CN206828441U - Quantum dot nucleocapsid synthesizer - Google Patents

Quantum dot nucleocapsid synthesizer Download PDF

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Publication number
CN206828441U
CN206828441U CN201720426276.5U CN201720426276U CN206828441U CN 206828441 U CN206828441 U CN 206828441U CN 201720426276 U CN201720426276 U CN 201720426276U CN 206828441 U CN206828441 U CN 206828441U
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core shell
reaction zone
zone
quantum dot
helical form
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陈绍楷
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Dongguan Reteck Coating Technology Co Ltd
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Dongguan Reteck Coating Technology Co Ltd
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Abstract

The utility model discloses a kind of quantum dot nucleocapsid synthesizer, it includes being used for the core shell reaction zone for carrying out core shell reaction, the reaction zone includes at least one helical form reaction tube, the helical form reaction tube is provided with the reactant made in injection reaction tube of the helical form opposite direction because friction produces the approach groove of bubbling effect, the leading portion of the core shell reaction zone is coated with heating zone, the back segment of the core shell reaction zone is coated with cooling zone, several inlets are provided with the front end of the core shell reaction zone, several floating material outlets are provided with the rear end of the core shell reaction zone, the front end of the core shell reaction zone is connected with pressue device.Quantum dot nucleocapsid synthesizer of the present utility model can improve quantum dot stability and particle size it is uniform, while it can be made not have defect, therefore quantum efficiency can be maximized, so as to synthesize the quantum dot for improving luminous efficiency and vividness.

Description

Quantum dot nucleocapsid synthesizer
Technical field
It the utility model is related to quantum dot synthesis field, and in particular to a kind of quantum dot nucleocapsid synthesizer.
Background technology
In the prior art, the synthetic method of quantum dot is solwution method technique, mainly by the flask around heating mantle, can make The uniform magnetic stirring apparatus of flask interior solution and the thermoregulator and thermometer composition for controlling solution temperature.In addition, add The capacitor for maintaining steady concentration and the manifold composition that vacuum/nitrogen atmosphere can be changed are added.
Synthetic method is the organic compound synthetic kernel (core) using presoma (precursor), in order that synthesis Core and stabilizer form appropriate shell in the reactor of mixing, inject presoma repeatedly and form constitutionally stable core shell Structure, one-pot techniques are further developed recently, all reactive materials are disposably put into reactor and add shell process again Method.
In this way, when solution process synthetic method becomes high capacity, for the uniformity in reactive material, can also use sometimes Impeller replaces magnetic stirring apparatus, but because the uneven temperature difference, uneven environment cause the difference of concentration in reactant with And the difference of combination.Quantum dot synthesis is Ostwald ripening (Ostwald ripening), and temperature and time Function, it is reported that this technology is small particle and the fit growth afterwards of relatively large particle, when the nano-particle of size needed for formation When stop particle growth technology.But current method is when controlling particle growth by cooling down, to produce temperature difference, it is difficult to Synthesize particle of uniform size.Therefore, these factors can also influence the characteristics of luminescence of quantum dot nano-particle and spread size Uniform particle.
In order to obtain a certain size nano-particle, rapidly cooled down.Also have in this reactant reaction accessory substance, Organic matter, so removing organic matter by centrifugal filtration.Nano-particle separation can be by intensive polar solvents such as acetone or alcohols, profit The size of particle is distinguished with centrifugal filtration.Action of forced stirring is carried out by bar magnet or mixer in each course of reaction, although this is It is known that can reach the method for comparing uniform stirring, but according to the amount of reactant, reaction mixing speed can be different, this The size of particle can be influenceed and stablize the formation of nano-particle.
This existing synthetic method there is additionally required forerunner's reactor according, nuclear reactor, core shell reactor etc., because It is that metering, measurement are re-started after each autoreaction, is then synthesized, so the shortcomings that in the presence of that can not work continuously.And Because the differences such as reaction time, separate particles, it is possible to the nano-particle with the characteristics of uniform can not be obtained.
The synthesis of quantum dot nucleocapsid is an important step in quantum dot synthesis, how to pass through the synthesis of advantages of simple Device make nucleocapsid synthesis technique simplify, and can produce the high-quality quantum dot for meeting use condition become industry need Ask.
Utility model content
In order to solve the above problems, the utility model discloses a kind of quantum dot nucleocapsid synthesizer.
Used technical scheme is the utility model to achieve the above object:
A kind of quantum dot nucleocapsid synthesizer, it includes being used for the core shell reaction zone for carrying out core shell reaction, the reaction zone Including at least one helical form reaction tube, the helical form reaction tube is provided with makes injection with the helical form opposite direction Reactant in reaction tube produces the approach groove of bubbling effect because rubbing, and the leading portion of the core shell reaction zone is coated with heating zone, The back segment of the core shell reaction zone is coated with cooling zone, and several inlets are provided with the front end of the core shell reaction zone, in The rear end of the core shell reaction zone is provided with several floating material outlets, and the front end of the core shell reaction zone is connected with pressurization dress Put.
The heating zone, cooling zone include the temperature control zone being wound on the helical form reaction tube, the temperature respectively Fill the full aqueous water or oil for being used to control temperature in control pipe, the heating zone, cooling zone temperature control zone respectively with heating Device, external cooler connection.
The back segment of the core shell reaction zone is provided with rapidly rotary area and floating material discharging area, the floating material discharge Mouth is located at the floating material discharging area.
This rapidly in rotary area the tube pitch of helical form reaction tube from the helical form reaction less than core shell reaction zone leading portion The tube pitch of pipe from, the floating material discharging area tube pitch from the helical form reaction tube more than core shell reaction zone leading portion pipe Between distance.
Three times of the rapidly helical form reaction tube diameter of a diameter of core shell reaction zone leading portion of rotary area;This is rapidly The flexibility of rotary area reduces 50% than the helical form reaction tube of core shell reaction zone leading portion.
Be provided with the first to the 5th inlet by spacing distance in the front end of the core shell reaction zone, adjacent two inlet it Between distance be 100cm, it is corresponding in the rear end of the core shell reaction zone described in rapidly rotary area be provided with the 6th inlet, in the core/ The rear end of shell reaction zone is provided with three floating material outlets.
A kind of quantum dot nucleocapsid synthetic method implemented by foregoing quantum dot nucleocapsid synthesizer, it includes following step Suddenly:Will core shell reaction zone carry out vacuum exhaust after be converted to nitrogen environment, by CdSe core, 1- vaccenic acids and oleyl amine inject core/ The helical form reaction tube of shell reaction zone, helical form reaction tube is heated to by design temperature by heating zone, makes CdSe core, 1- 18 Carbene and oleyl amine reaction, Cd presomas and Zn presomas, S presomas, Zn presomas and Cd forerunner are sequentially added by interval time Body, S presomas, Zn presomas and Cd presomas, and Zn presomas and S presomas, so as to accumulate multilayered shell on CdSe core, close Into CdSe/CdZnS/ZnS quantum dots.
The back segment of the core shell reaction zone is provided with rapidly rotary area and floating material discharging area, the floating material discharge Mouth is located at the floating material discharging area;
Be provided with the first to the 5th inlet by spacing distance in the front end of the core shell reaction zone, adjacent two inlet it Between distance be 100cm, it is corresponding in the rear end of the core shell reaction zone described in rapidly rotary area be provided with the 6th inlet, in the core/ The rear end of shell reaction zone is provided with three floating material outlets.
Metering injection CdSe core, 1- vaccenic acids and oleyl amine, are converted to nitrogen ring in the first inlet after vacuum exhaust Border, the temperature control of heating zone is 220~250 degrees Celsius, and reactant is because of nitrogen pressure as helical form reaction tube moves progress Heating response, the reaction time between adjacent two inlet is 10 minutes, before injecting Cd presomas and Zn in the second inlet Body is driven, continues to be moved ahead by nitrogen pressure driving a reaction thing, reaction forms first layer shell;The 3rd inlet injection Cd presomas, Zn presomas and S presomas, reaction form second layer shell;In the 4th inlet injection Cd presomas, Zn presomas and S forerunner Body, reaction form third layer shell;Zn presomas and S presomas are injected in the 5th inlet, reaction forms the 4th layer of shell, so as to To CdSe/CdZnS/ZnS quantum dots.
In order to separate the quantum dot of synthesis and impurity, reactant enters rapidly rotary area, in the 6th inlet injector Property strong ethanol, acetone, the temperature of cooling zone maintained to 0~4 degree Celsius, and reactant was led under nitrogen pressure promotion with 5 minutes The reaction tube that length is 150~200cm is crossed, as the radian of reaction tube becomes soft, impurity in light weight swims in reactant On flow through, floating material is now scavenged into by outside by floating material outlet, the CdSe/CdZnS/ZnS quantum gone after the removal of impurity Point is delivered to keeping by conveyance conduit and preserved with container.
The beneficial effects of the utility model are:Quantum dot nucleocapsid synthesizer of the present utility model can improve the steady of quantum dot It is qualitative and particle size uniform, while it can be made not have defect, therefore quantum efficiency can be maximized, so as to synthesize lifting The quantum dot of luminous efficiency and vividness, apparatus structure is rationally simple, ingenious in design, can be synthesized as needed on core more Layer housing, so as to the high-quality quantum dot met the size requirements.
Below in conjunction with the accompanying drawings with embodiment, the utility model is further illustrated.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
Embodiment
Embodiment, referring to Fig. 1, present embodiment discloses a kind of quantum dot nucleocapsid synthesizer, it include being used for carrying out core/ The core shell reaction zone of shell reaction, the reaction zone include at least one helical form reaction tube 1, on the inwall of helical form reaction tube 1 It is described provided with the reactant made in injection reaction tube with the helical form opposite direction because friction produces the approach groove of bubbling effect The leading portion of core shell reaction zone is coated with heating zone 2, and the back segment of the core shell reaction zone is coated with cooling zone 3, in the core shell The front end of reaction zone is provided with several inlets, and several floating material outlets 4, institute are provided with the rear end of the core shell reaction zone The front end for stating core shell reaction zone is connected with pressue device.
The heating zone 2, cooling zone 3 include the temperature control zone being wound on the helical form reaction tube 1, the temperature respectively Fill the full aqueous water or oil for being used to control temperature in degree control pipe, the heating zone 2, cooling zone 3 temperature control zone respectively with Heater 5, external cooler 6 connect.
The back segment of the core shell reaction zone is provided with rapidly rotary area 11 and floating material discharging area, the floating material row Outlet 4 is located at the floating material discharging area.
This rapidly in rotary area 11 tube pitch of helical form reaction tube 1 from the helical form less than core shell reaction zone leading portion The tube pitch of reaction tube 1 is from the tube pitch of the floating material discharging area is from the helical form reaction tube more than core shell reaction zone leading portion 1 tube pitch from.
Three times of the rapidly diameter of helical form reaction tube 1 of a diameter of core shell reaction zone leading portion of rotary area 11;The urgency The flexibility of fast rotary area 11 reduces 50% than the helical form reaction tube 1 of core shell reaction zone leading portion.
In the front end of the core shell reaction zone the first to the 5th inlet 75, adjacent two inlet are provided with by spacing distance Between distance be 100cm, it is corresponding in the rear end of the core shell reaction zone described in rapidly rotary area 11 be provided with the 6th inlet 76, Three floating material outlets 4 are provided with the rear end of the core shell reaction zone.
A kind of quantum dot nucleocapsid synthetic method implemented by foregoing quantum dot nucleocapsid synthesizer, it includes following step Suddenly:Will core shell reaction zone carry out vacuum exhaust after be converted to nitrogen environment, by CdSe core, 1- vaccenic acids and oleyl amine inject core/ The helical form reaction tube 1 of shell reaction zone, helical form reaction tube 1 is heated to by design temperature by heating zone 2, makes CdSe core, 1- Vaccenic acid and oleyl amine reaction, Cd presomas and Zn presomas, S presomas, Zn presomas and Cd are sequentially added by interval time Presoma, S presomas, Zn presomas and Cd presomas, and Zn presomas and S presomas, so as to accumulate multilayer on CdSe core Shell, synthesize CdSe/CdZnS/ZnS quantum dots.
The back segment of the core shell reaction zone is provided with rapidly rotary area 11 and floating material discharging area, the floating material row Outlet 4 is located at the floating material discharging area;
In the front end of the core shell reaction zone the first to the 5th inlet 75, adjacent two inlet are provided with by spacing distance Between distance be 100cm, it is corresponding in the rear end of the core shell reaction zone described in rapidly rotary area 11 be provided with the 6th inlet 76, Three floating material outlets 4 are provided with the rear end of the core shell reaction zone.
Metering injection CdSe core, 1- vaccenic acids and oleyl amine, nitrogen is converted to after vacuum exhaust in the first inlet 71 Environment, the temperature control of heating zone 2 is 220~250 degrees Celsius, and reactant is because of nitrogen pressure as helical form reaction tube 1 moves Heating response is carried out, the reaction time between adjacent two inlet is 10 minutes, and Cd presomas are injected in the second inlet 72 With Zn presomas, continue to be moved ahead by nitrogen pressure driving a reaction thing, reaction forms first layer shell;Cd is injected in the 3rd inlet 73 Presoma, Zn presomas and S presomas, reaction form second layer shell;In the 4th inlet 74 injection Cd presomas, Zn presomas With S presomas, reaction forms third layer shell;Zn presomas and S presomas are injected in the 5th inlet 75, reaction forms the 4th layer Shell, so as to obtain CdSe/CdZnS/ZnS quantum dots.
In order to separate the quantum dot of synthesis and impurity, reactant enters rapidly rotary area 11, in the note of the 6th inlet 76 Enter the strong ethanol of polarity, acetone, the temperature of cooling zone 3 is maintained to 0~4 degree Celsius, and reactant is under nitrogen pressure promotion with 5 points Clock is by the reaction tube that length is 150~200cm, and as the radian of reaction tube becomes soft, impurity in light weight swims anti- Answer and flowed through on thing, floating material is now scavenged into by outside by floating material outlet 4, the CdSe/CdZnS/ZnS gone after the removal of impurity Quantum dot is delivered to keeping by conveyance conduit 8 and preserved with container.
The size and emission wavelength of quantum dot can be depending on the wavelength of core, the quantity of shell, in order that quantum dot becomes big, meeting Relatively large number of shell is accumulated, but can so reduce the characteristics of luminescence, therefore the housing number of plies recommended is 4~6 layers.
Quantum dot nucleocapsid synthesizer of the present utility model can improve quantum dot stability and particle size it is uniform, together When it can be made not have defect, therefore quantum efficiency can be maximized, so as to synthesize the amount for improving luminous efficiency and vividness Sub-, apparatus structure is rationally simple, ingenious in design, can the synthesizing multilayer housing on core as needed, so as to obtain meeting chi The high-quality quantum dot of very little requirement.
In other embodiments, core and core, shell can by ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, HgTe、MgS、MgSe、MgTe、CaS、CaSe、CaTe、SrS、SrSe、SrTe、BaS、BaSe、BaTe、GaN、GaP、GaAs、 Make a choice in the group of GaSb, InN, InP, InSb, Ge, Si and these combination compositions, and as needed, reacted in nucleocapsid These more than one combinations or lattice constant can be synthesized between the quantum dot core and quantum dot shell in area again by analogous element group Into quantum dot cushion.
It is described above, only it is preferred embodiment of the present utility model, not the utility model is made any formal Limitation.Any those skilled in the art, it is all available in the case where not departing from technical solutions of the utility model ambit The technological means and technology contents of the disclosure above make many possible changes and modifications to technical solutions of the utility model, or repair It is changed to the equivalent embodiment of equivalent variations.Therefore every content without departing from technical solutions of the utility model, according to the utility model The equivalence changes made of shape, construction and principle, all should be covered by the scope of protection of the utility model.

Claims (6)

  1. A kind of 1. quantum dot nucleocapsid synthesizer, it is characterised in that:It includes being used for the core shell reaction zone for carrying out core shell reaction, The reaction zone includes at least one helical form reaction tube, and the helical form reaction tube is provided with and the helical form opposite direction The reactant made in injection reaction tube because friction produce bubbling effect approach groove, the core shell reaction zone leading portion cladding There is heating zone, the back segment of the core shell reaction zone is coated with cooling zone, and several are provided with the front end of the core shell reaction zone Inlet, several floating material outlets, the front end connection of the core shell reaction zone are provided with the rear end of the core shell reaction zone There is pressue device.
  2. 2. quantum dot nucleocapsid synthesizer according to claim 1, it is characterised in that the heating zone, cooling zone difference The full liquid for being used to control temperature is filled including the temperature control zone being wound on the helical form reaction tube, in the temperature control zone State water or oil, the heating zone, the temperature control zone of cooling zone are connected with heater, external cooler respectively.
  3. 3. quantum dot nucleocapsid synthesizer according to claim 1, it is characterised in that the back segment of the core shell reaction zone Provided with rapidly rotary area and floating material discharging area, the floating material outlet is located at the floating material discharging area.
  4. 4. quantum dot nucleocapsid synthesizer according to claim 3, it is characterised in that the rapidly helical form in rotary area The tube pitch of reaction tube from the helical form reaction tube less than core shell reaction zone leading portion tube pitch from the floating material discharging area Tube pitch from the helical form reaction tube more than core shell reaction zone leading portion tube pitch from.
  5. 5. quantum dot nucleocapsid synthesizer according to claim 3, it is characterised in that the rapidly rotary area it is a diameter of Three times of the helical form reaction tube diameter of core shell reaction zone leading portion;Before the flexibility of the rapidly rotary area is than core shell reaction zone The helical form reaction tube of section reduces 50%.
  6. 6. quantum dot nucleocapsid synthesizer according to claim 3, it is characterised in that before the core shell reaction zone End is provided with the first to the 5th inlet by spacing distance, in rapidly rotary area is set described in the correspondence of the rear end of the core shell reaction zone There is the 6th inlet, three floating material outlets are provided with the rear end of the core shell reaction zone.
CN201720426276.5U 2017-04-21 2017-04-21 Quantum dot nucleocapsid synthesizer Active CN206828441U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018192540A1 (en) * 2017-04-21 2018-10-25 东莞市睿泰涂布科技有限公司 Quantum dot core-shell synthesis device and quantum dot core-shell synthesis method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018192540A1 (en) * 2017-04-21 2018-10-25 东莞市睿泰涂布科技有限公司 Quantum dot core-shell synthesis device and quantum dot core-shell synthesis method

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Address after: 523000 No.68, Qiaotou Dongxin Road, Qiaotou town, Dongguan City, Guangdong Province

Patentee after: Dongguan Lijing New Material Technology Co., Ltd

Address before: 523000 A building, 12 East Xin Lu, community community, Qiaotou town, Dongguan, Guangdong

Patentee before: DONGGUAN RETECK COATING TECHNOLOGY Co.,Ltd.