald) Ripening), also a function of temperature and time, is known to be a technique in which small particles are grown after merging with relatively large particles, stopping particle growth when forming nanoparticles of the desired size.
  • Ostwald ripening Ostwald Ripening
  • 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 distribution of particles.
  • reaction product 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 using a strong polar solvent such as acetone or ethanol. Forced agitation by a magnetic bar or a stirrer during each reaction. Although it is known that a relatively uniform agitation can be achieved, the reaction agitation speed will vary depending on the amount of the reactants, which will affect the particle size and stabilize the nanoparticles. Formation.
  • Such a conventional synthesis method additionally requires a precursor reactor, a nuclear reactor, a core/shell reactor, and the like, and since it is re-measured and measured after each reaction, and then synthesized, there is a disadvantage that continuous operation cannot be performed. Moreover, due to differences in reaction time, particle separation, etc., it may be impossible to obtain nanoparticles having uniform characteristics.
  • the present invention discloses a quantum dot precursor synthesis device.
  • the invention also discloses a quantum dot precursor synthesis method implemented by the quantum dot precursor synthesis device.
  • a quantum dot precursor synthesis device comprising a precursor reaction zone, the precursor reaction zone comprising at least one spiral reaction tube, the inner wall of the spiral reaction tube being provided with an injection reaction tube opposite to the spiral shape a reaction tank in which a reactant generates a bubbling effect due to friction, a front portion of the precursor reaction zone is coated with a heating zone, and a rear section of the precursor reaction zone is coated with a cooling zone in the precursor reaction zone
  • the front end is provided with an injection port, and a front end of the precursor reaction zone is further connected with a pressurizing device, and the precursor raw material is mixed and reacted by a nitrogen gas pressure through a spiral reaction tube.
  • 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, and the temperature control tube of the heating zone and the cooling zone They are connected to the heating device and the external cooler respectively.
  • the precursor reaction zone includes four spiral reaction tubes arranged side by side.
  • At least one conveying pipe is connected to the rear end of the spiral reaction tube.
  • a quantum dot precursor synthesis method implemented by the foregoing quantum dot precursor synthesis device comprising the steps of: vacuum-venting a spiral reaction tube of a precursor reaction zone, converting it into a nitrogen atmosphere, and passing the precursor-generating raw material
  • the injection inlet is injected into the spiral reaction tube of the reaction zone of the precursor, and the reactant is stirred by the passage groove provided in the spiral reaction tube, and the spiral reaction tube is heated to a set temperature through the heating zone, and is passed through a pressurizing device. Nitrogen pressure is used to mix and react the precursor-forming raw material through a spiral reaction tube.
  • the length of the spiral reaction tube is adjusted according to the time required for the reaction, and the inner diameter or length of the spiral reaction tube is adjusted according to the time required for stirring, and the reaction is completed.
  • the precursor is transferred to the cooling zone for cooling. Since the precursors of Cd, S, and Zn are solidified, gelled, or solidified when cooled at room temperature, in order to smoothly carry out the reaction, a certain temperature should be maintained to obtain a quantum. Point precursor.
  • 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, and the temperature control tube of the heating zone and the cooling zone They are connected to the heating device and the external cooler respectively.
  • oleic acid Oleic acid
  • Cd cadmium oxide
  • the temperature of the heating zone is maintained at 170 degrees Celsius by a heating device, and the raw material injected through the injection port is mixed and reacted through a spiral reaction tube by nitrogen pressure, and the reaction takes time.
  • the stirring time can be adjusted according to the change of the inner diameter of the spiral tube and the length.
  • the inner diameter of the Cd precursor is 0.5 ⁇ 3cm, and the reaction time through the reaction tube is 3 ⁇ 7. Minutes, the Cd precursor that completed the reaction was transferred to the cooling zone and cooled in a spiral reaction tube with a length of 100 cm for 5 minutes.
  • the cooling temperature was 50. ⁇ 60 degrees Celsius.
  • the S precursor In order to produce the S precursor, 0.1 mol/L of 1-octadecene and S powder were metered into the injection port, and after vacuum evacuation, it was converted into a nitrogen atmosphere, and the temperature of the heating zone was maintained at 120 ° C by a heating device.
  • the nitrogen pressure causes the raw material injected through the injection port to be mixed and reacted through the spiral reaction tube, and the time required for the reaction is determined according to the length of the spiral reaction tube, and the stirring time can be adjusted according to the change of the inner diameter of the spiral tube and the change of the length.
  • the raw material is passed through a spiral reaction tube with an inner diameter of 1 cm and a length of 150 cm for 5 minutes and 30 seconds, and the synthesis can be completed.
  • the synthesized S precursor is passed through a threaded tube having a length of 100 cm in the cooling zone at 50 ⁇ . The cooling zone at 60 degrees Celsius takes 5 minutes.
  • 1-oleic acid and octadecene and zinc oxide having a molar concentration of 0.5 to 1.5 mol/L are metered into the injection port, and after vacuum evacuation, the mixture is converted into a nitrogen atmosphere, and the temperature of the heating zone is heated by a heating device. Maintaining at 300 degrees Celsius, the raw material injected through the injection port is mixed and reacted through a spiral reaction tube by nitrogen pressure. The time required for the reaction is determined according to the length of the spiral reaction tube, and the stirring time can be changed according to the inner diameter of the spiral tube.
  • the change of the length is adjusted, and the raw material is passed through a spiral reaction tube having an inner diameter of 1 cm and a length of 200 cm for 5 minutes and 30 seconds, and the synthesis reaction is completed, and the synthesized reactant is transferred to the cooling zone by the nitrogen pressure injected into the tube, and the cooling zone is cooled.
  • the length of the spiral reaction tube is 100 cm, and the Zn precursor passes through the cooling zone of 100 to 120 ° C for 5 minutes. Since the precursor of Cd, S, and Zn cools at room temperature, solidification, gelation or Solidified, so in order to carry out the reaction smoothly, a certain temperature should be maintained.
  • the trioctylphosphine and selenium powder having a molar concentration of 0.7 to 1.5 mol/L are metered into the injection port, and after being evacuated, the gas is converted into a nitrogen atmosphere, and the temperature of the heating zone is maintained at 50 by a heating device.
  • the raw material injected through the injection port is mixed and reacted through a spiral reaction tube by nitrogen pressure.
  • the time required for the reaction is determined according to the length of the spiral reaction tube, and the stirring time can be changed according to the inner diameter of the spiral tube and the length. The change was adjusted, and the raw material was passed through a spiral reaction tube having an inner diameter of 1 cm and a length of 430 cm for 10 minutes and 30 seconds to complete the synthesis.
  • the invention has the beneficial effects that the temperature of the liquid heating device varies according to the precursor type, and the temperature can be controlled to normal temperature to 300 degrees Celsius.
  • the quantum dot precursor synthesis device of the invention has a simple and reliable structure and passes through the spiral reaction tube.
  • the channel tank is provided for stirring the reactants, adjusting the inner diameter and length of the spiral reaction tube for different kinds of precursors, and controlling the passage time of the reactants in the spiral reaction tube, thereby obtaining a high-quality precursor, which is highly efficient and stable. It lays a solid foundation for the synthesis of quantum dots that improve luminous efficiency and vividness.
  • Figure 1 is a schematic view of the structure of the present invention.
  • this embodiment discloses a quantum dot precursor synthesis apparatus including a precursor reaction zone including at least one spiral reaction tube 4, and an inner wall of the spiral reaction tube 4.
  • a precursor reaction zone including at least one spiral reaction tube 4, and an inner wall of the spiral reaction tube 4.
  • the front portion of the precursor reaction region is coated with a heating zone 1, the precursor reaction zone
  • the rear stage is covered with a cooling zone 2, and an injection port 3 is arranged at the front end of the precursor reaction zone, and a front end of the precursor reaction zone is further connected with a pressurizing device, and the precursor is used to generate raw materials by nitrogen pressure.
  • the mixture is reacted through a spiral reaction tube.
  • the heating zone 1 and the cooling zone 2 respectively comprise a temperature control tube wound on the spiral reaction tube 4, and the temperature control tube is filled with liquid water or oil for controlling temperature, the heating zone 1, the cooling zone
  • the temperature control tubes of 2 are connected to the heating device 5 and the external cooler 6, respectively.
  • the precursor reaction zone includes four spiral reaction tubes 4 arranged side by side.
  • At least one conveying pipe 7 is connected to the rear end of the spiral reaction tube 4.
  • a method for synthesizing a quantum dot precursor by the foregoing quantum dot precursor synthesis device comprising the steps of: vacuum-venting a spiral reaction tube 4 of a precursor reaction zone, converting it into a nitrogen atmosphere, and forming a precursor into a raw material.
  • the spiral reaction tube 4 of the precursor reaction zone is injected through the injection port 3, the spiral reaction tube 4 is heated to a set temperature through the heating zone 1, and the precursor-generating raw material is passed through the spiral reaction tube 4 by a nitrogen pressure using a pressurizing device.
  • the heating zone 1 and the cooling zone 2 respectively comprise a temperature control tube wound on the spiral reaction tube 4, and the temperature control tube is filled with liquid water or oil for controlling temperature, the heating zone 1, the cooling zone
  • the temperature control tubes of 2 are connected to the heating device 5 and the external cooler 6, respectively.
  • oleic acid (Oleic) is placed at a molar concentration of 0.05 to 1.0 mol/L at the injection port 3.
  • Acid) and cadmium oxide (Cd oxide), after being vacuum-exhausted, converted into a nitrogen atmosphere, the temperature of the heating zone 1 is maintained at 170 degrees Celsius by the heating device 5, and the raw material injected through the injection port 3 is passed through a spiral reaction tube by nitrogen pressure. 4 mixing and reaction, the time required for the reaction is determined according to the length of the spiral reaction tube 4, the stirring time can be adjusted according to the change of the inner diameter of the spiral tube and the length, and the inner diameter of the Cd precursor is 0.5 ⁇ 3 cm.
  • the reaction time required for the reaction through the reaction tube is 3 to 7 minutes, and the Cd precursor which has completed the reaction is transferred to the cooling zone 2, and is cooled by a spiral reaction tube 4 having a length of 100 cm for 5 minutes, and the cooling temperature is 50 °. 60 degrees Celsius.
  • the S (sulfur) precursor In order to produce the S (sulfur) precursor, 0.1 mol/L of 1-octadecene and S powder are metered and injected into the injection port 3, and after vacuum evacuation, the temperature is changed to a nitrogen atmosphere, and the temperature of the heating zone 1 is made by the heating device 5. Maintaining at 120 degrees Celsius, the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by nitrogen pressure. The time required for the reaction is determined according to the length of the spiral reaction tube 4, and the stirring time can be determined according to the inner diameter of the spiral tube.
  • the change and the change of the length are adjusted, and the raw material is passed through the spiral reaction tube 4 having an inner diameter of 1 cm and a length of 150 cm for 5 minutes and 30 seconds, that is, the synthesis can be completed, and the synthesized S precursor passes through the cooling zone 2
  • a threaded pipe of length 100 cm is used for 5 minutes in a cooling zone 2 of 50 to 60 degrees Celsius.
  • a Zn (zinc) precursor 1-oleic acid and octadecene and zinc oxide having a molar concentration of 0.5 to 1.5 mol/L are metered into the injection port 3, and after vacuum evacuation, the mixture is converted into a nitrogen atmosphere and passed through a heating device. 5, the temperature of the heating zone 1 is maintained at 300 degrees Celsius, and the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by the pressure of nitrogen gas, and the time required for the reaction is determined according to the length of the spiral reaction tube 4, and stirring is performed. The time can be adjusted according to the change of the inner diameter of the spiral tube and the change of the length.
  • the raw material can be synthesized by using a spiral reaction tube 4 having an inner diameter of 1 cm and a length of 200 cm for 5 minutes and 30 seconds, and the synthesized reactant is injected into the mixture.
  • the nitrogen pressure in the tube is transferred to the cooling zone 2, the length of the spiral reaction tube 4 of the cooling zone 2 is 100 cm, and the Zn precursor is passed in the cooling zone 2 of 100 to 120 degrees Celsius for 5 minutes, due to the Cd, S, and Zn.
  • the precursor is cooled at room temperature, solidification, gelation or solidification occurs, so in order to carry out the reaction smoothly, a certain temperature should be maintained.
  • the Zn precursor is produced, the temperature of the cooling zone 2 is 100 to 120 degrees Celsius.
  • trioctylphosphine and selenium powder having a molar concentration of 0.7 to 1.5 mol/L are metered into the injection port 3, vacuum-ventilated, and then converted into a nitrogen atmosphere, and the heating zone 1 is heated by the heating device 5.
  • the temperature is maintained at 50 to 60 degrees Celsius, and the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by nitrogen pressure.
  • the time required for the reaction is determined according to the length of the spiral reaction tube 4, and the stirring time can be determined according to The change of the inner diameter of the spiral tube and the change of the length were adjusted, and the raw material was passed through a spiral reaction tube 4 having an inner diameter of 1 cm and a length of 430 cm for 10 minutes and 30 seconds to complete the synthesis.
  • the temperature of the cooling zone 2 coincides with the temperature of the heating zone 1.
  • the temperature of the liquid heating device may be different, and the temperature can be controlled to normal temperature to 300 degrees Celsius.
  • the quantum dot precursor synthesis device of the present invention has a simple and reliable structure, and can be provided through the channel groove provided in the spiral reaction tube 4. The reactant is stirred, and the inner diameter and length of the spiral reaction tube 4 are adjusted for different kinds of precursors, and the passage time of the reactant in the spiral reaction tube 4 is controlled, thereby obtaining a high-quality precursor, which is highly efficient and stable, and is synthesized.
  • a quantum foundation that enhances luminous efficiency and sharpness lays a solid foundation.
  • this embodiment discloses a quantum dot precursor synthesis apparatus including a precursor reaction zone including at least one spiral reaction tube 4, and an inner wall of the spiral reaction tube 4.
  • a precursor reaction zone including at least one spiral reaction tube 4, and an inner wall of the spiral reaction tube 4.
  • the front portion of the precursor reaction region is coated with a heating zone 1, the precursor reaction zone
  • the rear stage is covered with a cooling zone 2, and an injection port 3 is arranged at the front end of the precursor reaction zone, and a front end of the precursor reaction zone is further connected with a pressurizing device, and the precursor is used to generate raw materials by nitrogen pressure.
  • the mixture is reacted through a spiral reaction tube.
  • the heating zone 1 and the cooling zone 2 respectively comprise a temperature control tube wound on the spiral reaction tube 4, and the temperature control tube is filled with liquid water or oil for controlling temperature, the heating zone 1, the cooling zone
  • the temperature control tubes of 2 are connected to the heating device 5 and the external cooler 6, respectively.
  • the precursor reaction zone includes four spiral reaction tubes 4 arranged side by side.
  • At least one conveying pipe 7 is connected to the rear end of the spiral reaction tube 4.
  • a method for synthesizing a quantum dot precursor by the foregoing quantum dot precursor synthesis device comprising the steps of: vacuum-venting a spiral reaction tube 4 of a precursor reaction zone, converting it into a nitrogen atmosphere, and forming a precursor into a raw material.
  • the spiral reaction tube 4 of the precursor reaction zone is injected through the injection port 3, the spiral reaction tube 4 is heated to a set temperature through the heating zone 1, and the precursor-generating raw material is passed through the spiral reaction tube 4 by a nitrogen pressure using a pressurizing device.
  • the heating zone 1 and the cooling zone 2 respectively comprise a temperature control tube wound on the spiral reaction tube 4, and the temperature control tube is filled with liquid water or oil for controlling temperature, the heating zone 1, the cooling zone
  • the temperature control tubes of 2 are connected to the heating device 5 and the external cooler 6, respectively.
  • oleic acid (Oleic) is placed at a molar concentration of 0.05 to 1.0 mol/L at the injection port 3.
  • Acid) and cadmium oxide (Cd oxide), after being vacuum-exhausted, converted into a nitrogen atmosphere, the temperature of the heating zone 1 is maintained at 170 degrees Celsius by the heating device 5, and the raw material injected through the injection port 3 is passed through a spiral reaction tube by nitrogen pressure. 4 mixing and reaction, the time required for the reaction is determined according to the length of the spiral reaction tube 4, the stirring time can be adjusted according to the change of the inner diameter of the spiral tube and the length, and the inner diameter of the Cd precursor is 0.5 ⁇ 3 cm.
  • the reaction time required for the reaction through the reaction tube is 3 to 7 minutes, and the Cd precursor which has completed the reaction is transferred to the cooling zone 2, and is cooled by a spiral reaction tube 4 having a length of 100 cm for 5 minutes, and the cooling temperature is 50 °. 60 degrees Celsius.
  • the S (sulfur) precursor In order to produce the S (sulfur) precursor, 0.1 mol/L of 1-octadecene and S powder are metered and injected into the injection port 3, and after vacuum evacuation, the temperature is changed to a nitrogen atmosphere, and the temperature of the heating zone 1 is made by the heating device 5. Maintaining at 120 degrees Celsius, the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by nitrogen pressure. The time required for the reaction is determined according to the length of the spiral reaction tube 4, and the stirring time can be determined according to the inner diameter of the spiral tube.
  • the change and the change of the length are adjusted, and the raw material is passed through the spiral reaction tube 4 having an inner diameter of 1 cm and a length of 150 cm for 5 minutes and 30 seconds, that is, the synthesis can be completed, and the synthesized S precursor passes through the cooling zone 2
  • a threaded pipe of length 100 cm is used for 5 minutes in a cooling zone 2 of 50 to 60 degrees Celsius.
  • a Zn (zinc) precursor 1-oleic acid and octadecene and zinc oxide having a molar concentration of 0.5 to 1.5 mol/L are metered into the injection port 3, and after vacuum evacuation, the mixture is converted into a nitrogen atmosphere and passed through a heating device. 5, the temperature of the heating zone 1 is maintained at 300 degrees Celsius, and the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by the pressure of nitrogen gas, and the time required for the reaction is determined according to the length of the spiral reaction tube 4, and stirring is performed. The time can be adjusted according to the change of the inner diameter of the spiral tube and the change of the length.
  • the raw material can be synthesized by using a spiral reaction tube 4 having an inner diameter of 1 cm and a length of 200 cm for 5 minutes and 30 seconds, and the synthesized reactant is injected into the mixture.
  • the nitrogen pressure in the tube is transferred to the cooling zone 2, the length of the spiral reaction tube 4 of the cooling zone 2 is 100 cm, and the Zn precursor is passed in the cooling zone 2 of 100 to 120 degrees Celsius for 5 minutes, due to the Cd, S, and Zn.
  • the precursor is cooled at room temperature, solidification, gelation or solidification occurs, so in order to carry out the reaction smoothly, a certain temperature should be maintained.
  • the Zn precursor is produced, the temperature of the cooling zone 2 is 100 to 120 degrees Celsius.
  • trioctylphosphine and selenium powder having a molar concentration of 0.7 to 1.5 mol/L are metered into the injection port 3, vacuum-ventilated, and then converted into a nitrogen atmosphere, and the heating zone 1 is heated by the heating device 5.
  • the temperature is maintained at 50 to 60 degrees Celsius, and the raw material injected through the injection port 3 is mixed and reacted through the spiral reaction tube 4 by nitrogen pressure.
  • the time required for the reaction is determined according to the length of the spiral reaction tube 4, and the stirring time can be determined according to The change of the inner diameter of the spiral tube and the change of the length were adjusted, and the raw material was passed through a spiral reaction tube 4 having an inner diameter of 1 cm and a length of 430 cm for 10 minutes and 30 seconds to complete the synthesis.
  • the temperature of the cooling zone 2 coincides with the temperature of the heating zone 1.
  • the temperature of the liquid heating device may be different, and the temperature can be controlled to normal temperature to 300 degrees Celsius.
  • the quantum dot precursor synthesis device of the present invention has a simple and reliable structure, and can be adopted through a channel groove provided in the spiral reaction tube. The reactant is stirred, and the inner diameter and length of the spiral reaction tube are adjusted for different kinds of precursors, and the passage time of the reactant in the spiral reaction tube is controlled, thereby obtaining a high-quality precursor, which is highly efficient and stable, and improves the luminescence for synthesis.
  • the quantum point of efficiency and vividness lays a solid foundation.

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Abstract

本发明公开了一种量子点前驱体合成装置，其包括前驱体反应区，该前驱体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，所述前驱体反应区的前段包覆有加热区，所述前驱体反应区的后段包覆有冷却区，于该前驱体反应区的前端设有注入口，所述前驱体反应区的前端还连接有加压装置。本发明还公开了一种量子点前驱体合成方法。本发明的量子点前驱体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，针对不同种类的前驱体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时间，从而能获得优质的前驱体。

Description

量子点前驱体合成装置及量子点前驱体合成方法 技术领域
本发明涉及量子点合成领域，具体涉及一种量子点前驱体合成装置及通过该量子点前驱体合成装置实施的量子点前驱体合成方法。
 背景技术
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。
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，最近还开发出了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。
 技术问题
如此，溶液工艺合成方法变成大容量化时，为了反应物质内的均匀性，有时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），也是温度和时间的函数，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时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时，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。
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。
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。而且因为反应时间、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。
前驱体的合成是量子点合成中的一个关键工序，现有的合成装置难以很好的获得优质的前驱体。
 技术解决方案
为了解决上述问题，本发明公开了一种量子点前驱体合成装置。
本发明还公开了一种通过该量子点前驱体合成装置实施的量子点前驱体合成方法。
本发明为实现上述目的所采用的技术方案是：
一种量子点前驱体合成装置，其包括前驱体反应区，该前驱体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，所述前驱体反应区的前段包覆有加热区，所述前驱体反应区的后段包覆有冷却区，于该前驱体反应区的前端设有注入口，所述前驱体反应区的前端还连接有加压装置，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应。
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。
所述前驱体反应区包括并列设置的四个螺旋状反应管。
所述螺旋状反应管的后端连接有至少一根输送管道。
一种通过前述量子点前驱体合成装置实施的量子点前驱体合成方法，其包括以下步骤：将前驱体反应区的螺旋状反应管进行真空排气后转换为氮气环境，将前驱体生成原料通过注入口注入前驱体反应区的螺旋状反应管，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，通过加热区将螺旋状反应管加热到设定温度，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应，根据反应所需时间调整螺旋状反应管的长度，根据搅拌所需时间调整螺旋状反应管的内径或长度，反应完成后生产的前驱体转移至冷却区进行冷却，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度，从而制得量子点前驱体。
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。
为了制作Cd前驱体，于注入口以0.05~1.0mol/L的摩尔浓度放入油酸（Oleic acid）和氧化镉（Cd oxide），真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在170摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，反应所需的时间根据螺旋状反应管的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，Cd前驱体合成所需内径为0.5~3cm，通过反应管反应的所需时间为3~7分钟，完成反应的Cd前驱体会转移到冷却区内，用5分钟的时间通过长度为100cm的螺旋状反应管进行冷却，冷却温度为50 ~60摄氏度。
为了制作S前驱体，在注入口计量注入了0.1mol/L的1-十八碳烯和S粉末，真空排气后转换为氮气环境，通过加热装置使加热区的温度维持在120摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，反应所需的时间根据螺旋状反应管的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒的时间通过内径1㎝，长度为150㎝的螺旋状反应管，即能完成合成，完成合成的S前驱体在冷却区内通过长度为100㎝的螺纹管，在50~60摄氏度的冷却区内用时为5分钟。
为了制作Zn前驱体，在注入口中计量注入摩尔浓度为0.5~1.5mol/L的1-油酸和十八烯以及氧化锌，真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在300摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，反应所需的时间根据螺旋状反应管的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒经过内径1㎝、长度200㎝的螺旋状反应管，即可完成合成，完成合成的反应物通过注入到管内的氮气压力移送到冷却区，冷却区螺旋状反应管的长度为100㎝，Zn前驱体在100~120摄氏度的冷却区内用时为5分钟通过，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度。
为了制作Se前驱体，在注入口计量注入摩尔浓度为0.7~1.5mol/L的三辛基膦和硒粉，真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在50~60摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，反应所需的时间根据螺旋状反应管的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用10分30秒经过内径1㎝、长度430㎝的螺旋状反应管，即完成合成。
 有益效果
本发明的有益效果为：根据前驱体种类液状加热装置的温度会有所不同，可以将温度控制到常温~300摄氏度，本发明的量子点前驱体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，针对不同种类的前驱体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时间，从而能获得优质的前驱体，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。
 附图说明
下面结合附图与具体实施方式，对本发明进一步说明。
图1是本发明的结构示意图。
 本发明的最佳实施方式
实施例，参见图1，本实施例公开了一种量子点前驱体合成装置，其包括前驱体反应区，该前驱体反应区包括至少一个螺旋状反应管4，所述螺旋状反应管4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，所述前驱体反应区的前段包覆有加热区1，所述前驱体反应区的后段包覆有冷却区2，于该前驱体反应区的前端设有注入口3，所述前驱体反应区的前端还连接有加压装置，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应。
所述加热区1、冷却区2分别包括缠绕于该螺旋状反应管4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1、冷却区2的温度控制管分别与加热装置5、外部冷却器6连接。
所述前驱体反应区包括并列设置的四个螺旋状反应管4。
所述螺旋状反应管4的后端连接有至少一根输送管道7。
一种通过前述量子点前驱体合成装置实施的量子点前驱体合成方法，其包括以下步骤：将前驱体反应区的螺旋状反应管4进行真空排气后转换为氮气环境，将前驱体生成原料通过注入口3注入前驱体反应区的螺旋状反应管4，通过加热区1将螺旋状反应管4加热到设定温度，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管4进行混合、反应，根据反应所需时间调整螺旋状反应管4的长度，根据搅拌所需时间调整螺旋状反应管4的内径或长度，反应完成后生产的前驱体转移至冷却区2进行冷却，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度，从而制得量子点前驱体。
所述加热区1、冷却区2分别包括缠绕于该螺旋状反应管4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1、冷却区2的温度控制管分别与加热装置5、外部冷却器6连接。
为了制作Cd（镉）前驱体，于注入口3以0.05~1.0mol/L的摩尔浓度放入油酸（Oleic acid）和氧化镉（Cd oxide），真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在170摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，Cd前驱体合成所需内径为0.5~3cm，通过反应管反应的所需时间为3~7分钟，完成反应的Cd前驱体会转移到冷却区2内，用5分钟的时间通过长度为100cm的螺旋状反应管4进行冷却，冷却温度为50 ~60摄氏度。
为了制作S（硫）前驱体，在注入口3计量注入了0.1mol/L的1-十八碳烯和S粉末，真空排气后转换为氮气环境，通过加热装置5使加热区1的温度维持在120摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒的时间通过内径1㎝，长度为150㎝的螺旋状反应管4，即能完成合成，完成合成的S前驱体在冷却区2内通过长度为100㎝的螺纹管，在50~60摄氏度的冷却区2内用时为5分钟。
为了制作Zn（锌）前驱体，在注入口3中计量注入摩尔浓度为0.5~1.5mol/L的1-油酸和十八烯以及氧化锌，真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在300摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒经过内径1㎝、长度200㎝的螺旋状反应管4，即可完成合成，完成合成的反应物通过注入到管内的氮气压力移送到冷却区2，冷却区2螺旋状反应管4的长度为100㎝，Zn前驱体在100~120摄氏度的冷却区2内用时为5分钟通过，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度。在制作Zn前驱体时，冷却区2的温度为100~120摄氏度。
为了制作Se（硒）前驱体，在注入口3计量注入摩尔浓度为0.7~1.5mol/L的三辛基膦和硒粉，真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在50~60摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用10分30秒经过内径1㎝、长度430㎝的螺旋状反应管4，即完成合成。在制作Se（硒）前驱体时，冷却区2的温度与加热区1的温度一致。
根据前驱体种类液状加热装置的温度会有所不同，可以将温度控制到常温~300摄氏度，本发明的量子点前驱体合成装置结构简单可靠，通过螺旋状反应管4中设有的途径槽能够将反应物进行搅拌，针对不同种类的前驱体调整螺旋状反应管4的内径、长度，控制反应物在螺旋状反应管4内的通过时间，从而能获得优质的前驱体，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。
 本发明的实施方式
实施例，参见图1，本实施例公开了一种量子点前驱体合成装置，其包括前驱体反应区，该前驱体反应区包括至少一个螺旋状反应管4，所述螺旋状反应管4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，所述前驱体反应区的前段包覆有加热区1，所述前驱体反应区的后段包覆有冷却区2，于该前驱体反应区的前端设有注入口3，所述前驱体反应区的前端还连接有加压装置，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应。
所述加热区1、冷却区2分别包括缠绕于该螺旋状反应管4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1、冷却区2的温度控制管分别与加热装置5、外部冷却器6连接。
所述前驱体反应区包括并列设置的四个螺旋状反应管4。
所述螺旋状反应管4的后端连接有至少一根输送管道7。
一种通过前述量子点前驱体合成装置实施的量子点前驱体合成方法，其包括以下步骤：将前驱体反应区的螺旋状反应管4进行真空排气后转换为氮气环境，将前驱体生成原料通过注入口3注入前驱体反应区的螺旋状反应管4，通过加热区1将螺旋状反应管4加热到设定温度，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管4进行混合、反应，根据反应所需时间调整螺旋状反应管4的长度，根据搅拌所需时间调整螺旋状反应管4的内径或长度，反应完成后生产的前驱体转移至冷却区2进行冷却，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度，从而制得量子点前驱体。
所述加热区1、冷却区2分别包括缠绕于该螺旋状反应管4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1、冷却区2的温度控制管分别与加热装置5、外部冷却器6连接。
为了制作Cd（镉）前驱体，于注入口3以0.05~1.0mol/L的摩尔浓度放入油酸（Oleic acid）和氧化镉（Cd oxide），真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在170摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，Cd前驱体合成所需内径为0.5~3cm，通过反应管反应的所需时间为3~7分钟，完成反应的Cd前驱体会转移到冷却区2内，用5分钟的时间通过长度为100cm的螺旋状反应管4进行冷却，冷却温度为50 ~60摄氏度。
为了制作S（硫）前驱体，在注入口3计量注入了0.1mol/L的1-十八碳烯和S粉末，真空排气后转换为氮气环境，通过加热装置5使加热区1的温度维持在120摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒的时间通过内径1㎝，长度为150㎝的螺旋状反应管4，即能完成合成，完成合成的S前驱体在冷却区2内通过长度为100㎝的螺纹管，在50~60摄氏度的冷却区2内用时为5分钟。
为了制作Zn（锌）前驱体，在注入口3中计量注入摩尔浓度为0.5~1.5mol/L的1-油酸和十八烯以及氧化锌，真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在300摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用5分30秒经过内径1㎝、长度200㎝的螺旋状反应管4，即可完成合成，完成合成的反应物通过注入到管内的氮气压力移送到冷却区2，冷却区2螺旋状反应管4的长度为100㎝，Zn前驱体在100~120摄氏度的冷却区2内用时为5分钟通过，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度。在制作Zn前驱体时，冷却区2的温度为100~120摄氏度。
为了制作Se（硒）前驱体，在注入口3计量注入摩尔浓度为0.7~1.5mol/L的三辛基膦和硒粉，真空排气后转换成氮气环境，通过加热装置5使加热区1的温度维持在50~60摄氏度，利用氮气压力使通过注入口3注入的原料经过螺旋状反应管4进行混合、反应，反应所需的时间根据螺旋状反应管4的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用10分30秒经过内径1㎝、长度430㎝的螺旋状反应管4，即完成合成。在制作Se（硒）前驱体时，冷却区2的温度与加热区1的温度一致。
 工业实用性
根据前驱体种类液状加热装置的温度会有所不同，可以将温度控制到常温~300摄氏度，本发明的量子点前驱体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，针对不同种类的前驱体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时间，从而能获得优质的前驱体，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。

Claims (8)

  1. 一种量子点前驱体合成装置，其特征在于：其包括前驱体反应区，该前驱体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，所述前驱体反应区的前段包覆有加热区，所述前驱体反应区的后段包覆有冷却区，于该前驱体反应区的前端设有注入口，所述前驱体反应区的前端还连接有加压装置；利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应；
    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；
    所述前驱体反应区包括并列设置的四个螺旋状反应管。
  2. 根据权利要求1所述的量子点前驱体合成装置，其特征在于，所述螺旋状反应管的后端连接有至少一根输送管道。
  3. 一种通过权利要求1所述量子点前驱体合成装置实施的量子点前驱体合成方法，其特征在于，其包括以下步骤：将前驱体反应区的螺旋状反应管进行真空排气后转换为氮气环境，将前驱体生成原料通过注入口注入前驱体反应区的螺旋状反应管，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，通过加热区将螺旋状反应管加热到设定温度，利用加压装置通过氮气压力将前驱体生成原料经过螺旋状反应管进行混合、反应，根据反应所需时间调整螺旋状反应管的长度，根据搅拌所需时间调整螺旋状反应管的内径或长度，反应完成后生产的前驱体转移至冷却区进行冷却，由于Cd、S、Zn的前驱体在常温冷却时，会出现凝固、凝胶状或固体化，所以为了顺畅的进行反应，应保持一定温度，从而制得量子点前驱体。
  4. 根据权利要求3所述的量子点前驱体合成方法，其特征在于，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。
  5. 根据权利要求4所述的量子点前驱体合成方法，其特征在于，为了制作Cd前驱体，于注入口以0.05~1.0mol/L的摩尔浓度放入油酸和氧化镉，真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在170摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应， Cd前驱体合成所需内径为0.5~3cm，通过反应管反应的所需时间为3~7分钟，完成反应的Cd前驱体会转移到冷却区内，用5分钟的时间通过长度为100cm的螺旋状反应管进行冷却，冷却温度为50 ~60摄氏度。
  6. 根据权利要求4所述的量子点前驱体合成方法，其特征在于，为了制作S前驱体，在注入口计量注入了0.1mol/L的1-十八碳烯和S粉末，真空排气后转换为氮气环境，通过加热装置使加热区的温度维持在120摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，原料用5分30秒的时间通过内径1㎝，长度为150㎝的螺旋状反应管，即能完成合成，完成合成的S前驱体在冷却区内通过长度为100㎝的螺纹管，在50~60摄氏度的冷却区内用时为5分钟。
  7. 根据权利要求4所述的量子点前驱体合成方法，其特征在于，为了制作Zn前驱体，在注入口中计量注入摩尔浓度为0.5~1.5mol/L的1-油酸和十八烯以及氧化锌，真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在300摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，原料用5分30秒经过内径1㎝、长度200㎝的螺旋状反应管，即可完成合成，完成合成的反应物通过注入到管内的氮气压力移送到冷却区，冷却区螺旋状反应管的长度为100㎝，Zn前驱体在100~120摄氏度的冷却区内用时为5分钟通过。
  8. 根据权利要求4所述的量子点前驱体合成方法，其特征在于，为了制作Se前驱体，在注入口计量注入摩尔浓度为0.7~1.5mol/L的三辛基膦和硒粉，真空排气后转换成氮气环境，通过加热装置使加热区的温度维持在50~60摄氏度，利用氮气压力使通过注入口注入的原料经过螺旋状反应管进行混合、反应，反应所需的时间根据螺旋状反应管的长度决定，搅拌时间可根据螺旋式管内径的变化和长度的变化进行调节，原料用10分30秒经过内径1㎝、长度430㎝的螺旋状反应管，即完成合成。
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