CN110845961A - Hardened layer material, preparation method of hardened layer material and display device - Google Patents

Hardened layer material, preparation method of hardened layer material and display device Download PDF

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CN110845961A
CN110845961A CN201911012829.2A CN201911012829A CN110845961A CN 110845961 A CN110845961 A CN 110845961A CN 201911012829 A CN201911012829 A CN 201911012829A CN 110845961 A CN110845961 A CN 110845961A
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hardened layer
layer material
reactant
mixture
structural formula
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赵远
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D187/00Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14Protective coatings, e.g. hard coatings
    • GPHYSICS
    • G09EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09FDISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements

Abstract

In the hardened layer material, the preparation method of the hardened layer material and the display device provided by the application, the structural formula of the hardened layer material is shown in the specification
Figure DDA0002244721090000011
Wherein, the structural formula of R is
Figure DDA0002244721090000012
And
Figure DDA0002244721090000013
wherein m and n are each between 30 and 70, and m and n are the same, the hardened layer material provided in the present application can be used to lift a machine by utilizing a synergistic effect between organic and inorganic componentsThe mechanical property, simultaneously, alkyl chains with different lengths are added into the side chain of the polymer, so that the molecular weight and the dispersity of the polymer are adjusted, the solubility of the polymer in a solvent is increased, the film forming property and the processability of the polymer are improved, and the technical problem that the mechanical property of a hardened layer is influenced by the existing hardened layer material due to low surface hardness and poor friction resistance is solved.

Description

Hardened layer material, preparation method of hardened layer material and display device
Technical Field
The application relates to the field of display, in particular to a hardened layer material, a preparation method of the hardened layer material and a display device.
Background
At present, because the ideal hardened layer has the characteristics of excellent mechanical properties, good optical transparency, easy processing and the like, the hardened layer is applied to the protective film of the display screen, and now the hardened layer material has become the main material of choice for the protective film of the display screen.
In recent years, some organic polymer materials such as polyacrylate, polyurethane and the like are mainly used as the hardening layer material for the hardening layer, but the surface hardness of the materials is low, the friction resistance is poor, the mechanical performance of the hardening layer is affected, and the application of the hardening layer in the field of the protective film of the display screen is not favorable.
Therefore, how to select a new hardened layer material to improve the mechanical properties of the hardened layer is a constant challenge for panel manufacturers all over the world.
Disclosure of Invention
The application provides a hardened layer material, a preparation method of the hardened layer material and a display device, which can solve the technical problem that the mechanical property of the hardened layer is influenced by the existing hardened layer material due to low surface hardness and poor friction resistance.
A hardened layer material, the structural formula of the hardened layer material isWherein, the structural formula of R isWherein m and n are each between 30 and 70, and wherein m and n are the same.
A method of making a hardened layer material, comprising:
providing a first reactant and a second reactant, wherein the first reactant and the second reactant react to generate the hardened layer material, and the structural formula of the first reactant is shown in the specificationThe structural formula of the second reactant is
Figure BDA0002244721070000023
The structural formula of the hardened layer material is shown in the specificationWherein, the structural formula of R is
Figure BDA0002244721070000025
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
In the method for preparing a hardened layer material provided by the present application, in the step of reacting the first reactant and the second reactant to form the hardened layer material, the molar amount of the first reactant and the molar amount of the second reactant correspond to each other in a relationship of 1 mole of the first reactant to 1 mole of the second reactant.
In the preparation method of the hardened layer material provided by the application, the first reactant and the second reactant react in a first solution to generate the hardened layer material, the first solution comprises tetrahydrofuran, water and a first additive, and the first additive comprises one or a combination of potassium carbonate, sodium carbonate and sodium bicarbonate.
In the preparation method of the hardened layer material provided by the application, the reaction temperature for reacting the first reactant and the second reactant to generate the hardened layer material is room temperature.
In the preparation method of the hardened layer material provided by the application, the reaction time of the first reactant and the second reactant for generating the hardened layer material is 44 hours to 50 hours.
In the method for preparing a hardened layer material provided by the present application, the step of providing a first reactant and a second reactant, which react to form the hardened layer material, includes:
providing a first reactant and a second reactant, the first reactant and the second reactant reacting to form a mixture comprising the hardened layer material;
and separating and purifying the mixture containing the hardened layer material to obtain the hardened layer material.
In the method for preparing a hardened layer material provided by the present application, the step of separating and purifying the mixture including the hardened layer material to obtain the hardened layer material includes:
removing the organic solvent from the mixture comprising the hardened layer material to obtain a first mixture;
dissolving the first mixture in an extraction solvent, and extracting with water to obtain a second mixture;
removing water from the second mixture to obtain a third mixture;
and removing the extraction solvent in the third mixture to obtain the hardened layer material.
In the preparation method of the hardened layer material provided by the application, the first mixture is dissolved in an extraction solvent, and the extraction solvent comprises one or more of dichloromethane, chloroform and tetrahydrofuran.
A display device, comprising:
the display panel is provided with a protective cover plate on the light emergent side;
a hardened layer disposed on the protective cover plate, the hardened layer having a structure of
Figure BDA0002244721070000041
Wherein, the structural formula of R is
Figure BDA0002244721070000042
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
In this applicationPlease provide a hardened layer material, a method for preparing the hardened layer material and a display device, wherein the hardened layer material has a structural formula of
Figure BDA0002244721070000044
Wherein, the structural formula of R is
Figure BDA0002244721070000045
The hardened layer material provided by the application can utilize the synergistic effect between organic and inorganic components to improve the mechanical property, and alkyl chains with different lengths are added into the side chains of the polymer, so that the molecular weight and the dispersity of the hardened layer material are adjusted, the solubility of the hardened layer material in a solvent is improved, the film forming property and the processability of the hardened layer material are improved, and the technical problem that the mechanical property of the hardened layer is influenced by the existing hardened layer material due to low surface hardness and poor friction resistance is solved.
Drawings
In order to more clearly illustrate the technical solutions in the present application, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a display device provided in the present application.
Detailed Description
The technical solution in the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. It should be apparent that the described embodiments are only some embodiments of the present application, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any inventive step based on the embodiments in the present application, are within the scope of protection of the present application.
The application provides a hardened layer material, hardened layerThe structural formula of the material is
Figure BDA0002244721070000051
Wherein, the structural formula of R is
Figure BDA0002244721070000052
Figure BDA0002244721070000053
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
As can be understood, the hardened layer material provided by the present application contains organic modified nanoparticles, wherein the organic modified nanoparticles can improve the dispersibility of the inorganic nanoparticles in the organic coating layer, so that the compatibility of the organic and inorganic parts in the hardened layer material can be increased, and the processability of the hardened layer material can be improved; in addition, in the hardened layer material that this application provided, the chemical bond that organic and inorganic part formed can guarantee to form lasting chemical connection between two incompatible looks to can overcome the shortcoming of ordinary organic material, effectively promote the surface hardness and the antifriction performance of hardened layer material, and then improve the mechanical properties of hardened layer, be of value to the application of hardened layer material in this field of the protection film of display screen.
The hardened layer material provided by the application is formed by polymerizing silicon oxide and germanium oxide monomers, and alkyl side chains with different lengths are added in the germanium oxide monomers, so that the molecular weight and the dispersity of the hardened layer material are adjusted, the solubility of the hardened layer material in a solvent is improved, and the film forming property and the processability of the hardened layer material are further improved.
The application also provides a preparation method of the hardened layer material. The preparation method of the hardened layer material comprises the following steps:
providing a first reactant and a second reactant, wherein the first reactant and the second reactant react to generate the hardened layer material, and the structural formula of the first reactant is shown in the specificationThe structural formula of the second reactant is
Figure BDA0002244721070000062
The structural formula of the hardened layer material is shown in the specification
Figure BDA0002244721070000063
Wherein, the structural formula of R is
Figure BDA0002244721070000064
Figure BDA0002244721070000065
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
The general reaction formula of the first reactant and the second reactant reacting to form the hardened layer material may be:
Figure BDA0002244721070000071
in the step of reacting the first reactant and the second reactant to form the hardened layer material, the molar amount of the first reactant and the molar amount of the second reactant are in a corresponding relationship of 1 mole of the first reactant to 1 mole of the second reactant.
The first reactant and the second reactant react in a first solution to form the hardened layer material. The first solution may include tetrahydrofuran, water, and a first additive. The first additive may include one or a combination of potassium carbonate, sodium carbonate and sodium bicarbonate, wherein the first additive may also be potassium bicarbonate, and the first additive mainly provides a weak alkalization environment for the reaction of the first reactant and the second reactant in the first solution to generate the hardened layer material, so as to provide a catalytic effect for the reaction.
In one embodiment, the first reactant may beThe second reactant may be
Figure BDA0002244721070000073
The first reactant
Figure BDA0002244721070000081
And a second reactant
Figure BDA0002244721070000082
The reaction equation for generating the hardened layer material by carrying out the reaction is as follows:
Figure BDA0002244721070000083
in practice, potassium carbonate, deionized water and tetrahydrofuran are added to a round bottom flask, and then the first reactant is added under nitrogen atmosphere
Figure BDA0002244721070000084
And a second reactant
Figure BDA0002244721070000085
The corresponding relationship between the molar amounts of the first reactant and the second reactant may be 3 mmol, the first reactant may correspond to 2 mmol of the second reactant, the mixture including the hardened layer material may be obtained by stirring and reacting at room temperature for 48 hours, and then the mixture may be separated and purified to obtain the hardened layer material
Figure BDA0002244721070000086
The hardening layer material is a colorless and transparent oily product.
In one embodiment, the first reactant may be
Figure BDA0002244721070000091
The second reactant may be
Figure BDA0002244721070000092
The first reactant
Figure BDA0002244721070000093
And a second reactant
Figure BDA0002244721070000094
The reaction equation for generating the hardened layer material by carrying out the reaction is as follows:
Figure BDA0002244721070000095
in practice, potassium carbonate, deionized water and tetrahydrofuran are added to a round bottom flask, and then the first reactant is added under nitrogen atmosphere
Figure BDA0002244721070000101
And a second reactant
Figure BDA0002244721070000102
The molar weight of the first reactant and the second reactant may correspond to 3 mmol of the first reactant and 2 mmol of the second reactant, the first reactant and the second reactant are stirred and reacted for two days at room temperature to obtain a mixture including the material of the hardened layer, and then the mixture is separated and purified to obtain the material of the hardened layerThe hardening layer material is a colorless and transparent oily product.
In one embodiment, the first reactant may be
Figure BDA0002244721070000104
The second reactant may be
Figure BDA0002244721070000105
The first reactant
Figure BDA0002244721070000111
And a second reactant
Figure BDA0002244721070000112
The reaction equation for generating the hardened layer material by carrying out the reaction is as follows:
Figure BDA0002244721070000113
in practice, potassium carbonate, deionized water and tetrahydrofuran are added to a round bottom flask, and then the first reactant is added under nitrogen atmosphere
Figure BDA0002244721070000114
And a second reactant
Figure BDA0002244721070000115
The corresponding relationship between the molar amounts of the first reactant and the second reactant may be 3 mmol, the first reactant may correspond to 2 mmol of the second reactant, the mixture including the hardened layer material may be obtained by stirring and reacting at room temperature for 48 hours, and then the mixture may be separated and purified to obtain the hardened layer material
Figure BDA0002244721070000116
The hardening layer material is a colorless and transparent oily product.
In one embodiment, the first reactant may beThe second reactant may be
Figure BDA0002244721070000122
The first reactant
Figure BDA0002244721070000123
And a second reactant
Figure BDA0002244721070000124
The reaction equation for generating the hardened layer material by carrying out the reaction is as follows:
Figure BDA0002244721070000125
in practice, potassium carbonate, deionized water and tetrahydrofuran are added to a round bottom flask, and then the first reactant is added under nitrogen atmosphere
Figure BDA0002244721070000131
And a second reactant
Figure BDA0002244721070000132
The corresponding relationship between the molar amounts of the first reactant and the second reactant may be 3 mmol, the first reactant may correspond to 2 mmol of the second reactant, the mixture including the hardened layer material may be obtained by stirring and reacting at room temperature for 48 hours, and then the mixture may be separated and purified to obtain the hardened layer material
Figure BDA0002244721070000133
The hardening layer material is a colorless and transparent oily product.
In the separation and purification, the tetrahydrofuran, which is an organic solvent, in the mixture including the hardened layer material may be removed by using a rotary evaporator to obtain a first mixture, the first mixture is dissolved in an extraction solvent, the mixture is extracted with water for 2 to 5 times to obtain a second mixture, then anhydrous magnesium sulfate is added to the second mixture, the mixture is stirred for 16 hours to remove water in the second mixture to obtain a third mixture, and finally the extraction solvent in the third mixture is removed by filtration to obtain a colorless and transparent oily product, that is, the hardened layer material.
Among them, it can be understood that since the boiling point of the organic solvent is very low at high temperature and high vacuum, it is easily volatilized; and the first mixture does not volatilize into gas under the same condition due to the high boiling point of the first mixture, so that the organic solvent and the first mixture can be effectively separated by a rotary evaporator.
Wherein, the extraction solvent comprises one or a combination of several of dichloromethane, trichloromethane and tetrahydrofuran. The extraction solvent is an organic solvent as the material of the cured layer, and therefore, it is sufficient that the material of the cured layer is dissolved therein.
Among them, it is understood that the first mixture containing the hardened layer material is dissolved in the extraction solvent in order to sufficiently remove impurities generated in the previous reaction process.
The hardened layer material prepared by the preparation method of the hardened layer material provided by the application comprises the organic modified nanoparticles, wherein the organic modified nanoparticles can improve the dispersibility of the inorganic nanoparticles in the organic coating, so that the compatibility of organic and inorganic parts in the hardened layer material can be improved, and the processability of the hardened layer material can be improved; in addition, in the hardened layer material that this application provided, the chemical bond that organic and inorganic part formed can guarantee to form lasting chemical connection between two incompatible looks to can overcome the shortcoming of ordinary organic material, effectively promote the surface hardness and the antifriction performance of hardened layer material, and then improve the mechanical properties of hardened layer, be of value to the application of hardened layer material in this field of the protection film of display screen.
Fig. 1 is a schematic structural diagram of a display device provided in the present application, which includes a display panel 10, a protective cover 11, and a hardened layer 12.
The light-emitting side of the display panel 10 is provided with a protective cover plate 11, and the hardening layer 12 is arranged on the protective cover plate 11. The hardened layer 12 comprises a hardened layer material with the structural formula
Figure BDA0002244721070000141
Wherein, the structural formula of R is
Figure BDA0002244721070000143
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
In some embodiments, the hardened layer 12 includes at least one of the hardened layer materials. Specifically, the hardened layer 12 includes one or more hardened layer materials.
The application also provides a preparation method of the hardened layer film, which comprises the following steps: dissolving a hardening layer material in an organic solvent containing a photoinitiator, stirring for 1 hour at room temperature to obtain a colorless transparent solution containing the hardening layer material, uniformly coating the colorless transparent solution on a clean glass surface, drying for 16 hours at room temperature, and then drying for 2 hours at 70 ℃ in vacuum to obtain the hardening layer material film.
Wherein, it can be understood that, in the preparation method of the hardened layer film provided by the application, the hardened layer material is a hardened layer material with the structural formula as
Figure BDA0002244721070000151
Wherein, the structural formula of R isWherein m and n are each between 30 and 70, and wherein m and n are the same. Therefore, four different hardened layer material films can be obtained by using the hardened layer material, namely P1, P2, P3 and P4.
Referring to table 1, table 1 is a table of performance data of the hardened layer material film provided in the present application.
Sample (I) Weight average molecular weight (kg. mol)-1) Degree of dispersion Hardness of pencil Number of times of rub resistance
P1 19 3.3 3H 4000
P2 12 2.4 5H 3000
P3 8 1.8 3H 1000
P4 6 1.6 2H 1000
TABLE 1
The hardened layer film prepared from the hardened layer material provided by the application has excellent dispersity, hardness and friction resistance, is applied to the field of protective films of display screens, and can be beneficial to development of the field of protective films of display screens.
The foregoing provides a detailed description of embodiments of the present application, and the principles and embodiments of the present application have been described herein using specific examples, which are presented solely to aid in the understanding of the present application. Meanwhile, for those skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (10)

1. The hardened layer material is characterized in that the hardened layer material has a structural formulaWherein, the structural formula of R is
Figure FDA0002244721060000013
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
2. A method of preparing a hardened layer material, comprising:
providing a first reactant and a second reactant, wherein the first reactant and the second reactant react to generate the hardened layer material, and the structural formula of the first reactant is shown in the specification
Figure FDA0002244721060000014
The structural formula of the second reactant is
Figure FDA0002244721060000015
The structural formula of the hardened layer material is shown in the specification
Figure FDA0002244721060000021
Wherein, the structural formula of R is
Figure FDA0002244721060000023
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
3. The method for producing a hardened layer material according to claim 2, wherein in the reaction of the first reactant and the second reactant to produce the hardened layer material, the correspondence between the molar amount of the first reactant and the molar amount of the second reactant is 1 mole of the first reactant to 1 mole of the second reactant.
4. The method of claim 2, wherein the first reactant and the second reactant react in a first solution to form the hardened layer material, the first solution comprises tetrahydrofuran, water and a first additive, and the first additive comprises one or more of potassium carbonate, sodium carbonate and sodium bicarbonate.
5. The method for producing a hardened layer material according to claim 2, wherein the reaction temperature at which the first reactant and the second reactant react to form the hardened layer material is room temperature.
6. The method for producing a hardened layer material according to claim 2, wherein the reaction time for reacting the first reactant and the second reactant to form the hardened layer material is 44 hours to 50 hours.
7. The method of producing a hardened layer material according to claim 2, wherein said step of providing a first reactant and a second reactant, said first reactant and said second reactant reacting to form said hardened layer material comprises:
providing a first reactant and a second reactant, the first reactant and the second reactant reacting to form a mixture comprising the hardened layer material;
and separating and purifying the mixture containing the hardened layer material to obtain the hardened layer material.
8. The method for producing a hardened layer material according to claim 7, wherein said step of separating and purifying a mixture containing said hardened layer material to obtain said hardened layer material comprises:
removing the organic solvent from the mixture comprising the hardened layer material to obtain a first mixture;
dissolving the first mixture in an extraction solvent, and extracting with water to obtain a second mixture;
removing water from the second mixture to obtain a third mixture;
and removing the extraction solvent in the third mixture to obtain the hardened layer material.
9. The method for preparing a hardened layer material of claim 8, wherein said first mixture is dissolved in an extraction solvent comprising one or a combination of dichloromethane, chloroform and tetrahydrofuran.
10. A display device, comprising:
the display panel is provided with a protective cover plate on the light emergent side;
a hardening layer, the hardening layer is arranged on the protective cover plate, the structural formula of the material of the hardening layer is
Figure FDA0002244721060000031
Wherein, the structural formula of R is
Figure FDA0002244721060000032
Figure FDA0002244721060000033
Wherein m and n are each between 30 and 70, and wherein m and n are the same.
CN201911012829.2A 2019-10-23 2019-10-23 Hardened layer material, preparation method of hardened layer material and display device Pending CN110845961A (en)

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Application publication date: 20200228