CN109216512A - A kind of QLED device and preparation method thereof, high-pressure treatment apparatus - Google Patents

A kind of QLED device and preparation method thereof, high-pressure treatment apparatus Download PDF

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Publication number
CN109216512A
CN109216512A CN201710542314.8A CN201710542314A CN109216512A CN 109216512 A CN109216512 A CN 109216512A CN 201710542314 A CN201710542314 A CN 201710542314A CN 109216512 A CN109216512 A CN 109216512A
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pressure treatment
preparation
transport layer
qled device
high pressure
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CN109216512B (en
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王宇
曹蔚然
钱磊
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TCL Corp
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/04Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
    • H01L33/06Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005Processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/14Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008Processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008Processes
    • H01L2933/0033Processes relating to semiconductor body packages

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The present invention discloses a kind of QLED device and preparation method thereof, high-pressure treatment apparatus, wherein the preparation method includes after function transport layer is completed to deposit on device, in an inert atmosphere, the step of to function transport layer progress HIGH PRESSURE TREATMENT.The present invention is by carrying out HIGH PRESSURE TREATMENT to function transport layer, keep each functional layer material combination in QLED device finer and close, what is combined between function transport layer and quantum dot light emitting layer is closer, reduce the defect between interface, non-radiative recombination is reduced, the injection efficiency of carrier and the efficiency of recombination luminescence are further improved.

Description

A kind of QLED device and preparation method thereof, high-pressure treatment apparatus
Technical field
The present invention relates to technology of quantum dots field more particularly to a kind of QLED device and preparation method thereof, HIGH PRESSURE TREATMENTs to fill It sets.
Background technique
That semiconductor-quantum-point (Quantum dot, QDs) has that fluorescence quantum efficiency is high, visible light wave range shines is adjustable, The features such as colour gamut coverage is broad.It is referred to as light emitting diode with quantum dots by the light emitting diode of luminescent material of quantum dot (Quantum dot light-emitting diode, QLED), have color saturation, efficiency is higher, colour temperature more preferably, the service life The advantages that long, is expected to become the mainstream technology of next-generation solid-state lighting and FPD.
In order to improve the efficiency and performance of QLED device, most researchers mainly carry out quantum dot light emitting layer material Research, only a few studies person studies the function transport layer of QLED device, and the prior art is to function transport layer Research is also only limitted to modify to improve the efficiency of device QLED device function transmission layer material by the method for chemistry.
However, the function transport layer of QLED device is modified using the method for physics in device fabrication process, with The research for improving device film quality and carrier transport efficiency is but rarely reported.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of QLED device and preparation method thereof, High-pressure treatment apparatus, by carrying out physical modification to function transport layer in device fabrication process, it is intended to pass through physical method reality The raising of existing QLED device film quality and carrier transport efficiency.
Technical scheme is as follows:
A kind of preparation method of QLED device, wherein including when function transport layer completed on device deposition after, in inert environments Under, to the function transport layer carry out HIGH PRESSURE TREATMENT the step of.
Further, the preparation method of the QLED device, wherein the function transport layer be hole transmission layer and/ Or electron transfer layer.
Further, the preparation method of the QLED device, wherein the pressure of HIGH PRESSURE TREATMENT is carried out to function transport layer For 0.1-10MPa, time 5-120min.
In a kind of wherein embodiment, the preparation method of the QLED device, wherein the process of the HIGH PRESSURE TREATMENT Include: S10, after function transport layer completes deposition on device, device is fixed on to the closed container of a high-pressure treatment apparatus In, the high-pressure treatment apparatus further includes that inert gas is passed through by intake valve and air outlet valve by opening intake valve and air outlet valve Closed container and by the air clean in closed container;S20, air outlet valve is closed, continues to be passed through inert gas until closed container Interior pressure reaches predetermined pressure, HIGH PRESSURE TREATMENT predetermined time.It further, further include step after the completion of the step S20 S30, air outlet valve is opened, and adjusts air outlet valve and intake valve pressure, closed container is made to form the inert gas of flowing, remove device The inert gas of adsorption.The inert gas is one of nitrogen, helium, neon or argon gas.
Further, the preparation method of the QLED device, wherein further include the function transport layer through HIGH PRESSURE TREATMENT Afterwards, the step of being made annealing treatment.
Further, the preparation method of the QLED device, wherein the function transport layer is moved back after HIGH PRESSURE TREATMENT The annealing temperature of fire processing is 50-200 DEG C, time 10-30min.
The present invention also provides a kind of QLED devices being prepared by any one method of the present invention.
Further, the present invention also provides a kind of high-pressure treatment apparatus of QLED device, wherein including a closed container, One is provided in the closed container for fixing the bracket of QLED device, described closed container one end is connected with admission line, The other end is connected with outlet pipe, and intake valve and first pressure gauge, the outlet pipe connection are provided on the admission line There are air outlet valve and second pressure gauge, the other end of the admission line is connected with inert gas gas cylinder.
The utility model has the advantages that the present invention carries out HIGH PRESSURE TREATMENT by the function transport layer to QLED device, make in QLED device The transmission layer material combination of each function is finer and close, combines closer between each function transport layer, reduces the defect between interface, Non-radiative recombination is reduced, the injection efficiency of carrier and the efficiency of recombination luminescence are further increased, to promote QLED The whole efficiency of device.
Detailed description of the invention
Fig. 1 is the flow chart of HIGH PRESSURE TREATMENT process preferred embodiment of the present invention;
Fig. 2 is a kind of structural schematic diagram of the preferred embodiment of the high-pressure treatment apparatus of QLED device of the present invention;
Fig. 3 is the structural schematic diagram of eurymeric QLED device preferred embodiment in the embodiment of the present invention 1;
Fig. 4 is the structural schematic diagram of transoid QLED device preferred embodiment in the embodiment of the present invention 2.
Specific embodiment
The present invention provides a kind of QLED devices and preparation method thereof, high-pressure treatment apparatus, to make the purpose of the present invention, skill Art scheme and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that tool described herein Body embodiment is only used to explain the present invention, is not intended to limit the present invention.
The prior art during preparing QLED device, transmit layer material and combine not fine and close, each function transport layer by function Between between usually there will be boundary defect, easily lead to carrier efficiency of transmission reduce.For this purpose, the present invention mainly passes through pair The function transport layer of QLED device carries out HIGH PRESSURE TREATMENT, by carrying out further high pressure effect, energy to the function transport layer The compactness combined between adjacent film layers is enough significantly improved, the defect between interface is reduced, to improve the biography of carrier The efficiency of defeated efficiency and recombination luminescence.Function transport layer of the invention includes electron injecting layer, electron transfer layer, hole injection layer And hole transmission layer, preferably adjacent with quantum dot light emitting layer electron transfer layer and/or hole transmission layer.
Electron transport layer materials of the invention there is no limit, can for the common N-shaped ZnO with electronic transmission performance, TiO2, can also be the Ca of low work function, and the metals such as Ba can also be the compounds material such as ZrO2, CsF, LiF, CsCO3 and Alq3 Material is other electron transport materials.
Hole transport layer material of the invention can be PEDOT:PSS, nickel oxide, molybdenum oxide, vanadium oxide, copper oxide, sulphur Change copper, copper rhodanide, cupric iodide etc. and other hole mobile materials.
After function transport layer completes deposition on device, in an inert atmosphere, device is placed in a closed container The step of middle progress HIGH PRESSURE TREATMENT.In order to guarantee pressing result, fine and close film is formed, the pressure of HIGH PRESSURE TREATMENT should be greater than 1MPa, time 5-120min.It is verified through inventor's many experiments, it is preferred that the pressure of the HIGH PRESSURE TREATMENT is greater than 4MPa.Into One step is preferred, is greater than 6MPa.Due to biggish pressure the high requirements on the equipment, and it is be easy to cause device failure, at high pressure The pressure of reason should be less than 10MPa.
Further, in a specific embodiment, as shown in Figure 1, the process of HIGH PRESSURE TREATMENT of the invention is specific Comprising steps of
S10, when function transport layer completed on device deposition after, device is fixed on to the closed container of a high-pressure treatment apparatus In, the high-pressure treatment apparatus further includes that inert gas is passed through by intake valve and air outlet valve by opening intake valve and air outlet valve Closed container and by the air clean in closed container;
S20, air outlet valve is closed, continues to be passed through inert gas until the pressure in closed container reaches predetermined pressure, HIGH PRESSURE TREATMENT Predetermined time.
Further, after the completion of the step of S20, air inlet can be controlled with further progress step S30, opening air outlet valve The pressure of valve and air outlet valve makes the inert gas that flowing is formed in closed container, removes the inert gas of device adsorption.
In the present invention, it carries out HIGH PRESSURE TREATMENT to function transport layer to realize in an inert atmosphere, the indifferent gas Body can be nitrogen, helium, neon or argon gas etc..
Further, the present invention also provides a kind of high-pressure treatment apparatus of QLED device, as shown in Fig. 2, the high pressure Processing unit includes a closed container 10, and a bracket 20 for being used to fix device to be processed is provided in the closed container 10, Described 10 one end of closed container is connected with admission line 30, and the other end is connected with outlet pipe 40, sets on the admission line 30 It is equipped with intake valve 31 and first pressure gauge 32, is provided with air outlet valve 41 and second pressure gauge 42 on the outlet pipe 40;It is described The other end of admission line 30 connects inert gas gas cylinder 50.
Specifically, in the step S10, before carrying out HIGH PRESSURE TREATMENT, device is first fixed on to the branch of closed container 10 In frame 20, intake valve 31 and air outlet valve 41 are then opened simultaneously, is passed through inert gas for the air clean in closed container 10, from And prevent the oxygen in air from having an effect under high pressure with function transport layer each in device, influence the performance of device.
In the step S20, by the air clean in closed container 10 it is complete after, close air outlet valve 41, continue to be passed through lazy Property gas until reaching scheduled pressure value 1-10MPa in closed container, continuous high-pressure handles 5-120min.
In the step S30, air outlet valve 41 is opened, the pressure of intake valve 31 and air outlet valve 41 is controlled, makes closed container 10 The interior inert gas for forming flowing, avoids device surface from being adsorbed with inert gas as far as possible.This is because device is after HIGH PRESSURE TREATMENT, Its surface can adsorb inert gas, be easy to cause in device between neighboring layers and combine not closely, and influence the transmission of carrier Rate.By the pressure between control intake valve and air outlet valve, so that the pressure of intake valve is greater than the pressure of the air outlet valve, formed Inert gas flows, to the inert gas of device surface absorption be removed clean.
Further, the invention also includes the steps after carrying out HIGH PRESSURE TREATMENT to function transport layer, made annealing treatment Suddenly.The function transport layer need to also continue to deposit quantum dot light emitting layer or the transmission of another function on its surface after HIGH PRESSURE TREATMENT Layer, in order to ensure during depositing quantum dot light emitting layer or another function transport layer, the function is transmitted in layer material Solute component will not be washed away by the solvent composition in quantum dot light emitting layer or another function transport layer, be needed in advance to the function Energy transport layer is made annealing treatment, and the annealing temperature of the function transport layer is 50-200 DEG C, preferably 120 DEG C -180 DEG C, time 10-30min.
Explanation is further explained below by the specific embodiment preparation method for improving QLED device a kind of to the present invention:
The preparation of 1 eurymeric QLED device of embodiment
As shown in figure 3, the eurymeric QLED device successively includes substrate 100, hearth electrode 200, hole injection layer from bottom to up 300, hole transmission layer 400, quantum dot light emitting layer 500, electron transfer layer 600 and top electrode 700, specific preparation process are as follows It is shown:
1) glass substrate 100 first, is placed on ultrapure water, acetone water and isopropanol first to be cleaned by ultrasonic, every step cleaning Time be 15 minutes, glass substrate is dried up after the completion of the ultrasound with nitrogen gun, drying in oven is placed in, after being cleaned Glass substrate 100 is spare;
2), in glass substrate after cleaning, pass through the ITO electrode of mask plate one pattern layers of sputtering sedimentation on it, i.e. bottom Electrode 200, ITO electrode with a thickness of 50nm;
3) one layer of hole injection layer 300, is deposited in the hearth electrode 200,300 material of hole injection layer is PEDOT:PSS, After the completion of to be deposited, 150 DEG C of annealing 15min are carried out;
4) one layer of hole transmission layer 400, is deposited on hole injection layer 300,400 material of hole transmission layer is TFB, then by it It is put into closed container as shown in Figure 2 and carries out HIGH PRESSURE TREATMENT, the pressure of HIGH PRESSURE TREATMENT is 5MPa, and the HIGH PRESSURE TREATMENT time is 30min after the completion of HIGH PRESSURE TREATMENT, is made annealing treatment, and annealing temperature is 150 DEG C, time 15min;
5) one layer of quantum dot light emitting layer 500, is deposited on hole transmission layer 400,500 material of quantum dot light emitting layer is red quantum Point material;After the completion of deposition, the quantum dot light emitting layer is made annealing treatment, annealing temperature is 60 DEG C, time 10min.
6) one layer of electron transfer layer 600, is deposited on quantum dot light emitting layer 500,600 material of electron transfer layer is N-shaped Device is put into closed container as shown in Figure 2 after depositing to the layer and carries out HIGH PRESSURE TREATMENT by ZnO, the pressure of HIGH PRESSURE TREATMENT Power is 7MPa, time 2h, after the completion of HIGH PRESSURE TREATMENT, continues to twist annealing, annealing temperature is 150 DEG C, time 15min;
7), the device for having deposited each functional layer is placed in vapor deposition storehouse to the top electrode for passing through one layer of 100nm of mask plate hot evaporation 700, the top electrode material is Ag;
8), after the completion of device vapor deposition, it is packaged, common machine encapsulation can be used also can be used and is simpler Encapsulation manually, obtains the eurymeric QLED device of the present embodiment.
The preparation of 2 transoid QLED device of embodiment
As shown in figure 4, the transoid QLED device successively includes substrate 100, hearth electrode 200, electron transfer layer from bottom to up 600, quantum dot light emitting layer 500, hole transmission layer 400 and top electrode 700, specific preparation process are as follows:
1) mica sheet substrate 100 first, is placed on ultrapure water, acetone water and isopropanol first to be cleaned by ultrasonic, every step is clear The time washed is 15 minutes, dries up mica sheet substrate with nitrogen gun after the completion of ultrasound, is placed in drying in oven, is cleaned Mica sheet substrate 100 afterwards is spare;
2), on mica sheet substrate after cleaning, by the ITO electrode of mask plate one pattern layers of sputtering sedimentation on it, i.e., Hearth electrode 200, ITO electrode with a thickness of 70nm;
3) one layer of electron transfer layer 600, is deposited on the substrate containing hearth electrode, the material of electron transfer layer 600 is Alq3;To After the layer deposits, then device is put into closed container as shown in Figure 2 and carries out HIGH PRESSURE TREATMENT, the pressure of HIGH PRESSURE TREATMENT For 6MPa, the time of HIGH PRESSURE TREATMENT is 2h, after the completion of HIGH PRESSURE TREATMENT, is made annealing treatment, and annealing temperature is 80 DEG C, and the time is 15min;
4) one layer of quantum dot light emitting layer 500, is deposited on electron transfer layer 600, the material of quantum dot light emitting layer is blue light quantum Point material;After the completion of deposition, the quantum dot light emitting layer is made annealing treatment, annealing temperature is 80 DEG C, time 20min.
5) one layer of hole transmission layer 400, is deposited on quantum dot light emitting layer 500, the material of hole transmission layer 400 is Device is put into closed container as shown in Figure 2 and carries out HIGH PRESSURE TREATMENT by Poly-TPD, and the pressure of HIGH PRESSURE TREATMENT is 10MPa, place The reason time is 1.5h, is made annealing treatment later, and annealing temperature is 120 DEG C, time 5min;
6), the device for having deposited each functional layer is placed in vapor deposition storehouse to the top electrode 700 for passing through one layer of 80nm of mask plate hot evaporation, The top electrode material is Al.
7), after the completion of device vapor deposition, it is packaged, common machine encapsulation, which can be used, also can be used simply Manual encapsulation, obtain the transoid QLED device of the present embodiment.
In conclusion the present invention provides a kind of preparation method of QLED device, by the quantum prepared by nano material Point luminescent layer carries out HIGH PRESSURE TREATMENT, forms it into fine and close film, and the nano material generates certain knot under high pressure effect Crystallization then improves the carrier transport rate of quantum dot light emitting layer;Further, function of the present invention also to QLED device Transport layer carry out HIGH PRESSURE TREATMENT so that the function transport layer in QLED device and combined between quantum dot light emitting layer it is closer, Reduce the defect between interface, reduce non-radiative recombination, further improve carrier injection efficiency and compound hair The efficiency of light, to promote the whole efficiency of QLED device.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention Protect range.

Claims (10)

1. a kind of preparation method of QLED device, which is characterized in that including when function transport layer completed on device deposition after, Under inert environments, to the function transport layer carry out HIGH PRESSURE TREATMENT the step of.
2. the preparation method of QLED device according to claim 1, which is characterized in that the function transport layer is hole Transport layer and/or electron transfer layer.
3. the preparation method of QLED device described in -2 any one according to claim 1, which is characterized in that the HIGH PRESSURE TREATMENT Pressure be 0.1-10MPa, time 5-120min.
4. the preparation method of QLED device described in -2 any one according to claim 1, which is characterized in that the HIGH PRESSURE TREATMENT Process include the following steps:
(1) after completing deposition on device when function transport layer, device is fixed in the closed container of a high-pressure treatment apparatus, The high-pressure treatment apparatus further includes that inert gas is passed through close by intake valve and air outlet valve by opening intake valve and air outlet valve Close container and by the air clean in closed container;
(2) air outlet valve is closed, continues to be passed through inert gas until the pressure in closed container reaches predetermined pressure, HIGH PRESSURE TREATMENT is pre- It fixes time.
5. the preparation method of QLED device according to claim 4, which is characterized in that after the completion of the step (2), open Air outlet valve, and air outlet valve and intake valve pressure are adjusted, so that closed container is formed the inert gas of flowing, removes device adsorption Inert gas.
6. the preparation method of QLED device according to claim 4, which is characterized in that the inert gas is nitrogen, helium One of gas, neon or argon gas.
7. the preparation method of QLED device described in -2 any one according to claim 1, which is characterized in that further include the function Energy transport layer is after HIGH PRESSURE TREATMENT, the step of annealing.
8. the preparation method of QLED device according to claim 7, which is characterized in that the function transport layer is through high pressure After processing, the annealing temperature of annealing is 50-200 DEG C, time 10-30min.
9. a kind of QLED device, which is characterized in that the preparation method as described in claim 1-8 any one is prepared.
10. a kind of high-pressure treatment apparatus of QLED device, which is characterized in that including a closed container, set in the closed container One is equipped with for fixing the bracket of QLED device, described closed container one end is connected with admission line, and the other end is connected with outlet Pipeline, intake valve and first pressure gauge are provided on the admission line, and the outlet pipe is connected with air outlet valve and the second pressure Power table, the other end of the admission line are connected with inert gas gas cylinder.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022143553A1 (en) * 2020-12-31 2022-07-07 Tcl科技集团股份有限公司 Method for preparing quantum dot light emitting diode device

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CN1164934A (en) * 1995-08-31 1997-11-12 株式会社东芝 Blue light emitting element and method for manufacturing same
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KR20140077257A (en) * 2012-12-12 2014-06-24 연세대학교 산학협력단 Method for manufacturing colloidal quantum dot thin film and quantum dot solar cells
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Publication number Priority date Publication date Assignee Title
CN1164934A (en) * 1995-08-31 1997-11-12 株式会社东芝 Blue light emitting element and method for manufacturing same
CN1828976A (en) * 2005-03-04 2006-09-06 日本东北先锋公司 Method and apparatus for fabricating self-emission device
US20070241351A1 (en) * 2006-04-14 2007-10-18 Applied Materials, Inc. Double-sided nitride structures
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022143553A1 (en) * 2020-12-31 2022-07-07 Tcl科技集团股份有限公司 Method for preparing quantum dot light emitting diode device

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