CN112820844A - Thin film packaging structure and preparation method thereof - Google Patents
Thin film packaging structure and preparation method thereof Download PDFInfo
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- CN112820844A CN112820844A CN202110106846.3A CN202110106846A CN112820844A CN 112820844 A CN112820844 A CN 112820844A CN 202110106846 A CN202110106846 A CN 202110106846A CN 112820844 A CN112820844 A CN 112820844A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
Abstract
The invention relates to a film packaging structure and a preparation method thereof, wherein the film packaging structure comprises an organic polymer substrate, a flexible organic photoelectric device and an inorganic and organic overlapped film packaging layer with a periodic fluctuation nano structure, which are sequentially arranged from bottom to top, the film packaging layer is formed by alternately laminating an inorganic blocking layer and an organic blocking layer, the organic blocking layer is stamped by a template with the periodic fluctuation nano structure to form the periodic fluctuation nano structure, then the inorganic blocking layer is prepared on the periodic fluctuation nano structure, and the film packaging layer is formed by overlapping. The thin film encapsulation structure has high water oxygen barrier performance and bending performance.
Description
Technical Field
The invention belongs to the technical field of flexible display, and particularly relates to a thin film packaging structure and a preparation method thereof.
Background
The Organic Light Emitting Diode (Organic Light Emitting Diode) display technology has attracted great attention due to its own series of advantages, and is considered to be the next generation mainstream display technology most likely to replace the LCD. However, organic materials and cathode materials in the OLED device are prone to fail after reaction with water and oxygen, and therefore, encapsulation of the OLED device is very important.
The packaging techniques mainly include rigid cover packaging and flexible film packaging. The cover plate package is difficult to make the device flexible, and the requirement of future display cannot be met. Among the thin film encapsulation technologies, the inorganic/organic overlapping thin film encapsulation structure is the most commonly used, and is the only encapsulation technology that is currently possible to realize flexible devices. However, on the one hand, the water and oxygen barrier properties of organic materials with porous structures are not very good; on the other hand, the inorganic layer has a large young's modulus, and has a large internal stress when bent, which easily deforms the device, and the organic layer and the inorganic layer have a large stress mismatch, which easily causes cracks and falls off during the bending process. For flexible displays and wearable devices, achieving bending is the most fundamental requirement.
Disclosure of Invention
The invention aims to provide a thin film packaging structure and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the film packaging structure comprises an organic polymer substrate, a flexible organic photoelectric device and an inorganic and organic overlapped film packaging layer with a periodic fluctuation nano structure, wherein the organic polymer substrate, the flexible organic photoelectric device and the inorganic and organic overlapped film packaging layer are sequentially arranged from bottom to top, the film packaging layer is formed by alternately laminating an inorganic blocking layer and an organic blocking layer, the organic blocking layer is stamped through a template with the periodic fluctuation nano structure to form the periodic fluctuation nano structure, then the inorganic blocking layer is prepared on the organic blocking layer, and the film packaging layer is formed by overlapping.
Furthermore, the periodically fluctuating micro-nano structure comprises a one-dimensional and two-dimensional micro-nano structure, the period is 10 nanometers-1000 micrometers, and the depth is 20 nanometers-500 micrometers.
Further, the form of the periodic undulations includes sine wave, triangular wave, and trapezoidal wave shapes.
The invention also provides a preparation method of the film packaging structure, which comprises the following steps:
s1, preparing a PDMS thin layer, stretching the PDMS thin layer in a single direction or multiple directions simultaneously, and performing plasma treatment to obtain a PDMS template with a periodic fluctuation nano structure;
s2, preparing a flexible organic photoelectric device on the surface of a prepared organic polymer substrate, and preparing an inorganic nano stacked film, namely an inorganic barrier layer, by adopting atomic layer deposition;
s3, preparing an organic barrier layer on the surface of the inorganic barrier layer obtained in the step S2, vacuumizing the PDMS template prepared in the step S1 to form negative pressure, placing the surface with the periodic undulating nano-structure on the surface of the organic barrier layer in a downward mode, applying set pressure, curing the organic barrier layer, and forming the periodic undulating nano-structure on the surface of the organic barrier layer;
s4, carrying out surface modification treatment on the surface of the organic barrier layer obtained in the step S3 by adopting plasma;
s5, preparing an inorganic nano stacked film on the surface of the organic barrier layer with the periodic fluctuating nano structure obtained in the step S4 by adopting atomic layer deposition;
s6, repeating the steps S3-S5 to form n inorganic/organic overlapped thin film encapsulation layers.
Further, in the step S1, stirring and mixing PDMS and a curing agent in a set ratio, standing, removing bubbles, and performing thermal curing to obtain a PDMS thin layer, wherein the ratio of the PDMS to the curing agent is 100: 1-1: 1, and the thermal curing time is 15 min-160 min.
Further, in the step S1, the plasma processing gas is one or more of argon, oxygen, SF6 and CHF3, the gas flow rate is 10-60 sccm, the gas pressure is 1-10 pa, the plasma power is 20W-200W, and the processing time is 40-240S.
In step S2, the inorganic barrier layer is one of aluminum oxide, titanium oxide, organic aluminum, zinc oxide, hafnium oxide, and zirconium oxide, and has a thickness of 20nm to 100 nm.
Further, in the step S3, the organic barrier layer is one or more of organic resins with high visible light transmittance and good transparency, including polyurethane, silicone resin, acrylic resin, and epoxy resin, and has a thickness of 2 μm to 20 μm.
Further, in the step S4, the plasma processing gas is one or more of argon, nitrogen, SF6, CF4, CHF3, and CCl4, the gas flow rate is 5sccm to 20sccm, the gas pressure is 1Pa to 30Pa, the plasma power is 1W to 1000W, and the processing time is 5S to 60 min.
Further, in step S5, the inorganic nano-stacked film forms a periodic undulating nano-structure identical to that of the organic barrier layer, and the inorganic/organic film interface is a periodic undulating micro-nano structure.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, the organic barrier layer is subjected to patterning treatment through the PDMS with the periodic fluctuation nano structure treated by the plasma, and then the organic layer is subjected to surface modification by the plasma, so that the water oxygen barrier property of the organic layer is improved, the internal stress of the packaging film under bending is reduced, and the bending property of the packaging film is improved. The periodic nanostructure is controlled by regulating and controlling the time and power of plasma treatment, so that packaging films with different mechanical properties can be obtained. In addition, the invention has the advantages of easily obtained required materials, simple operation, high manufacturing efficiency and good packaging effect.
Drawings
FIG. 1 is a schematic representation of a first intermediate product obtained during the preparation of an example of the present invention.
FIG. 2 is a schematic representation of a second intermediate product obtained during the preparation of an example of the present invention.
FIG. 3 is a schematic representation of a third intermediate product obtained during the preparation of an example of the present invention.
FIG. 4 is a schematic representation of a fourth intermediate product obtained during the preparation of an example of the present invention.
FIG. 5 is a schematic representation of a fifth intermediate product obtained during the preparation of an example of the present invention.
FIG. 6 is a schematic representation of a sixth intermediate product obtained during the preparation of an example of the present invention.
Fig. 7 is a schematic view of a film package structure finally obtained in the embodiment of the present invention.
In the figure: 10 is PDMS; 20 is an organic polymer substrate; 30 is a flexible organic optoelectronic device; 40. 41 and 42 are both inorganic barrier layers; 50. 51, 52 are both organic barrier layers; and 60 is plasma.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail with reference to the following embodiments and the accompanying drawings. The drawings are only for reference and illustration purposes and are not intended to limit the invention.
The embodiment provides a film packaging structure with high water oxygen barrier performance and bending performance, and the film packaging structure comprises an organic polymer substrate, a flexible organic photoelectric device and an inorganic and organic overlapped film packaging layer with a periodic fluctuating nano structure, wherein the organic polymer substrate, the flexible organic photoelectric device and the inorganic and organic overlapped film packaging layer with the periodic fluctuating nano structure are sequentially arranged from bottom to top, the film packaging layer is formed by alternately laminating an inorganic blocking layer and an organic blocking layer, the organic blocking layer is stamped through a template with the periodic fluctuating nano structure to form the periodic fluctuating nano structure, then the inorganic blocking layer is prepared on the periodic fluctuating nano structure, and the film packaging layer is formed by overlapping.
In this embodiment, the periodically fluctuating micro-nano structure includes a one-dimensional and a two-dimensional micro-nano structure, the period is 10 nanometers to 1000 micrometers, and the depth is 20 nanometers to 500 micrometers. The form of the periodic undulations includes sine wave, triangular wave, and trapezoidal wave shapes.
The preparation method of the film packaging structure comprises the following steps:
s1, as shown in fig. 1, a PDMS template 10 having a periodic relief nanostructure was prepared using plasma treatment. The method specifically comprises the following steps:
s11, as shown in fig. 1 (a), mixing a certain proportion of PDMS with a curing agent, standing for a while to remove air bubbles, and thermally curing to obtain a thin PDMS layer 10.
S12, as shown in fig. 1 (b), the PDMS thin layer 10 obtained in step S11 is stretched in one direction or in multiple directions simultaneously.
S13, as shown in fig. 1 (c), the surface of the PDMS thin layer 10 stretched in the step S12 is processed by plasma 60, so as to obtain the PDMS template 10 with the periodic relief nano-structure.
S2, as shown in fig. 2, preparing a flexible organic photoelectric device 30 on the surface of the organic polymer substrate 20 with high water oxygen barrier property, and preparing an inorganic nano-stack film, i.e. an inorganic barrier layer 40, by atomic layer deposition.
S3, as shown in fig. 3, an organic barrier layer 50 is prepared on the surface of the inorganic barrier layer 40 of step S2. As shown in fig. 4, the PDMS template 10 obtained in step S1 is vacuumized to form a negative pressure, one side of the PDMS template having the periodic relief nanostructure is placed on the surface of the organic barrier layer 50, a certain pressure is applied, the organic barrier layer is cured by photo-curing or thermal-curing, and then the periodic relief nanostructure is formed on the surface of the organic barrier layer 50.
S4, as shown in fig. 5, the PDMS film layer 10 is uncovered, and the surface of the organic barrier layer 50 obtained in step S3 is subjected to surface modification treatment using the plasma 60.
S5, as shown in fig. 6, the inorganic nano-stack film 41 is prepared on the surface of the organic barrier layer 50 containing the periodic relief nano-structure obtained in step S4 by atomic layer deposition.
S6, repeating the steps S3-S5 to form n inorganic/organic overlapped thin film encapsulation layers. As shown in fig. 7, in the present embodiment, steps S3 to S51 are repeated, and then the organic barrier layer 51 is prepared to form a thin film encapsulation layer having 3 inorganic/organic overlapping periods.
In the step S1, stirring and mixing PDMS and a curing agent in a set proportion, standing for a period of time, removing bubbles, and performing thermal curing to obtain a PDMS thin layer, wherein the proportion of PDMS to the curing agent is 100: 1-1: 1, and the thermal curing time is 15 min-160 min; the stretching degree is 0% -500%. The plasma processing gas is one or more of argon, oxygen, SF6 and CHF3, the gas flow is 10-60 sccm, the gas pressure is 1-10 pa, the plasma power is 20-200W, and the processing time is 40-240 s.
In this embodiment, the ratio of the PDMS to the curing agent in step S11 is 10: 1, standing for 30min and thermosetting for 20 min. The degree of stretching of the PDMS thin layer 10 in step S12 was 30%. The processing gas of the plasma 60 in step S13 includes, but is not limited to, argon, oxygen and a mixture of argon and oxygen, the gas flow is 40sccm, the gas pressure is 10pa, the plasma power is 200W, and the processing time is 50S.
In the step S2, the inorganic barrier layer is one of aluminum oxide, titanium oxide, organic aluminum, zinc oxide, hafnium oxide, and zirconium oxide, and has a thickness of 20nm to 100 nm.
In this embodiment, the material of the inorganic barrier layers 40, 41, and 42 is alumina, and the thickness of the inorganic barrier layers 40, 41, and 42 is 50 nm.
In the step S3, the organic barrier layer is one or more of organic resins with high visible light transmittance and good transparency, including polyurethane, silicone resin, acrylic resin, and epoxy resin, and has a thickness of 2 μm to 20 μm.
In the present embodiment, the material of the organic barrier layers 50, 51, and 52 is an organic resin, the organic resin is an acrylic resin, and the thicknesses of the organic barrier layers 50, 51, and 52 are all 8 μm. The organic barrier layer is prepared by a spin coating method. The spin coating process conditions are as follows: rotating at low speed of 300 turns for 1 minute; the high speed is 1000r, and the high speed time is 15 seconds. The curing mode is ultraviolet curing, and the curing time is 3 min;
in the step S4, the plasma processing gas is one or more of argon, nitrogen, SF6, CF4, CHF3 and CCl4, the gas flow is 5sccm to 20sccm, the gas pressure is 1Pa to 30Pa, the plasma power is 1W to 1000W, and the processing time is 5S to 60 min.
In the present embodiment, the plasma processing gas is a mixed gas of argon, nitrogen, SF, and CF 4; the gas flow rate is 30sccm, the gas pressure is 10Pa, the plasma power is 300W, and the treatment time is 20 minutes.
Three effects occur when the plasma modifies the surface of the organic layer: (1) the plasma can modify the surface of the organic barrier layer and enhance the hydrophobicity of the surface of the organic barrier layer; (2) after the plasma contacts the surface of the organic barrier layer, the local surface of the organic barrier layer is heated to melt the surface of the organic layer, and the surface defects and pinholes on the organic layer are filled; (3) injecting plasma into the surface of the organic layer to make the surface of the organic barrier layer more compact; the three modification modes can improve the water and oxygen barrier property of the organic barrier layer, increase the contact area of the organic layer and the inorganic layer and reduce the stress mismatch of the organic layer and the inorganic layer.
In the step S5, the inorganic nano-stack film forms a periodic fluctuating nano-structure identical to that of the organic barrier layer, and the inorganic/organic film interface is a periodic fluctuating micro-nano-structure similar to a spring.
In this embodiment, the inorganic nano-stacked films 41 and 42 form a periodic fluctuating nano-structure identical to the surface of the organic barrier layer, and the inorganic/organic film interface is a periodic fluctuating micro-nano structure similar to a spring, which increases the contact area between the organic barrier layer and the inorganic layer, improves the binding force between the organic layer and the inorganic layer, and reduces the stress inside the encapsulation film layer under the same bending degree; on the other hand, the periodically fluctuating micro-nano structure similar to a spring increases the toughness of the packaging film layer and improves the mechanical property of the packaging film layer.
The schematic provided by the present invention has the thicknesses of layers and regions exaggerated for clarity, but should not be considered as strictly reflecting the geometric scaling as a schematic.
The above preferred embodiments are provided to further illustrate the objects, technical solutions and advantages of the present invention, and the present invention is not limited to the above preferred embodiments, and other forms of packaging methods for flexible OLED devices can be found by anyone in the light of the present invention. All equivalent changes, modifications and improvements which come within the spirit and scope of the invention are desired to be protected by the following claims.
Claims (10)
1. The thin film packaging structure is characterized by comprising an organic polymer substrate, a flexible organic photoelectric device and an inorganic and organic overlapped thin film packaging layer with a periodic fluctuation nano structure, wherein the organic polymer substrate, the flexible organic photoelectric device and the inorganic and organic overlapped thin film packaging layer with the periodic fluctuation nano structure are sequentially arranged from bottom to top, the thin film packaging layer is formed by alternately laminating an inorganic blocking layer and an organic blocking layer, the organic blocking layer is stamped through a template with the periodic fluctuation nano structure to form the periodic fluctuation nano structure, then the inorganic blocking layer is prepared on the periodic fluctuation nano structure, and the inorganic blocking layer is overlapped to form the thin film packaging.
2. The film package structure of claim 1, wherein the periodic undulating micro-nano structure comprises one-dimensional and two-dimensional micro-nano structures, the period is 10 nm to 1000 μm, and the depth is 20nm to 500 μm.
3. The film encapsulation structure according to claim 1, wherein the periodic undulation forms include sine wave, triangular wave and trapezoidal wave shapes.
4. The method for preparing a thin film encapsulation structure according to any one of claims 1 to 3, comprising the steps of:
s1, preparing a PDMS thin layer, stretching the PDMS thin layer in a single direction or multiple directions simultaneously, and performing plasma treatment to obtain a PDMS template with a periodic fluctuation nano structure;
s2, preparing a flexible organic photoelectric device on the surface of a prepared organic polymer substrate, and preparing an inorganic nano stacked film, namely an inorganic barrier layer, by adopting atomic layer deposition;
s3, preparing an organic barrier layer on the surface of the inorganic barrier layer obtained in the step S2, vacuumizing the PDMS template prepared in the step S1 to form negative pressure, placing the surface with the periodic undulating nano-structure on the surface of the organic barrier layer in a downward mode, applying set pressure, curing the organic barrier layer, and forming the periodic undulating nano-structure on the surface of the organic barrier layer;
s4, carrying out surface modification treatment on the surface of the organic barrier layer obtained in the step S3 by adopting plasma;
s5, preparing an inorganic nano stacked film on the surface of the organic barrier layer with the periodic fluctuating nano structure obtained in the step S4 by adopting atomic layer deposition;
s6, repeating the steps S3-S5 to form n inorganic/organic overlapped thin film encapsulation layers.
5. The method of claim 4, wherein in the step S1, PDMS and a curing agent are mixed at a predetermined ratio, and the mixture is left to stand to remove air bubbles, and then thermally cured to obtain a PDMS thin layer, wherein the ratio of PDMS to the curing agent is 100: 1-1: 1, and the thermal curing time is 15 min-160 min.
6. The method as claimed in claim 4, wherein in step S1, the plasma processing gas is one or more of argon, oxygen, SF6 and CHF3, the gas flow rate is 10-60 sccm, the gas pressure is 1-10 pa, the plasma power is 20W-200W, and the processing time is 40-240S.
7. The method as claimed in claim 4, wherein in step S2, the inorganic barrier layer is one of alumina, titania, organic aluminum, zinc oxide, hafnium oxide, and zirconium oxide, and has a thickness of 20nm to 100 nm.
8. The method as claimed in claim 4, wherein in step S3, the organic barrier layer is one or more of organic resins with high visible light transmittance and good transparency, including polyurethane, silicone resin, acrylic resin, and epoxy resin, and has a thickness of 2 μm to 20 μm.
9. The method as claimed in claim 4, wherein in step S4, the plasma processing gas is one or more of argon, nitrogen, SF6, CF4, CHF3, and CCl4, the gas flow rate is 5sccm to 20sccm, the gas pressure is 1Pa to 30Pa, the plasma power is 1W to 1000W, and the processing time is 5S to 60 min.
10. The method of claim 4, wherein in step S5, the inorganic nano-stacked film forms a periodic undulating nano-structure identical to that of the organic barrier layer, and the inorganic/organic film interface is a periodic undulating micro-nano structure.
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| CN103996629A (en) * | 2014-06-12 | 2014-08-20 | 广州新视界光电科技有限公司 | Packaging process of flexible semiconductor film electronic device |
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| CN109427989A (en) * | 2017-08-22 | 2019-03-05 | 中华映管股份有限公司 | Encapsulation layer structure |
| CN110187417A (en) * | 2019-06-27 | 2019-08-30 | 电子科技大学 | The production method of PDMS film microlens array |
| CN111071983A (en) * | 2019-12-23 | 2020-04-28 | 大连海洋大学 | Rapid preparation method of elastomer PDMS (polydimethylsiloxane) multistage wrinkled surface |
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2021
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Patent Citations (8)
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| CN103996629A (en) * | 2014-06-12 | 2014-08-20 | 广州新视界光电科技有限公司 | Packaging process of flexible semiconductor film electronic device |
| CN104401144A (en) * | 2014-11-12 | 2015-03-11 | 天津大学 | Channeled template-based transfer method |
| CN104690991A (en) * | 2014-11-12 | 2015-06-10 | 天津大学 | Method for manufacturing wrinkled template with large shaft diameter ratio |
| CN105810845A (en) * | 2016-05-17 | 2016-07-27 | 武汉华星光电技术有限公司 | OLED device encapsulation structure, OLED device and display screen |
| CN106684256A (en) * | 2016-12-23 | 2017-05-17 | 上海天马有机发光显示技术有限公司 | Display panel and fabrication method thereof |
| CN109427989A (en) * | 2017-08-22 | 2019-03-05 | 中华映管股份有限公司 | Encapsulation layer structure |
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Application publication date: 20210518 |