CN112095077B - OLED device and evaporation method thereof - Google Patents
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Abstract
An evaporation method of an OLED device comprises the following process steps: 1) carrying out evaporation pretreatment on the ITO substrate; 2) sequentially laminating an evaporation-plated hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate; 3) placing a luminescent guest material and a hole type host material in the same rotating tray by adopting a ternary evaporation mode, placing an electronic type host material outside the rotating tray, heating the hole type host material after the evaporation rate of the luminescent guest material is stable, starting the rotating tray, controlling the rotating speed of the rotating tray to be 10-15 r/min, and opening a baffle to carry out evaporation continuously to obtain a luminescent layer; 4) and sequentially laminating an evaporation electron transmission layer, an electron injection layer and a cathode on the light-emitting layer to obtain the finished product of the OLED device. The evaporation method effectively avoids the quenching phenomenon between the cavity type main body and the electron type main body, and greatly improves the service life and the luminous efficiency of the OLED device.
Description
Technical Field
The invention belongs to the field of OLED and particularly relates to an OLED device and an evaporation method thereof.
Background
In recent years, Organic Light Emitting Diodes (OLEDs) have received much attention from academic and industrial fields as a lighting and display technology with great application prospects. The phosphorescent material of the iridium complex has been developed more mature, but is blocked by foreign patents, and China begins to turn to the research on the phosphorescent material of the platinum complex.
The platinum complex forms a planar structure relative to the octahedral structure of the iridium complex. Such organic planar structures readily form pi-pi bonds upon aggregation. However, the pi-pi combination has the advantages and disadvantages that the energy transfer and electron transfer performance between organic materials are enhanced, the rigidity of the materials is increased due to the more compact stacking of the materials, the service life of the device is better, and the defects that exciton quenching is easy to occur when the exciton concentration of the materials is too high, so that the service life and the efficiency of the OLED are reduced.
In the light emitting layer structure of the dual host, the two hosts form a radical excited complex, and then the excited energy is transferred to the light emitting guest to emit light. In this process, there is a possibility that collision quenching occurs between the electron-type host and the hole-type host, and the platinum complex itself exciton collision quenching also occurs, so that it is difficult to avoid reduction in the lifetime and efficiency of the OLED. Therefore, how to avoid pi-pi combination between two hosts and the occurrence of pi-pi combination of a light-emitting object in the evaporation process is a great problem to be solved urgently in the industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an OLED device and an evaporation method thereof.
The technical scheme adopted by the invention is as follows: an evaporation method of an OLED device comprises the following process steps:
1) carrying out evaporation pretreatment on the ITO substrate;
2) placing an ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 2.0-4.0E-5 Pa, and sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate;
3) adopting a ternary evaporation mode, placing a light-emitting object material and a hole type host material in the same rotating tray, placing an electron type host material outside the rotating tray, heating the electron type host material and the light-emitting object material in sequence, heating the hole type host material after the evaporation rate of the light-emitting object material is stable, and when the evaporation rate of the light-emitting object material and the hole type host material reaches the evaporation rateWhen the luminescent layer is formed, starting the rotary tray, controlling the rotating speed of the rotary tray to be 10-15 r/min, and opening the baffle plate to continue evaporation to obtain the luminescent layer;
4) and sequentially laminating an evaporation electron transmission layer, an electron injection layer and a cathode on the light-emitting layer to obtain the finished product of the OLED device.
Specifically, the ternary evaporation mode in step 3) of the invention utilizes the principle that the vapor of the luminescent guest material and the vapor of the hole type host material which are placed in the same rotating tray in the evaporation process can be preferentially mixed for evaporation through rotation and then mixed for evaporation with the vapor of the electron type host material outside the rotating tray, so that more pi-pi combinations are formed between the luminescent guest material and the hole type host material, the normal functions of the luminescent guest and the hole type host can be realized, the phenomenon that the electron type host and the hole type host are easily quenched is effectively slowed down, and the service life and the luminous efficiency of the luminescent layer are improved.
As a further improvement of the scheme, the cavity type host material in the step 3) is DPQP, and the chemical structural formula of the cavity type host material is shown in the specificationCan effectively form more pi-pi combination with the luminous object material in the process of mixed evaporation. The cavity type host material can be obtained by adopting the following synthetic route:
the hole-type host material can better highlight the planar characteristic of a light-emitting object material, particularly the planar characteristic of a platinum complex, so that the light-emitting direction is more consistent, the coupling coefficient is higher, and the device efficiency is improved by 8-12%.
The hole injection layer in step 2) of the present invention is prepared by heating terphenylamine derivative (such as E051 product available from Angele photoelectric materials, Inc., Guangdong) to 230-240 deg.C at a rate ofMeanwhile, the tetrafluorobenzonitrile is heated to 260-270 ℃, and the tetrafluorobenzonitrile are prepared by doping and evaporating according to the proportion of 3%. The hole transport layer is heated to 230-240 ℃ by adopting terphenylamine derivatives at a rateAnd is formed by evaporation. The electron blocking layer is prepared by heating spirofluorene derivative (such as E081 product obtained from Arleiya, Guangdong Co., Ltd.) to 220-230 deg.C at a rate And is formed by evaporation.
The electron transport layer in the step 4) of the invention is prepared by heating 8-hydroxyquinoline Lithium (LiQ) and anthracene derivative (such as 11518 product from Argle electro-optical materials, Inc. of Guangdong) to 280-290 deg.C at a rateMixing and evaporating to obtain the final product. The electron injection layer is heated to 1000 +/-100 ℃ by metal Yb at a rateAnd is formed by evaporation. The cathode is heated to 1200 +/-100 ℃ by adopting metal Ag at a speed rateAnd is formed by evaporation.
As a further improvement of the above scheme, the light-emitting guest material in step 3) is a platinum compound, which has a strong compatibility with the hole-type host material of the present invention.
As a further improvement of the scheme, the electronic type host material in the step 3) is a derivative of 2,4, 6-triphenyl-1, 3, 5-triazine. Specifically, the chemical structural formula of the 2,4, 6-triphenyl-1, 3, 5-triazine derivative described in the invention can be selected from one of the following, but is not limited thereto.
As a further improvement of the scheme, the heating temperature of the electronic type main body material in the step 3) is 220-230 ℃, and the evaporation rate isThe heating temperature of the light-emitting object material is 250-260 ℃, and the evaporation rate is The heating temperature of the cavity type main body material is 220-230 ℃. Specifically, in the evaporation process, the electron-type host material and the hole-type host material are mixed according to the mass ratio of 1:1, so that the balance of electron and hole can be ensured, the heating temperature and the evaporation rate of the light-emitting object material are limited, the concentration of the light-emitting object material is moderate, and the light-emitting efficiency and the service life of the light-emitting object material are better.
As a further improvement of the scheme, the pre-evaporation treatment in the step 1) comprises the steps of sequentially brushing the ITO substrate with a cleaning solution, ultrasonically cleaning the ITO substrate with the cleaning solution and repeatedly carrying out pure water ultrasonic cleaning for three times, then baking the ITO substrate, placing the ITO substrate in a vacuum sample feeding chamber, vacuumizing until the vacuum degree is 3.0-5.0E-0.4 Pa and the rotating speed of a rotating tray is 10-15 r/min. Specifically, the ultrasonic cleaning of the cleaning solution can remove impurities such as oil stains, dust and the like, and the film forming quality is ensured; removing residual cleaning liquid and avoiding water stain after baking by pure water ultrasonic cleaning; the moisture of the panel can be removed through subsequent baking; the panel is kept in a low water-oxygen state by being stored in a vacuum chamber (water and oxygen can seriously affect the efficiency and the service life of the device).
The OLED device obtained by the evaporation method comprises an ITO anode, a hole injection layer, a hole transport layer, an electron blocking layer, a light emitting layer, an electron transport layer, an electron injection layer and an Ag cathode which are sequentially stacked from top to bottom, and the OLED device has the working principle that: on one hand, holes enter the device from an ITO anode, the energy level difference between the ITO and an organic layer is reduced through a hole injection layer, the starting voltage can be reduced, the hole transmission layer mainly controls the transmission rate of the holes, the electron transmission rate of the device is higher than that of the holes, an electron blocking layer is arranged to prevent electrons and the holes from being combined to emit light on other layers, on the other hand, the electrons enter the device from an Ag cathode, Yb and Ag are both metals which are in ohmic contact, the electrons are smoothly injected into the Yb, the work function of the Yb is more matched with the LUMO of the electron transmission layer, the electrons smoothly reach the electron transmission layer, and finally the electrons are transmitted to a light emitting layer to be combined with the holes, so that the light emitting is realized.
The invention has the beneficial effects that:
the evaporation method realizes the purpose of preferentially mixing the hole type host material and the light-emitting object material by improving the evaporation mode of the light-emitting layer, so that more pi-pi combinations are formed between the hole type host material and the light-emitting object material, thus slowing down the pi-pi combination formed by the light-emitting object material and the pi-pi combination formed between the electron type host material and the hole type host material, effectively avoiding the quenching phenomenon between the hole type host and the electron type host, and greatly improving the service life and the light-emitting efficiency of the OLED device.
The OLED device prepared by the invention can be effectively improved by 15-20% in service life.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It is to be expressly understood that the examples are for illustrative purposes only and are not to be construed as limiting the scope of the present invention, as those skilled in the art will appreciate that various modifications and adaptations of the present invention as set forth herein are possible and can be made without departing from the spirit and scope of the present invention. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercial products; the process steps or preparation methods not mentioned in detail are all process steps or preparation methods known to the person skilled in the art.
Example 1
An OLED device comprises an ITO anode, a hole injection layer, a hole transmission layer, an electron blocking layer, a light emitting layer, an electron transmission layer, an electron injection layer and an Ag cathode which are sequentially stacked from top to bottom, wherein the evaporation method of the OLED device comprises the following process steps:
1) carrying out evaporation pretreatment on the ITO substrate: sequentially brushing cleaning liquid, ultrasonically cleaning the cleaning liquid and repeatedly ultrasonically cleaning pure water for three times on the ITO substrate, then baking the ITO substrate, and placing the ITO substrate in a vacuum sample injection chamber for vacuumizing until the vacuum degree is 5.0E-0.4Pa and the rotating speed of a rotating tray is 5 r/min;
2) placing the pretreated ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 2.0E-5Pa, sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate, wherein the hole injection layer is formed by heating terphenylamine derivative (such as E051 product from Arleiya Guangdong photoelectric materials Co., Ltd.) to 235 deg.C at a rateSimultaneously, the tetrafluorobenzonitrile is heated to 265 ℃, and the tetrafluorobenzonitrile are formed by doping and evaporation according to 3 percent. The hole transport layer is heated to 235 deg.C with terphenylamine derivativeAnd is formed by evaporation. The electron blocking layer is prepared by heating a spirofluorene derivative (e.g. type E081 from Argerya, Guangdong Co.) to 225 deg.C at a rateIndependently evaporating and plating;
3) a ternary evaporation mode is adopted, a platinum compound (a luminescent object material) and DPQP (a cavity type host material) are placed in the same rotating tray, and a derivative (an electron type host material, the chemical structural formula of which is shown in the specification) of 2,4, 6-triphenyl-1, 3, 5-triazine is placed in the rotating tray) Placing outside the rotating tray, sequentially heating 2,4, 6-triphenyl-1, 3, 5-triazine derivative (heating temperature is 225 deg.C, evaporation rate is) And platinum compound (heating temperature 255 ℃ C., evaporation rate) Heating DPQP to 225 ℃ after the evaporation rate of the platinum compound is stabilizedWhen the evaporation rate of the platinum compound and the DPQP is reachedWhen the luminescent layer is formed, starting the rotary tray, controlling the rotating speed of the rotary tray to be 10r/min, and opening the baffle plate to carry out evaporation continuously to obtain the luminescent layer;
4) sequentially laminating an electron transport layer, an electron injection layer and a cathode on the light-emitting layer, wherein the electron transport layer is prepared by heating 8-hydroxyquinoline Lithium (LiQ) and anthracene derivative (such as 11518 product from Argerya, Guangdong) to 285 deg.CMixing and evaporating to obtain the final product. The electron injection layer is formed by heating metal Yb to 1000 deg.C at a rateAnd is formed by evaporation. The cathode is heated to 1200 ℃ by adopting metal Ag at a speed rateAnd (4) independently evaporating to obtain the finished product of the OLED device in the embodiment 1.
Example 2
An OLED device comprises an ITO anode, a hole injection layer, a hole transmission layer, an electron blocking layer, a light emitting layer, an electron transmission layer, an electron injection layer and an Ag cathode which are sequentially stacked from top to bottom, wherein the evaporation method of the OLED device comprises the following process steps:
1) carrying out evaporation pretreatment on the ITO substrate: sequentially brushing cleaning liquid, ultrasonically cleaning the cleaning liquid and repeatedly carrying out pure water ultrasonic cleaning for three times on the ITO substrate, then baking the ITO substrate, placing the ITO substrate in a vacuum sample injection chamber, vacuumizing until the vacuum degree is 3.0E-0.4Pa and the rotating speed of a rotating tray is 12 r/min;
2) placing the pretreated ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 4.0E-5Pa, and sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate, wherein the hole injection layer is used for injecting holesThe interlayer is prepared by heating terphenylamine derivative (such as E051 product from Argerya, Guangdong) to 230 deg.C at a rateSimultaneously, the tetrafluorobenzonitrile and the fluorobenzonitrile are heated to 270 ℃, and the tetrafluorobenzonitrile and the fluorobenzonitrile are formed by doping and evaporation according to 3 percent. The hole transport layer is heated to 230 deg.C with terphenylamine derivative at a rateAnd is formed by evaporation. The electron blocking layer is prepared by heating a spirofluorene derivative (e.g. type E081 from Argerya, Guangdong Co.) to 230 deg.C at a rateIndependently evaporating and plating;
3) a ternary evaporation method is adopted, a platinum compound (a luminous guest material) and DPQP (a hole type host material) are placed in the same rotary tray, and a derivative (an electronic type host material with a chemical structural formula of 2,4, 6-triphenyl-1, 3, 5-triazine) is put in the trayPlacing outside the rotary tray, sequentially heating 2,4, 6-triphenyl-1, 3, 5-triazine derivative at 220 deg.C and evaporation rate) And platinum compound (heating temperature 260 ℃ C., evaporation rate) After the platinum compound evaporation rate is stable, heating the DPQP to 220 ℃ until the platinum compound evaporation rate and the DPQP reach the sameWhen the vapor deposition device is used, the rotating tray is started, the rotating speed of the rotating tray is controlled to be 15r/min, then the baffle is opened, the vapor deposition is continuously carried out, and the light emitting effect is obtainedA layer;
4) sequentially laminating an electron transport layer, an electron injection layer and a cathode on the luminescent layer, wherein the electron transport layer is prepared by heating 8-hydroxyquinoline Lithium (LiQ) and anthracene derivative (such as 11518 product from Argerya, Guangdong) to 280 deg.C at a rateMixing and evaporating to obtain the final product. The electron injection layer is heated to 1100 ℃ by metal Yb at a rateAnd is formed by evaporation. The cathode is heated to 1100 ℃ by adopting metal Ag at a speedAnd (4) independently evaporating to obtain the finished product of the OLED device in the embodiment 2.
Example 3
An OLED device comprises an ITO anode, a hole injection layer, a hole transmission layer, an electron blocking layer, a light emitting layer, an electron transmission layer, an electron injection layer and an Ag cathode which are sequentially stacked from top to bottom, wherein the evaporation method of the OLED device comprises the following process steps of:
1) carrying out evaporation pretreatment on the ITO substrate: sequentially brushing cleaning liquid, ultrasonically cleaning the cleaning liquid and repeatedly carrying out pure water ultrasonic cleaning for three times on the ITO substrate, then baking the ITO substrate, placing the ITO substrate in a vacuum sample injection chamber, vacuumizing until the vacuum degree is 4.0E-0.4Pa and the rotating speed of a rotating tray is 12 r/min;
2) placing the pretreated ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 3.0E-5Pa, and sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate, wherein the hole injection layer is formed by heating a terphenylamine derivative (such as a product E051 which is purchased from Argentia-Jaegiella-Ci, Ltd.) to 230-240 ℃, and the speed rate is highSimultaneous miningHeating to 260 deg.C with tetrafluorobenzonitrile, and evaporating to obtain final product with 3% of doping concentration. The hole transport layer is heated to 240 deg.C with a terphenylamine derivative at a rateAnd is formed by evaporation. The electron blocking layer is prepared by heating a spirofluorene derivative (e.g. type E081 from Arleiya, Guangdong Co., Ltd.) to 220 deg.C at a rateIndependently evaporating and plating;
3) a ternary evaporation mode is adopted, a platinum compound (a luminescent object material) and DPQP (a cavity type host material) are placed in the same rotating tray, and a derivative (an electron type host material, the chemical structural formula of which is shown in the specification) of 2,4, 6-triphenyl-1, 3, 5-triazine is placed in the rotating tray) Placing outside the rotating tray, sequentially heating 2,4, 6-triphenyl-1, 3, 5-triazine derivative (heating temperature is 230 deg.C, evaporation rate is 230 deg.C)) And platinum compound (heating temperature 250 ℃ C., evaporation rate) After the platinum compound evaporation rate is stable, heating the DPQP to 230 ℃ until the platinum compound evaporation rate and the DPQP reach the sameWhen the luminescent layer is formed, starting the rotary tray, controlling the rotating speed of the rotary tray to be 12r/min, and opening the baffle plate to carry out evaporation continuously to obtain the luminescent layer;
4) sequentially laminating an electron transport layer, an electron injection layer and a cathode on the luminescent layer, wherein the electron transport layer is prepared from 8-hydroxyquinoline Lithium (LiQ), anthracene derivative (such as 11518 product from Argerya, Guangdong Co.) andheating to 290 deg.C and heating at a rate ofMixing and evaporating to obtain the final product. The electron injection layer is formed by heating metal Yb to 900 deg.C at a rateAnd is formed by evaporation. The cathode is heated to 1300 ℃ by adopting metal Ag at a rateAnd (4) independently evaporating to obtain the finished product of the OLED device in the embodiment 3.
Example 4
An OLED device comprises an ITO anode, a hole injection layer, a hole transmission layer, an electron blocking layer, a light emitting layer, an electron transmission layer, an electron injection layer and an Ag cathode which are sequentially stacked from top to bottom, wherein the evaporation method of the OLED device comprises the following process steps:
1) carrying out evaporation pretreatment on the ITO substrate: sequentially brushing cleaning liquid, ultrasonically cleaning the cleaning liquid and repeatedly ultrasonically cleaning pure water for three times on the ITO substrate, then baking the ITO substrate, and placing the ITO substrate in a vacuum sample injection chamber for vacuumizing until the vacuum degree is 5.0E-0.4Pa and the rotating speed of a rotating tray is 15 r/min;
2) placing the pretreated ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 3.5E-5Pa, sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate, wherein the hole injection layer is formed by heating terphenylamine derivative (such as E051 product from Arleiya Guangdong photoelectric materials Co., Ltd.) to 232 deg.C at a rateSimultaneously, the tetrafluorobenzonitrile is heated to 268 ℃, and the tetrafluorobenzonitrile are doped and evaporated according to 3 percent. The hole transport layer is heated to 232 deg.C with terphenylamine derivativeSteaming aloneAnd plating to obtain the final product. The electron blocking layer is prepared by heating a spirofluorene derivative (such as E081 available from Argentia photoelectric materials, Inc. of Guangdong) to 226 deg.C at a rateIndependently evaporating and plating;
3) a ternary evaporation method is adopted, a platinum compound (a luminous guest material) and DPQP (a hole type host material) are placed in the same rotary tray, and a derivative (an electronic type host material with a chemical structural formula of 2,4, 6-triphenyl-1, 3, 5-triazine) is put in the tray) Placing outside the rotating tray, sequentially heating 2,4, 6-triphenyl-1, 3, 5-triazine derivative (heating temperature is 230 deg.C, evaporation rate is 230 deg.C)) And platinum compound (heating temperature 250 ℃ C., evaporation rate) After the platinum compound evaporation rate is stable, heating the DPQP to 230 ℃ until the platinum compound evaporation rate and the DPQP reach the sameWhen the luminescent layer is formed, starting the rotary tray, controlling the rotating speed of the rotary tray to be 12r/min, and opening the baffle plate to carry out evaporation continuously to obtain the luminescent layer;
4) sequentially laminating an electron transport layer, an electron injection layer and a cathode on the light-emitting layer, wherein the electron transport layer is prepared by heating 8-hydroxyquinoline Lithium (LiQ) and anthracene derivative (such as 11518 product from Alegley photoelectric materials, Inc. in Guangdong) to 285 deg.CMixing and evaporating to obtain the final product. The electron injection layer is formed by heating metal Yb to 1000 deg.C at a rateAnd is formed by evaporation. The cathode is heated to 1200 ℃ by adopting metal Ag at a speed rateAnd (4) independently evaporating to obtain the finished product of the OLED device of the embodiment 4.
Example 5: performance testing
The finished products of the OLED devices of the embodiments 1 to 4 are respectively subjected to photoelectric property tests, and the test results are shown in the following table 1.
Table 1 test results of photoelectric properties of finished products in examples 1-4
@10mA/cm2,bottom
The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (4)
1. An evaporation method of an OLED device is characterized by comprising the following process steps:
1) carrying out evaporation pretreatment on the ITO substrate;
2) placing an ITO substrate in an evaporation chamber, controlling the vacuum degree in the evaporation chamber to be 2.0-4.0E-5 Pa, and sequentially laminating an evaporation hole injection layer, a hole transport layer and an electron blocking layer on the ITO substrate;
3) adopting a ternary evaporation mode, placing a light-emitting object material and a hole type host material in the same rotating tray, placing an electron type host material outside the rotating tray, heating the electron type host material and the light-emitting object material in sequence, heating the hole type host material after the evaporation rate of the light-emitting object material is stable, and when the evaporation rate of the light-emitting object material and the hole type host material reaches the evaporation rateWhen the luminescent layer is formed, starting the rotary tray, controlling the rotating speed of the rotary tray to be 10-15 r/min, and opening the baffle plate to continue evaporation to obtain the luminescent layer;
4) sequentially laminating an evaporation electron transmission layer, an electron injection layer and a cathode on the light-emitting layer to obtain an OLED device finished product;
the cavity type main body material in the step 3) is DPQP;
the luminescent guest material in the step 3) is a platinum compound;
the electronic type main body material in the step 3) is a derivative of 2,4, 6-triphenyl-1, 3, 5-triazine;
the heating temperature of the electronic type main body material in the step 3) is 220-230 ℃, and the evaporation rate is The heating temperature of the light-emitting object material is 250-260 ℃, and the evaporation rate isThe heating temperature of the cavity type main body material is 220-230 ℃.
2. An evaporation method of an OLED device according to claim 1, wherein: the pre-evaporation treatment in the step 1) comprises the steps of sequentially brushing an ITO substrate with a cleaning solution, ultrasonically cleaning the ITO substrate with the cleaning solution and repeatedly ultrasonically cleaning the ITO substrate with pure water for three times, then baking the ITO substrate, placing the ITO substrate in a vacuum sample injection chamber, vacuumizing to the vacuum degree of 3.0-5.0E-0.4 Pa, and rotating the rotary tray at the rotating speed of 10-15 r/min.
3. The evaporation method of the OLED device according to claim 1, wherein: the cathode in the step 4) is an Ag cathode.
4. An OLED device obtained by evaporation according to the evaporation method of any one of claims 1 to 3.
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