Thin film and preparation method thereof, light-emitting device and preparation method thereof, and display device

By gradually increasing the vacuum degree during the vacuum drying process and drying the liquid film, the problems of high surface roughness and poor density of the film are solved, and high-quality film film formation is achieved.

CN120035358APending Publication Date: 2025-05-23TCL TECHNOLOGY GROUP CORPORATION
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Patent Information

Application Number
CN202311581639.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-11-23
Publication Date
2025-05-23

AI Technical Summary

Technical Problem

Due to process reasons, existing films have problems with high surface roughness and poor density.

Method used

The liquid film is dried by gradually increasing the vacuum degree, and a tightly arranged single-molecular layer is formed by self-assembly, and the single-molecular layer continues to grow until it is completely precipitated, and the residual solvent is removed to form a high-density film.

Benefits of technology

The film formation quality of the film is improved, the surface roughness is reduced, and the density and conductive properties of the film are improved.

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Abstract

The embodiment of the invention provides a thin film and a preparation method thereof, a light-emitting device and a preparation method thereof, and a display device. The preparation method of the thin film comprises the following steps: providing a film forming solution, wherein the film forming solution comprises a film forming material and a solvent; depositing a film forming solution to form a liquid film; and drying the liquid film in an environment with gradually increased vacuum degree to obtain the thin film. The thin film prepared by the preparation method is relatively high in density, good in film forming quality and relatively low in surface roughness.
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Description

Technical Field

[0001] The present application relates to the field of light-emitting devices, and in particular to a thin film and a method for preparing the same, a light-emitting device and a method for preparing the same, and a display device. Background Art

[0002] Thin film refers to a two-dimensional material formed by at least one of atoms, molecules or ions deposited on the surface of a substrate. The material of the thin film can be at least one of an organic compound and an inorganic compound. The types of thin films include but are not limited to optical thin films and semiconductor thin films. Thin films are widely used in electronics, machinery, printing and other fields. Due to process reasons, thin films have problems such as high surface roughness and poor density of the film. Summary of the invention

[0003] Based on this, the embodiments of the present application provide a thin film and a method for preparing the same, a light-emitting device and a method for preparing the same, and a display device.

[0004] In a first aspect, an embodiment of the present application provides a method for preparing a thin film, comprising:

[0005] Providing a film-forming solution, wherein the film-forming solution comprises a film-forming material and a solvent;

[0006] Depositing the film-forming solution to form a liquid film;

[0007] The liquid film is dried in an environment with gradually increasing vacuum degree to obtain a thin film.

[0008] In some embodiments, when the liquid film is dried in an environment with gradually increasing vacuum degree, a first time period, a second time period and a third time period are sequentially experienced in chronological order, and the average pressure of the environment in which the liquid film is located during the first time period is defined as a first pressure, the average pressure of the environment in which the liquid film is located during the second time period is defined as a second pressure, and the average pressure of the environment in which the liquid film is located during the third time period is defined as a third pressure;

[0009] Among them, the first pressure, the second pressure and the third pressure decrease in sequence.

[0010] In some embodiments, the pressure of the environment in which the liquid film is located remains constant during the first time period, or the pressure of the environment in which the liquid film is located continues to decrease during the first time period; and / or

[0011] The pressure of the environment in which the liquid film is located remains constant during the second time period, or the pressure of the environment in which the liquid film is located continues to decrease during the second time period; and / or

[0012] The pressure of the environment in which the liquid membrane is located remains constant during the third time period, or the pressure of the environment in which the liquid membrane is located continues to decrease during the third time period.

[0013] In some embodiments, the pressure of the environment in which the liquid film is located in the first time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located in the first time period and the time present a curvilinear relationship; and / or

[0014] The pressure of the environment in which the liquid film is located during the second time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located during the second time period and the time present a curvilinear relationship; and / or

[0015] The pressure of the environment in which the liquid film is located in the third time period and time present a linear relationship, or the pressure of the environment in which the liquid film is located in the third time period and time present a curvilinear relationship.

[0016] In some embodiments, the first pressure is 10 -1 Pa~10 -2 Pa, the first time period is 10 minutes to 90 minutes; and / or

[0017] The second pressure is 10 -3 Pa~10 -5 Pa, the second time period is 10 minutes to 90 minutes; and / or

[0018] The third pressure is 10 -5 Pa~10 -7 Pa, the third time period is 10 minutes to 90 minutes.

[0019] In some embodiments, drying the liquid film in an environment with gradually increasing vacuum degree comprises:

[0020] The liquid film is subjected to a vacuum drying process, during which the pressure of the environment in which the liquid film is located gradually decreases with time, and the pressure of the environment in which the liquid film is located and time present a linear relationship or a curvilinear relationship.

[0021] In some embodiments, the film-forming material includes at least one of a P-type semiconductor material, a light-emitting material, and an N-type semiconductor material; and / or

[0022] The concentration of the film-forming solution is 5 mg / ml to 100 mg / ml; and / or

[0023] The film-forming solution is deposited by inkjet printing.

[0024] In some embodiments, the luminescent material includes at least one of an organic luminescent material and a quantum dot luminescent material, and the organic luminescent material includes one or more of 4,4'-bis(N-carbazole)-1,1'-biphenyl:tri[2-(p-tolyl)pyridine iridium(III), 4,4',4"-tri(carbazole-9-yl)triphenylamine:tri[2-(p-tolyl)pyridine iridium, diarylanthracene derivatives, distilbene aromatic derivatives, pyrene derivatives, fluorene derivatives, 1,4,7,10-tetra-tert-butylperylene, rubrene derivatives, thermally activated delayed fluorescence materials, exciplex luminescent materials, polyacetylene and its derivatives, polyparaphenylene and its derivatives, polythiophene and its derivatives, polyfluorene and its derivatives;The quantum dot luminescent material comprises at least one of a single structure quantum dot and a core-shell structure quantum dot, the material of the single structure quantum dot, the core material of the core-shell structure quantum dot and the shell material of the core-shell structure quantum dot each comprise at least one of a II-VI group compound, a IV-VI group compound, a III-V group compound and a I-III-VI group compound, the shell layer of the core-shell quantum dot comprises one or more layers, wherein the II-VI group compound is selected from CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, HgS, HgSe, HgTe, At least one of CdSeS, CdSeTe, CdSTe, ZnSeS, ZnSeTe, ZnSTe, HgSeS, HgSeTe, HgSTe, CdZnS, CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, HgZnSe, HgZnTe, CdZnSeS, CdZnSeTe, CdZnSTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe and HgZnSTe, the IV-VI group compound At least one selected from SnS, SnSe, SnTe, PbS, PbSe, PbTe, SnSeS, SnSeTe, SnSTe, PbSeS, PbSeTe, PbSTe, SnPbS, SnPbSe, SnPbTe, SnPbSSe, SnPbSeTe, SnPbSTe, the III-V group compound selected from GaN, GaP, GaAs, GaSb, AlN, AlP, AlAs, AlSb, InN, InP, InAs, InSb, GaNP, GaNAs, GaNSb, GaPAs, At least one of GaPSb, AlNP, AlNAs, AlNSb, AlPAs, AlPSb, InNP, InNAs, InNSb, InPAs, InPSb, GaAlNP, GaAlNAs, GaAlNSb, GaAlPAs, GaAlPSb, GaInNP, GaInNAs, GaInNSb, GaInPAs, GaInPSb, InAlNP, InAlNAs, InAlNSb, InAlPAs and InAlPSb, wherein the Group I-III-VI compound is selected from CuInS; 2 、CuInSe 2 AgInS 2 At least one of; and / or

[0025] The P-type semiconductor material includes 4,4'-N,N'-dicarbazolyl-biphenyl, poly[bis(4-phenyl)(2,4,6-trimethylphenyl)amine], N,N'-diphenyl-N,N'-bis(1-naphthyl)-1,1'-biphenyl-4,4"-diamine, N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'-biphenyl)-4,4'-diamine, poly(N,N'-bis(4-butylphenyl)-N,N'-bis(phenyl)benzidine), N,N'-bis(4-(N,N'-diphenyl-amino)phenyl)-N,N'-diphenylbiphenyl amine, 4,4',4'-tri(N-carbazolyl)-triphenylamine, 4,4',4'-tri(N-3-methylphenyl-N-phenylamino)triphenylamine, poly[(9,9'-dioctylfluorene-2,7-diyl)-co-(4,4'-(N-(4-sec-butylphenyl)diphenylamine))], poly(N-vinylcarbazole) and its derivatives, N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4-4'-diamine, poly(phenylene vinylene), poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylene vinylene], poly[ 2-methoxy-5-(3',7'-dimethyloctyloxy)-1,4-phenylene vinylene], 2,2',7,7'-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9'-spirobifluorene, 4,4'-cyclohexylbis[N,N-di(4-methylphenyl)aniline], 1,3-bis(carbazol-9-yl)benzene, polyaniline, polypyrrole, poly(p-phenylene vinylene), aromatic tertiary amines, polynuclear aromatic tertiary amines, 4,4'-bis(p-carbazyl)-1,1'-biphenyl compounds, N,N,N',N'-tetraarylbenzidine, poly(3,4-ethylenedioxythiophene) At least one of poly(vinyl)sulfonic acid and its derivatives, poly(methacrylate) and its derivatives, poly(9,9-octylfluorene) and its derivatives, polyspirofluorene and its derivatives, polythiophene and its derivatives, poly(3,4-ethylenedioxythiophene)-polystyrenesulfonic acid and its derivatives, copper phthalocyanine, 2,3,6,7,10,11-hexacyano-1,4,5,8,9,12-hexaazatriphenylene, poly(dioxyethylthiophene), 4,4',4'-tris(N-3-methylphenyl-N-phenylamino)triphenylamine, tetracyanoquinodimethane, transition metal oxides and transition metal sulfur compounds; and / or

[0026] The N-type semiconductor material includes at least one of metal oxide, doped metal oxide, II-VI semiconductor material, III-V semiconductor material and I-III-VI semiconductor material, and the metal oxide is selected from ZnO, BaO, TiO 2 SnO 2 At least one of the following; the metal oxide in the doped metal oxide is selected from ZnO, TiO 2 SnO2 At least one of the doping elements is selected from at least one of Al, Mg, Li, In, and Ga; the II-VI semiconductor group material is selected from at least one of ZnS, ZnSe, and CdS; the III-V semiconductor group material is selected from at least one of InP and GaP; the I-III-VI semiconductor material is selected from at least one of CuInS and CuGaS.

[0027] In a second aspect, an embodiment of the present application provides a thin film, which is prepared using the thin film preparation method as described above.

[0028] In a third aspect, an embodiment of the present application provides a light emitting device, including:

[0029] a first electrode;

[0030] a second electrode, arranged opposite to the first electrode;

[0031] The functional film layer is arranged between the first electrode and the second electrode, and the functional film layer includes a functional sub-film layer, and the functional sub-film layer is prepared by the thin film preparation method as described above.

[0032] In some embodiments, when the first electrode is an anode and the second electrode is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer and an electron functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electron functional layer is a thin film prepared by the thin film preparation method as described above; and / or

[0033] When the first electrode is a cathode and the second electrode is an anode, the functional film layer includes an electronic functional layer, a light-emitting layer and a hole functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electronic functional layer is a thin film prepared by the thin film preparation method as described above.

[0034] In a fourth aspect, an embodiment of the present application provides a method for preparing a light-emitting device, comprising:

[0035] Providing a light-emitting device preform, wherein the light-emitting device preform comprises a first electrode;

[0036] Preparing a functional film layer on the light-emitting device preform, wherein the functional film layer is prepared by the thin film preparation method as described above;

[0037] A second electrode is formed on the functional film layer to obtain a light-emitting device.

[0038] In some embodiments, when the first electrode is an anode and the second electrode is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer and an electron functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electron functional layer is prepared by the thin film preparation method as described above; and / or

[0039] When the first electrode is a cathode and the second electrode is an anode, the functional film layer includes an electronic functional layer, a light-emitting layer and a hole functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electronic functional layer is prepared using the thin film preparation method as described above.

[0040] In a fifth aspect, an embodiment of the present application provides a display device, comprising a light-emitting device as described above or a light-emitting device manufactured by the method for manufacturing a light-emitting device as described above.

[0041] The method for preparing a thin film provided in an embodiment of the present application comprises the following steps: after depositing a film-forming solution to form a liquid film, the liquid film is dried by gradually increasing the vacuum degree. When the vacuum degree is low, the solute in the liquid film slowly precipitates from the solution and forms a tightly arranged monolayer by self-assembly. When the vacuum degree increases, the solute continues to grow on the monolayer until it is completely precipitated, and the solute particles precipitated later are stacked on the particles precipitated earlier, and the particle arrangement becomes more regular. When the residual solvent in the liquid film is completely removed, a thin film is obtained, thereby forming a thin film with a higher density, improving the film formation quality, and reducing the surface roughness of the thin film. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for describing the embodiments.

[0043] Figure 1 A flow chart of a method for preparing a thin film provided in an embodiment of the present application.

[0044] Figure 2 A schematic diagram of the first vacuum degree change in the method for preparing a thin film provided in an embodiment of the present application.

[0045] Figure 3 A schematic diagram of the second vacuum degree change in the method for preparing a thin film provided in an embodiment of the present application.

[0046] Figure 4 A schematic diagram of the third vacuum degree change in the method for preparing a thin film provided in an embodiment of the present application.

[0047] Figure 5A schematic diagram of the fourth vacuum degree change in the method for preparing a thin film provided in an embodiment of the present application.

[0048] Figure 6 This is a schematic diagram of the fifth vacuum degree change in the method for preparing a thin film provided in an embodiment of the present application.

[0049] Figure 7 A schematic diagram of the first structure of the light-emitting device provided in an embodiment of the present application.

[0050] Figure 8 A second structural schematic diagram of the light-emitting device provided in an embodiment of the present application.

[0051] Fig. 9 A flow chart of a method for preparing a light-emitting device provided in an embodiment of the present application. DETAILED DESCRIPTION

[0052] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without making creative work are within the scope of protection of this application.

[0053] In this application, "and / or" describes the association relationship of associated objects, indicating that there may be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone. A and B can be singular or plural.

[0054] In the present application, "at least one" means one or more, and "plurality" means two or more. "At least one", "at least one of the following" or similar expressions refer to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b or c", or "at least one of a, b and c" can all mean: a, b, c, a+b, a+c, b+c, or a+b+c, where a, b, c can be single or multiple, respectively.

[0055] In the present application, when another layer is formed "on" a certain layer, the so-called "on" is a broad concept, which may indicate that the formed another layer is adjacent to the certain layer, or may indicate that there are other spacing structural layers between the another layer and the certain layer. For example, when a second electrode is formed "on" the first carrier functional layer, the so-called "on" may indicate that the formed second electrode is adjacent to the first carrier functional layer, or may indicate that there are other spacing structural layers between the second electrode and the first carrier functional layer, such as a light-emitting layer.

[0056] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.

[0057] See also Figure 1 , the present application embodiment provides a method for preparing a thin film, comprising:

[0058] S110, providing a film-forming solution, where the film-forming solution includes a film-forming material and a solvent.

[0059] S120, depositing a film-forming solution to form a liquid film.

[0060] S130, drying the liquid film in an environment with gradually increasing vacuum degree to obtain a thin film.

[0061] See also Figures 2 to 4 , when the liquid film is dried in an environment with gradually increasing vacuum degree, a first time period, a second time period and a third time period are sequentially experienced in chronological order, and the average pressure of the environment in which the liquid film is located during the first time period is defined as a first pressure, the average pressure of the environment in which the liquid film is located during the second time period is defined as a second pressure, and the average pressure of the environment in which the liquid film is located during the third time period is defined as a third pressure;

[0062] Among them, the first pressure, the second pressure and the third pressure decrease in sequence.

[0063] It can be understood that the average pressure of the environment in which the liquid film is located during the first / second / third time period refers to the average value of the pressure at each time node in the first / second / third time period as time changes.

[0064] It is known that the higher the vacuum degree, the lower the pressure. That is to say, when the first pressure, the second pressure and the third pressure decrease successively, it means that the vacuum degree of the environment in which the liquid film is located in the first time period, the vacuum degree of the environment in which the liquid film is located in the second time period, and the vacuum degree of the environment in which the liquid film is located in the third time period increase successively.

[0065] It should be noted that during the vacuum drying of the liquid film, in the first time period, under the first pressure condition, the solute in the liquid film slowly precipitates from the solution and forms a tightly arranged monolayer through self-assembly; in the second time period, under the second pressure condition, the solute continues to grow on the monolayer until it is completely precipitated, and the solute particles precipitated later are stacked on the particles precipitated earlier, and the particle arrangement is more regular; in the third time period, under the third pressure condition, the residual solvent in the liquid film is completely removed to obtain a thin film. The thin film formed in this way has a higher density and better conductivity, thereby being able to improve the electrical properties of the electroluminescent device containing the thin film.

[0066] Exemplarily, the pressure of the environment in which the liquid film is located remains constant during the first time period, or the pressure of the environment in which the liquid film is located continues to decrease during the first time period.

[0067] Exemplarily, the pressure of the environment in which the liquid film is located remains constant during the second time period, or the pressure of the environment in which the liquid film is located continues to decrease during the second time period.

[0068] Exemplarily, the pressure of the environment in which the liquid film is located remains constant during the third time period, or the pressure of the environment in which the liquid film is located continues to decrease during the third time period.

[0069] Exemplarily, the pressure of the environment in which the liquid film is located in the first time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located in the first time period and the time present a curvilinear relationship.

[0070] Exemplarily, the pressure of the environment in which the liquid film is located in the second time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located in the second time period and the time present a curvilinear relationship.

[0071] Exemplarily, the pressure of the environment in which the liquid film is located in the third time period and time present a linear relationship, or the pressure of the environment in which the liquid film is located in the third time period and time present a curvilinear relationship.

[0072] See also Figure 2 In some embodiments, the pressure of the environment in which the liquid film is located is constant during the first time period, the pressure of the environment in which the liquid film is located is constant during the second time period, and the pressure of the environment in which the liquid film is located is constant during the third time period.

[0073] See also Figure 3In some embodiments, the pressure of the environment in which the liquid film is located continues to decrease during the first time period, and the pressure of the environment in which the liquid film is located is linearly related to time during the second time period; the pressure of the environment in which the liquid film is located continues to decrease during the second time period, and the pressure of the environment in which the liquid film is located is linearly related to time during the second time period; the pressure of the environment in which the liquid film is located continues to decrease during the third time period, and the pressure of the environment in which the liquid film is located is linearly related to time during the third time period.

[0074] See also Figure 2 and Figure 3 , when the pressure of the environment in which the liquid film is located in the first / second / third time period and time show a linear relationship or a curvilinear relationship, the pressure of the environment in which the liquid film is located at the end of the first time period is greater than or equal to the pressure of the environment in which the liquid film is located at the starting point of the second time period, and the pressure of the environment in which the liquid film is located at the end of the second time period is greater than or equal to the pressure of the environment in which the liquid film is located at the starting point of the third time period.

[0075] See also Figure 4 In some embodiments, the pressure of the environment in which the liquid film is located continues to decrease during the first time period, and the pressure of the environment in which the liquid film is located and time present a curved relationship during the second time period; the pressure of the environment in which the liquid film is located continues to decrease during the second time period, and the pressure of the environment in which the liquid film is located and time present a curved relationship during the second time period; the pressure of the environment in which the liquid film is located continues to decrease during the third time period, and the pressure of the environment in which the liquid film is located and time present a curved relationship during the third time period.

[0076] It is understandable that Figure 2 Compared with the schematic diagram of vacuum degree change shown in Figure 3 and Figure 4 In the first / second / third time period, the pressure of the environment in which the liquid film is located presents a gradual trend, that is, there is no obvious mutation in the vacuum drying rate, so that the precipitation rate of the solute in the liquid film will not produce an obvious mutation. At this time, the film-forming quality of the film is higher.

[0077] Exemplarily, the first pressure is 10 -1 Pa~10 -2 Pa, the first time period is 10 minutes to 90 minutes, for example, 10 minutes, 30 minutes, 50 minutes, 70 minutes, 90 minutes, etc.

[0078] Exemplarily, the second pressure is 10 -3 Pa~10 -5 Pa, the second time period is 10 minutes to 90 minutes, for example, 10 minutes, 30 minutes, 50 minutes, 70 minutes, 90 minutes, etc.

[0079] Exemplarily, the third pressure is 10 -5 Pa~10 -7 Pa, the third time period is 10 minutes to 90 minutes, for example, 10 minutes, 30 minutes, 50 minutes, 70 minutes, 90 minutes, etc.

[0080] Exemplarily, the film-forming material includes at least one of a P-type semiconductor material, a light-emitting material, and an N-type semiconductor material.

[0081] See also Figure 5 and Figure 6 , the drying process of the liquid film in an environment with gradually increasing vacuum degree may also include:

[0082] The liquid film is subjected to vacuum drying treatment. During the vacuum drying process, the pressure of the environment in which the liquid film is located gradually decreases with time, and the pressure of the environment in which the liquid film is located is linearly related to time (e.g. Figure 5 as shown) or a curve relationship (as shown Figure 6 As shown). For example, during the vacuum drying process, the pressure of the environment in which the liquid film is located is 10 -1 Pa~10 -7 Pa.

[0083] like Figure 5 and Figure 6 As shown, since the pressure of the environment in which the liquid film is located shows a gradual trend during the vacuum drying process, that is, there is no obvious mutation in the vacuum drying rate, so that the precipitation rate of the solute in the liquid film will not produce an obvious mutation. At this time, the film formation quality of the film is relatively high.

[0084] Exemplarily, the concentration of the film-forming solution is 5 mg / ml to 100 mg / ml, for example, 5 mg / ml, 10 mg / ml, 20 mg / ml, 30 mg / ml, 40 mg / ml, 50 mg / ml, 60 mg / ml, 70 mg / ml, 80 mg / ml, 90 mg / ml, 100 mg / ml, etc.

[0085] Exemplarily, the film-forming solution is deposited by inkjet printing.

[0086] Illustratively, the viscosity of the film-forming solution is 1 cps to 10 cps, for example, 1 cps, 2 cps, 3 cps, 4 cps, 5 cps, 6 cps, 7 cps, 8 cps, 9 cps, 10 cps, and the like.

[0087] Exemplarily, the surface tension of the film-forming solution is 30 dyne / cm to 40 dyne / cm, such as 30 dyne / cm, 32 dyne / cm, 35 dyne / cm, 37 dyne / cm, 40 dyne / cm, etc.

[0088] Exemplarily, the light-emitting material may include at least one of an organic light-emitting material and a quantum dot light-emitting material.

[0089] For example, the organic light-emitting material may include, but is not limited to, 4,4'-bis(N-carbazole)-1,1'-biphenyl:tris[2-(p-tolyl)pyridine iridium(III)] (CBP:Ir(mppy) 3 ), 4,4',4"-tri(carbazole-9-yl)triphenylamine:tri[2-(p-tolyl)pyridineiridium (TCTX:Ir(mmpy)), diarylanthracene derivatives, distilbene aromatic derivatives, pyrene derivatives, fluorene derivatives, 1,4,7,10-tetra-tert-butyldinaphthylene (TBPe), rubrene derivatives (TBRb), thermally activated delayed fluorescence (TADF) materials, luminescent materials with hybrid localized-charge transfer (HLCT) excited state characteristics, exciplex luminescent materials, polyacetylene and its derivatives, polyparaphenylene and its derivatives, polythiophene and its derivatives, polyfluorene and its derivatives. One or more of them.

[0090] Exemplarily, the quantum dot luminescent material includes at least one of a single structure quantum dot and a core-shell structure quantum dot. Specifically, the material of the single structure quantum dot, the core material of the core-shell structure quantum dot and the shell material of the core-shell structure quantum dot can each include at least one of a II-VI group compound, a IV-VI group compound, a III-V group compound and a I-III-VI group compound. The shell layer of the core-shell quantum dot includes one or more layers, and the II-VI group compound is selected from CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, HgS, HgSe, HgTe, CdSeS, CdSeTe, CdSTe, ZnSeS, ZnSeTe, ZnSTe, HgSeS, HgSeTe, HgSTe, CdZnS, CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, At least one of HgZnSe, HgZnTe, CdZnSeS, CdZnSeTe, CdZnSTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe and HgZnSTe, a group IV-VI compound At least one selected from SnS, SnSe, SnTe, PbS, PbSe, PbTe, SnSeS, SnSeTe, SnSTe, PbSeS, PbSeTe, PbSTe, SnPbS, SnPbSe, SnPbTe, SnPbSSe, SnPbSeTe, SnPbSTe, and the III-V group compound selected from GaN, GaP, GaAs, GaSb, AlN, AlP, AlAs, AlSb, InN, InP, InAs, InSb, GaNP, GaNAs, GaNSb, GaPAs , GaPSb, AlNP, AlNAs, AlNSb, AlPAs, AlPSb, InNP, InNAs, InNSb, InPAs, InPSb, GaAlNP, GaAlNAs, GaAlNSb, GaAlPAs, GaAlPSb, GaInNP, GaInNAs, GaInNSb, GaInPAs, GaInPSb, InAlNP, InAlNAs, InAlNSb, InAlPAs and InAlPSb, and the I-III-VI group compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of .

[0091] Exemplarily, the P-type semiconductor material includes 4,4'-N,N'-dicarbazolyl-biphenyl (CBP), poly[bis(4-phenyl)(2,4,6-trimethylphenyl)amine] (PTAA), N,N'-diphenyl-N,N'-bis(1-naphthyl)-1,1'-biphenyl-4,4"-diamine (α-NPD), N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'-biphenyl)-4,4'-diamine (TPD), poly(N,N'-bis(4-butylphenyl)-N,N'-bis(phenyl)benzidine) (Poly-TPD), N,N'-bis(4-(N,N'-diphenyl-amino)phenyl)-N,N '-diphenylbenzidine (DNTPD), 4,4',4'-tri(N-carbazolyl)-triphenylamine (TCTA), 4,4',4'-tri(N-3-methylphenyl-N-phenylamino)triphenylamine (m-MTDATA), poly[(9,9'-dioctylfluorene-2,7-diyl)-co-(4,4'-(N-(4-sec-butylphenyl)diphenylamine))] (TFB), poly(N-vinylcarbazole) (PVK) and its derivatives, N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4-4'-diamine (NPB), poly(phenylene vinylene) (PPV), poly[2-methoxy-5-(2-ethoxy)- [2-methoxy-5-(3',7'-dimethyloctyloxy)-1,4-phenylene vinylene] (MOMO-PPV), 2,2',7,7'-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9'-spirobifluorene (spiro-omeTAD), 4,4'-cyclohexylbis[N,N-di(4-methylphenyl)aniline] (TAPC), 1,3-bis(carbazol-9-yl)benzene (MCP), polyaniline, polypyrrole, poly(p-phenylene vinylene), aromatic tertiary amines, polynuclear aromatic tertiary amines, 4,4'-bis(p-carbazyl)-1,1 '-biphenyl compounds, N,N,N',N'-tetraaryl benzidine, poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid (PEDOT:PSS) and its derivatives, polymethacrylate and its derivatives, poly(9,9-octylfluorene) and its derivatives, polyspirofluorene and its derivatives, polythiophene (TPH) and its derivatives, poly(3,4-ethylenedioxythiophene)-polystyrene sulfonic acid (PEDOT:PSS), copper phthalocyanine (CuPc), 2,3,6,7,10,11-hexacyano-1,4,5,8,9,12-hexaazatriphenylene (HAT-CN), poly(ethylenedioxythiophene) (PEDOT), PEDOT:PSS doped with MoO 3 Derivatives (PEDOT:PSS-MoO 3), 4,4',4'-tris(N-3-methylphenyl-N-phenylamino)triphenylamine (m-MTDATA), tetracyanoquinodimethane (F4-TCNQ), at least one of a transition metal oxide and a transition metal sulfide compound. Exemplarily, the transition metal oxide may include MoO x , VO x , WO x CrO x , CuO or more. Exemplarily, the metal sulfide compound may include MoS 2 、MoSe 2 , WS 2 ,WSe 2 , CuS or more.

[0092] Exemplarily, the N-type semiconductor material may include at least one of a metal oxide, a doped metal oxide, a II-VI semiconductor material, a III-V semiconductor material, and a I-III-VI semiconductor material, wherein the metal oxide is selected from ZnO, BaO, TiO 2 SnO 2 At least one of the following; the metal oxide in the doped metal oxide is selected from ZnO, TiO 2 SnO 2 At least one of the doping elements is selected from at least one of Al, Mg, Li, In, and Ga; the II-VI semiconductor group material is selected from at least one of ZnS, ZnSe, and CdS; the III-V semiconductor group material is selected from at least one of InP and GaP; the I-III-VI semiconductor material is selected from at least one of CuInS and CuGaS.

[0093] The method for preparing a thin film provided in an embodiment of the present application comprises the following steps: after depositing a film-forming solution to form a liquid film, the liquid film is dried by gradually increasing the vacuum degree. When the vacuum degree is low, the solute in the liquid film slowly precipitates from the solution and forms a tightly arranged monolayer by self-assembly. When the vacuum degree increases, the solute continues to grow on the monolayer until it is completely precipitated. The solute particles precipitated later are stacked on the particles precipitated earlier, and the particle arrangement becomes more regular. When the residual solvent in the liquid film is completely removed, a thin film is obtained, thereby forming a thin film with a higher density, improving the film formation quality, and reducing the surface roughness of the thin film.

[0094] The embodiment of the present application also provides a film, which is prepared by the film preparation method in any of the above embodiments.

[0095] See also Figure 7 and Figure 8The embodiment of the present application also provides a light-emitting device 100, including a first electrode 20 and a second electrode 70 arranged opposite to each other and a functional film layer arranged between the first electrode 20 and the second electrode 70, wherein the functional film layer includes a functional sub-film layer, and the functional sub-film layer is prepared by the thin film preparation method in any of the above embodiments.

[0096] See also Figure 7 When the first electrode 20 is an anode and the second electrode 70 is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer 50 and an electronic functional layer 60 which are stacked in sequence in the direction from the first electrode 20 to the second electrode 70, and at least one of the hole functional layer, the light-emitting layer 50 and the electronic functional layer 60 is a thin film made by the thin film preparation method in any of the above embodiments.

[0097] See also Figure 8 When the first electrode 20 is a cathode and the second electrode 70 is an anode, the functional film layer includes an electronic functional layer 60, a light-emitting layer 50, and a hole functional layer stacked in sequence in the direction from the first electrode 20 to the second electrode 70, and at least one of the hole functional layer, the light-emitting layer 50 and the electronic functional layer 60 is a thin film made by the thin film preparation method in any of the above embodiments.

[0098] See also Figure 7 and Figure 8 The hole functional layer may include at least one of a hole injection layer 30 and a hole transport layer 40 .

[0099] Exemplarily, the material of the electronic functional layer 60 can be an N-type semiconductor material, the material of the light-emitting layer 50 can be a light-emitting material, and the material of the hole functional layer (hole injection layer 30 and / or hole transport layer 40) can be a P-type semiconductor material. Since the N-type semiconductor material, the light-emitting material and the P-type semiconductor material have been described in detail above, they will not be repeated here.

[0100] See also Figure 7 and Figure 8 The light emitting device 100 may further include a substrate 10 , which is disposed on a side of the first electrode 20 away from the light emitting layer 50 .

[0101] Exemplarily, the substrate 10 may be a flexible substrate or a rigid substrate; Exemplarily, the material of the flexible substrate 10 may be an organic polymer, such as polyethylene terephthalate (PET) or polyimide (PI); Exemplarily, the rigid substrate 10 may be a glass substrate.

[0102] It can be understood that when the substrate 10 is a flexible substrate, the light-emitting device 100 is a flexible light-emitting device.

[0103] Exemplarily, the first electrode 20 and the second electrode 70 can be independently selected from a doped metal oxide electrode, a composite electrode, a graphene electrode, a carbon nanotube electrode, a metal single substance electrode or an alloy electrode. The material of the doped metal oxide electrode can include, but is not limited to, one or more of indium doped tin oxide (ITO), fluorine doped tin oxide (FTO), antimony doped tin oxide (ATO), aluminum doped zinc oxide (AZO), gallium doped zinc oxide (GZO), indium doped zinc oxide (IZO), magnesium doped zinc oxide (MZO), aluminum doped magnesium oxide (AMO), and cadmium doped zinc oxide. The composite electrode is an electrode formed by stacking two or more layers of conductive materials, such as AZO / Ag / AZO, AZO / Al / AZO, ITO / Ag / ITO, ITO / Al / ITO, ZnO / Ag / ZnO, ZnO / Al / ZnO, TiO 2 / Ag / TiO 2 、TiO 2 / Al / TiO 2 , ZnS / Ag / ZnS, ZnS / Al / ZnS, Ca / Al, LiF / Ca, LiF / Al, BaF 2 / Al、CsF / Al、CaCO 3 / Al、BaF 2 / Ca / Al, etc., where " / " represents a stacked structure, for example, AZO / Ag / AZO represents a composite electrode including an AZO layer, an Ag layer and an AZO layer stacked in sequence. The material of the metal single substance electrode may include but is not limited to one or more of silver (Ag), magnesium (Mg), aluminum (Al), gold (Au), gallium (Ga), nickel (Ni), platinum (Pt), iridium (Ir), copper (Cu), molybdenum (Mo), calcium (Ca), and barium (Ba). The alloy electrode includes but is not limited to an Au:Mg alloy electrode or an Ag:Mg alloy electrode.

[0104] In some embodiments, one of the first electrode 20 and the second electrode 70 serving as an anode may be an electrode with a relatively high work function, for example, it may include but is not limited to one or more of a doped metal oxide electrode with a relatively high work function, a metal single substance electrode with a relatively high work function, and a carbon nanotube electrode; the material of the metal single substance electrode with a relatively high work function may be Ni, Pt, Au, Ag or Ir, etc.

[0105] In some embodiments, one of the first electrode 20 and the second electrode 70 that serves as a cathode may be an electrode with a relatively low work function, for example, it may include but is not limited to a metal single substance electrode with a relatively low work function, a composite electrode with a relatively low work function, and an alloy electrode with a relatively low work function; the material of the metal single substance electrode with a relatively low work function may be Ca, Ba, Al, Mg, etc.; the structure of the composite electrode with a relatively low work function may be Ca / Al, LiF / Ca, LiF / Al, BaF 2 / Al、CsF / Al、CaCO 3 / Al、BaF 2 / Ca / Al, etc.; the alloy electrode with relatively low work function can be Au:Mg or Ag:Mg, etc.

[0106] Exemplarily, the thickness of the first electrode 20 is 20nm-140nm, for example, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, 105nm, 110nm, 115nm, 120nm, 125nm, 130nm, 135nm, 140nm, etc.

[0107] Exemplarily, the thickness of the hole functional layer is 10 nm-200 nm, for example, 10 nm, 30 nm, 50 nm, 70 nm, 100 nm, 120 nm, 150 nm, 180 nm, 200 nm, etc.

[0108] Exemplarily, the thickness of the hole injection layer 30 is 10nm-100nm, for example, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, etc.

[0109] Exemplarily, the thickness of the hole transport layer 40 is 10nm-100nm, for example, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, etc.

[0110] Exemplarily, the thickness of the light-emitting layer 50 is 10nm-100nm, for example, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, etc.

[0111] Exemplarily, the thickness of the electronic functional layer 60 is 10nm-100nm, for example, 10nm, 15nm, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, etc.

[0112] Exemplarily, the thickness of the second electrode 70 is 20nm-140nm, for example, 20nm, 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm, 100nm, 105nm, 110nm, 115nm, 120nm, 125nm, 130nm, 135nm, 140nm, etc.

[0113] See also Fig. 9 , see also Figure 7 and Figure 8 The present application also provides a method for preparing a light-emitting device, comprising:

[0114] S210 , providing a light-emitting device preform, wherein the light-emitting device preform includes a first electrode 20 .

[0115] Exemplarily, the light emitting device preform may further include a substrate 10 , which is disposed on one side of the first electrode 20 .

[0116] S220, preparing a functional film layer on the light-emitting device preform, wherein the functional film layer includes a functional sub-film layer, and the functional sub-film layer is prepared by the thin film preparation method in any of the above embodiments.

[0117] See also Figure 7 When the first electrode 20 is an anode and the second electrode 70 is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer 50 and an electronic functional layer 60 stacked in sequence in the direction from the first electrode 20 to the second electrode 70, and at least one of the hole functional layer, the light-emitting layer 50 and the electronic functional layer 60 is prepared by the thin film preparation method in any of the above embodiments.

[0118] See also Figure 8When the first electrode 20 is a cathode and the second electrode 70 is an anode, the functional film layer includes an electronic functional layer 60, a light-emitting layer 50, and a hole functional layer stacked in sequence in the direction from the first electrode 20 to the second electrode 70, and at least one of the hole functional layer, the light-emitting layer 50 and the electronic functional layer 60 is prepared using the thin film preparation method in any of the above embodiments.

[0119] See also Figure 7 and Figure 8 The hole functional layer may include at least one of a hole injection layer 30 and a hole transport layer 40 .

[0120] S230 , forming a second electrode 70 on the functional film layer to obtain the light emitting device 100 .

[0121] An embodiment of the present application further provides a display device, comprising a light-emitting device 100 manufactured by the method for manufacturing a light-emitting device in any of the above embodiments or the light-emitting device 100 in any of the above embodiments.

[0122] Exemplarily, the display device can be a mobile terminal such as a television, a mobile phone, a tablet computer, a computer monitor, or a gaming device, an augmented reality (AR) device, a virtual reality (VR) device, a data storage device, an audio playback device, a video playback device, a wearable device, or other device with a display screen, wherein the wearable device can be a smart bracelet, smart glasses, a smart watch, smart decoration, etc.

[0123] The thin film and its preparation method, the light-emitting device and its preparation method of the embodiments of the present application are described in detail below in the form of specific embodiments.

[0124] Film Example 1

[0125] This embodiment provides a thin film, and the preparation method thereof includes:

[0126] Step 1, providing a P-type semiconductor material ink, the P-type semiconductor material ink comprising a P-type semiconductor material (PEDOT:PSS) and a solvent (water), the concentration of the P-type semiconductor material ink being 30 mg / mL;

[0127] Step 2: Depositing P-type semiconductor material ink by inkjet printing to form a liquid film;

[0128] Step 3: vacuum dry the liquid film at a vacuum degree of 10 -2 Pa (constant pressure) for 60 minutes, and at a vacuum degree of 10 -5 Pa (constant pressure) for 30 minutes, and at a vacuum degree of 10-7 The film was evacuated at 300 Pa (constant pressure) for 30 minutes to obtain a thin film (hole injection layer) with a thickness of 30 nm.

[0129] Film Example 2

[0130] This embodiment provides a film, and the preparation method thereof is different from that of the film embodiment 1 in that:

[0131] In step 3, the liquid film is vacuum dried at a vacuum degree of 10 -1 Pa~10 -2 Pa (pressure changes linearly with time and gradually decreases) for 60 minutes, and at a vacuum degree of 10 -3 Pa~10 -5 Pa (pressure changes linearly with time and gradually decreases) for 30 minutes. -5 Pa~10 -7 Pa (the pressure changes linearly with time and gradually decreases) for 30 minutes to obtain a thin film (hole injection layer) with a thickness of 30 nm.

[0132] Film Example 3

[0133] This embodiment provides a film, and the preparation method thereof is different from that of the film embodiment 1 in that:

[0134] In step 3, the liquid film is vacuum dried at a vacuum degree of 10 -1 Pa~10 -2 Pa (pressure changes with time in a curve and gradually decreases) for 60 minutes, and at a vacuum degree of 10 -3 Pa~10 -5 Pa (pressure changes with time in a curve and gradually decreases) for 30 minutes, and at a vacuum degree of 10 -5 Pa~10 -7 Pa (the pressure changes with time in a curve and gradually decreases) for 30 minutes to obtain a thin film (hole injection layer) with a thickness of 30 nm.

[0135] Film Example 4

[0136] This embodiment provides a thin film, and the preparation method thereof includes:

[0137] Step 1, providing a P-type semiconductor material ink, the P-type semiconductor material ink comprising a P-type semiconductor material (TFB) and a solvent (chlorobenzene), and the concentration of the P-type semiconductor material ink is 10 mg / mL;

[0138] Step 2: Depositing P-type semiconductor material ink by inkjet printing to form a liquid film;

[0139] Step 3: vacuum dry the liquid film at a vacuum degree of 10 -1 Pa (constant pressure) for 60 minutes, and at a vacuum degree of 10 -3 Pa (constant pressure) for 30 minutes, and at a vacuum degree of 10 -5 The film was evacuated at 300 Pa (constant pressure) for 30 minutes to obtain a thin film (hole transport layer) with a thickness of 30 nm.

[0140] Film Example 5

[0141] This embodiment provides a thin film, and the preparation method thereof includes:

[0142] Step 1, providing quantum dot ink, the quantum dot ink comprising quantum dots (CdSeS / ZnS) and solvent (p-xylene), the concentration of the quantum dot ink being 30 mg / mL;

[0143] Step 2: Depositing quantum dot ink by inkjet printing to form a liquid film;

[0144] Step 3: vacuum dry the liquid film at a vacuum degree of 10 -2 Pa (constant pressure) for 60 minutes, and at a vacuum degree of 10 -5 Pa (constant pressure) for 30 minutes, and at a vacuum degree of 10 -7 The film was evacuated at 300 Pa (constant pressure) for 30 minutes to obtain a thin film (light-emitting layer) with a thickness of 30 nm.

[0145] Film Example 6

[0146] This embodiment provides a thin film, and the preparation method thereof includes:

[0147] Step 1, providing N-type semiconductor material ink, the N-type semiconductor material ink comprising N-type semiconductor material (zinc oxide nanoparticles) and solvent (ethylene glycol), the concentration of the N-type semiconductor material ink being 40 mg / mL;

[0148] Step 2: Depositing N-type semiconductor material ink by inkjet printing to form a liquid film;

[0149] Step 3: vacuum dry the liquid film at a vacuum degree of 10 -1 Pa (constant pressure) for 60 minutes, and at a vacuum degree of 10 -3 Pa (constant pressure) for 30 minutes, and at a vacuum degree of 10 -5 The film was evacuated at 3000 psi (1000 psi) for 30 minutes to obtain a thin film (electronic functional layer) having a thickness of 40 nm.

[0150] Film Comparative Example 1

[0151] This embodiment provides a thin film, and the preparation method thereof is different from that of the thin film embodiment 1 in that step 3 comprises: vacuum drying the liquid film at a vacuum degree of 10 -7 The film was evacuated at 300 Pa (constant pressure) for 60 minutes to obtain a thin film (hole injection layer) with a thickness of 30 nm.

[0152] Film Comparative Example 2

[0153] This embodiment provides a thin film, and the preparation method thereof is different from that of the thin film embodiment 4 in that step 3 comprises: vacuum drying the liquid film at a vacuum degree of 10 -7 The film was evacuated at 300 Pa (constant pressure) for 60 minutes to obtain a thin film (hole transport layer) with a thickness of 30 nm.

[0154] Film Comparative Example 3

[0155] This embodiment provides a thin film, and the preparation method thereof is different from that of the thin film embodiment 5 in that step 3 comprises: vacuum drying the liquid film at a vacuum degree of 10 -7 The film was evacuated at 300 Pa (constant pressure) for 60 minutes to obtain a thin film (light-emitting layer) with a thickness of 30 nm.

[0156] Film Comparative Example 4

[0157] This embodiment provides a thin film, and the preparation method thereof is different from that of the thin film embodiment 6 in that step 3 comprises: vacuum drying the liquid film at a vacuum degree of 10 -7 The film was evacuated at 370°C (400°C) for 60 minutes under the condition of 1.577°C (Pa) (constant pressure) to obtain a thin film (electronic functional layer) with a thickness of 40 nm.

[0158] Light-emitting device comparative example 1

[0159] This comparative example provides a light-emitting device, and the preparation method thereof comprises:

[0160] Step S1, providing an ITO substrate, the ITO substrate comprising a substrate and an anode (ITO), the thickness of the anode being 25 nm;

[0161] Step S2, inkjet printing a P-type semiconductor material ink on the anode, the P-type semiconductor material ink comprising a P-type semiconductor material (PEDOT:PSS) and a solvent (water), the concentration of the P-type semiconductor material ink being 30 mg / mL, obtaining a hole injection wet film, injecting holes into the wet film in a vacuum drying chamber, and drying the wet film under a vacuum degree of 10 -7 The hole injection layer was obtained by evacuating the gas for 60 minutes under the condition of 1.577 Pa (constant pressure). The thickness of the hole injection layer was 30 nm.

[0162] Step S3, inkjet printing a P-type semiconductor material ink on the hole injection layer, the P-type semiconductor material ink comprising a P-type semiconductor material (TFB) and a solvent (chlorobenzene), the concentration of the P-type semiconductor material ink being 10 mg / mL, to obtain a hole transport wet film, placing the hole transport wet film in a vacuum drying chamber at a vacuum degree of 10 -7 Pa (constant pressure) for 60 minutes to obtain a hole transport layer with a thickness of 30 nm;

[0163] Step S4, inkjet printing quantum dot ink on the hole transport layer, the quantum dot ink includes quantum dots and solvent (p-xylene), the concentration of the quantum dot ink is 30 mg / mL, and the quantum dot wet film is obtained, and the quantum dot wet film is placed in a vacuum drying chamber at a vacuum degree of 10 -7 The gas was pumped for 60 minutes under the condition of 1.547 Pa (constant pressure) to obtain a light-emitting layer with a thickness of 30 nm.

[0164] Step S5, inkjet printing an N-type semiconductor material ink on the light-emitting layer, the N-type semiconductor material ink comprising an N-type semiconductor material (zinc oxide nanoparticles) and a solvent (ethylene glycol), the concentration of the N-type semiconductor material ink being 40 mg / mL, to obtain an electron transport wet film, placing the electron transport wet film in a vacuum drying chamber at a vacuum degree of 10 -7 Pa (constant pressure) for 60 minutes to obtain an electronic functional layer with a thickness of 40 nm;

[0165] Step S6: evaporate a cathode (Ag) on ​​the electronic functional layer, the thickness of the cathode is 100 nm, and obtain a light-emitting device.

[0166] Light emitting device embodiment 1

[0167] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1 in that, in step S2, a hole injection layer is formed on the anode by using the preparation method in thin film embodiment 1.

[0168] Light emitting device embodiment 2

[0169] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1, in that, in step S2, a hole injection layer is formed on the anode by using the preparation method in thin film embodiment 2.

[0170] Light emitting device embodiment 3

[0171] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1 in that, in step S2, a hole injection layer is formed on the anode by using the preparation method in thin film embodiment 3.

[0172] Light emitting device embodiment 4

[0173] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1, in that, in step S3, a hole transport layer is formed on the hole injection layer by using the preparation method in thin film embodiment 4.

[0174] Light emitting device embodiment 5

[0175] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1, in that, in step S4, the preparation method in thin film embodiment 5 is used to form a light-emitting layer on the hole transport layer.

[0176] Light emitting device embodiment 6

[0177] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device comparative example 1 in that, in step S5, an electronic functional layer is formed on the light-emitting layer by using the preparation method in thin film embodiment 6.

[0178] Light emitting device embodiment 7

[0179] This embodiment provides a light-emitting device, and the preparation method thereof is different from that of the light-emitting device in Comparative Example 1 in that:

[0180] In step S2, a hole injection layer is formed on the anode using the preparation method in thin film embodiment 1;

[0181] In step S3, a hole transport layer is formed on the hole injection layer using the preparation method in thin film embodiment 4;

[0182] In step S4, a light-emitting layer is formed on the hole transport layer using the preparation method in thin film embodiment 5;

[0183] In step S5, an electronic functional layer is formed on the light-emitting layer using the preparation method in thin film embodiment 6.

[0184] Performance Test:

[0185] 1. The surface roughness of the films prepared in Film Example 1, Film Example 4, Film Example 5, Film Example 6 and Film Comparative Examples 1-4 was tested. The surface roughness test method was to move the probe of an atomic force microscope on the sample surface and then record the height change of the surface touched by the probe. Generally, we use root mean square roughness (Rq) to describe the roughness of the sample surface.

[0186] The test steps are as follows:

[0187] (1) Place the probe on the sample surface and keep the force within the appropriate range.

[0188] (2) Start moving the probe and record the measured height change.

[0189] (3) Move the probe to another location and repeat the above steps.

[0190] (4) Record the measured height change and calculate the root mean square roughness of the sample surface.

[0191] The surface roughness test results of the films are shown in Table 1.

[0192] 2. The light-emitting devices prepared in the light-emitting device embodiments 1-7 and the light-emitting device comparative example 1 were subjected to performance tests. The test indicators and test methods were as follows:

[0193] External quantum efficiency (EQE): The efficiency test system built by LabView controlling QE PRO spectrometer, Keithley 2400, and Keithley6485 is calculated to obtain the external quantum efficiency of the device by the following formula:

[0194] Where, f is the correction factor, which is 0.1932;

[0195] R(λ) is the silicon light response function;

[0196] S(λ) spectrometer normalization function;

[0197] Is is the photocurrent;

[0198] Io is the device current.

[0199] Device T95_1knit life (hours): refers to the life of the device when the brightness decays to 95% at a starting brightness of 1000 nits.

[0200] The performance test results of the light emitting device are shown in Table 2.

[0201] Table 1

[0202] Film surface roughness Rq(nm) Film Example 1 0.152 Film Example 4 0.163 Film Example 5 0.142 Film Example 6 0.251 Film Comparative Example 1 0.643 Film Comparative Example 2 0.754 Film Comparative Example 3 0.698 Film Comparative Example 4 0.835

[0203] Table 2

[0204]

[0205]

[0206] As can be seen from Table 1, the surface roughness Rq of the film (hole injection layer) prepared in Film Example 1 is less than the surface roughness Rq of the film (hole injection layer) prepared in Film Comparative Example 1, the surface roughness Rq of the film (hole transport layer) prepared in Film Example 4 is less than the surface roughness Rq of the film (hole transport layer) prepared in Film Comparative Example 2, the surface roughness Rq of the film (luminescent layer) prepared in Film Example 5 is less than the surface roughness Rq of the film (luminescent layer) prepared in Film Comparative Example 3, and the surface roughness Rq of the film (electronic functional layer) prepared in Film Example 6 is less than the surface roughness Rq of the film (electronic functional layer) prepared in Film Comparative Example 4. The surface roughness Rq of the prepared film (electronic functional layer), that is to say, compared with the film comparison examples 1-4, the films prepared in Examples 1, 4, 5, and 6 of the present application have lower roughness and better film-forming quality; the difference between the known film comparison examples 1-4 and Examples 1, 4, 5, and 6 of the present application is that the film comparison examples 1-4 are all dried in an environment with a constant vacuum degree, while Examples 1, 4, 5, and 6 of the present application are dried in an environment with a gradually increasing vacuum degree, which indicates that the film prepared by the film preparation method provided in the embodiments of the present application has better film-forming quality.

[0207] It can be seen from the data in Table 2 that the external quantum efficiency (EQE) and T95_1knit life of the light-emitting devices of light-emitting device embodiments 1-7 are greater than the external quantum efficiency (EQE) and T95_1knit life of the light-emitting device of light-emitting device comparison example 1, that is, compared with the light-emitting device comparison example 1, the light-emitting devices of light-emitting device embodiments 1-7 have higher device efficiency and longer service life. The difference between the known light-emitting device embodiments 1-7 and the light-emitting device comparison example 1 is that, in the light-emitting device comparison example 1, when preparing each functional sub-film layer (hole injection layer, hole transport layer, light-emitting layer, electronic functional layer) of the light-emitting device, the method of gradually increasing the vacuum degree was not used to vacuum dry each functional film layer, but each functional film layer was vacuum dried using a method of keeping the vacuum degree constant, while in the light-emitting device embodiments 1-7 of the present application, at least one functional film layer of the light-emitting device was prepared using a method of gradually increasing the vacuum degree to vacuum dry the functional film layer. This indicates that the functional film layer obtained by vacuum drying using the method of gradually increasing the vacuum degree in the light-emitting device embodiments 1-7 of the present application has better conductivity and stability, thereby enabling the light-emitting device to have better electrical properties and a longer service life.

[0208] The above is a detailed introduction to the thin film and its preparation method, the light-emitting device and its preparation method, and the display device provided in the embodiments of the present application. Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the present application. At the same time, for those skilled in the art, according to the ideas of the present application, there will be changes in the specific implementation methods and application scopes. In summary, the content of this specification should not be understood as limiting the present application.

Claims

1. A method for preparing a thin film, It is characterized in that include: Providing a film-forming solution, wherein the film-forming solution comprises a film-forming material and a solvent; Depositing the film-forming solution to form a liquid film; The liquid film is dried in an environment with gradually increasing vacuum degree to obtain a thin film.

2. The method for preparing the thin film according to claim 1, It is characterized in that When the liquid film is dried in an environment with gradually increasing vacuum degree, a first time period, a second time period and a third time period are sequentially experienced in chronological order, and an average pressure of the environment in which the liquid film is located in the first time period is defined as a first pressure, an average pressure of the environment in which the liquid film is located in the second time period is defined as a second pressure, and an average pressure of the environment in which the liquid film is located in the third time period is defined as a third pressure; Among them, the first pressure, the second pressure and the third pressure decrease in sequence.

3. The method for preparing the thin film according to claim 2, It is characterized in that The pressure of the environment in which the liquid film is located remains constant during the first time period, or the pressure of the environment in which the liquid film is located continues to decrease during the first time period; and / or The pressure of the environment in which the liquid film is located remains constant during the second time period, or the pressure of the environment in which the liquid film is located continues to decrease during the second time period; and / or The pressure of the environment in which the liquid membrane is located remains constant during the third time period, or the pressure of the environment in which the liquid membrane is located continues to decrease during the third time period.

4. The method for preparing the thin film according to claim 3, It is characterized in that The pressure of the environment in which the liquid film is located during the first time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located during the first time period and the time present a curvilinear relationship; and / or The pressure of the environment in which the liquid film is located during the second time period and the time present a linear relationship, or the pressure of the environment in which the liquid film is located during the second time period and the time present a curvilinear relationship; and / or The pressure of the environment in which the liquid film is located in the third time period and time present a linear relationship, or the pressure of the environment in which the liquid film is located in the third time period and time present a curvilinear relationship.

5. The method for preparing the thin film according to claim 2, It is characterized in that The first pressure is 10 -1 Pa~10 - 2 Pa, the first time period is 10 minutes to 90 minutes; and / or The second pressure is 10 -3 Pa~10 -5 Pa, the second time period is 10 minutes to 90 minutes; and / or The third pressure is 10 -5 Pa~10 -7 Pa, the third time period is 10 minutes to 90 minutes.

6. The method for preparing the thin film according to claim 1, It is characterized in that The step of drying the liquid film in an environment with gradually increasing vacuum degree comprises: The liquid film is subjected to a vacuum drying process, during which the pressure of the environment in which the liquid film is located gradually decreases with time, and the pressure of the environment in which the liquid film is located and time present a linear relationship or a curvilinear relationship.

7. A method for preparing a thin film according to any one of claims 1 to 6, It is characterized in that The film-forming material includes at least one of a P-type semiconductor material, a light-emitting material, and an N-type semiconductor material; and / or The concentration of the film-forming solution is 5 mg / ml to 100 mg / ml; and / or The film-forming solution is deposited by inkjet printing.

8. The method for preparing the thin film according to claim 7, It is characterized in that The luminescent material includes at least one of an organic luminescent material and a quantum dot luminescent material, and the organic luminescent material includes one or more of 4,4'-bis(N-carbazole)-1,1'-biphenyl:tri[2-(p-tolyl)pyridine iridium(III), 4,4',4"-tri(carbazole-9-yl)triphenylamine:tri[2-(p-tolyl)pyridine iridium, diaromatic anthracene derivatives, distilbene aromatic derivatives, pyrene derivatives, fluorene derivatives, 1,4,7,10-tetra-tert-butyl perylene, rubrene derivatives, thermally activated delayed fluorescence materials, exciplex luminescent materials, polyacetylene and its derivatives, polyparaphenylene and its derivatives, polythiophene and its derivatives, polyfluorene and its derivatives;The quantum dot luminescent material comprises at least one of a single structure quantum dot and a core-shell structure quantum dot, the material of the single structure quantum dot, the core material of the core-shell structure quantum dot and the shell material of the core-shell structure quantum dot each comprise at least one of a II-VI group compound, a IV-VI group compound, a III-V group compound and a I-III-VI group compound, the shell layer of the core-shell quantum dot comprises one or more layers, wherein the II-VI group compound is selected from CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, ZnO, HgS, HgSe, HgTe, At least one of CdSeS, CdSeTe, CdSTe, ZnSeS, ZnSeTe, ZnSTe, HgSeS, HgSeTe, HgSTe, CdZnS, CdZnSe, CdZnTe, CdHgS, CdHgSe, CdHgTe, HgZnS, HgZnSe, HgZnTe, CdZnSeS, CdZnSeTe, CdZnSTe, CdHgSeS, CdHgSeTe, CdHgSTe, HgZnSeS, HgZnSeTe and HgZnSTe, the IV-VI group compound At least one selected from SnS, SnSe, SnTe, PbS, PbSe, PbTe, SnSeS, SnSeTe, SnSTe, PbSeS, PbSeTe, PbSTe, SnPbS, SnPbSe, SnPbTe, SnPbSSe, SnPbSeTe, SnPbSTe, the III-V group compound selected from GaN, GaP, GaAs, GaSb, AlN, AlP, AlAs, AlSb, InN, InP, InAs, InSb, GaNP, GaNAs, GaNSb, GaPAs, At least one of GaPSb, AlNP, AlNAs, AlNSb, AlPAs, AlPSb, InNP, InNAs, InNSb, InPAs, InPSb, GaAlNP, GaAlNAs, GaAlNSb, GaAlPAs, GaAlPSb, GaInNP, GaInNAs, GaInNSb, GaInPAs, GaInPSb, InAlNP, InAlNAs, InAlNSb, InAlPAs and InAlPSb, wherein the Group I-III-VI compound is selected from CuInS; 2 、CuInSe 2 AgInS 2 At least one of; and / or The P-type semiconductor material includes 4,4'-N,N'-dicarbazolyl-biphenyl, poly[bis(4-phenyl)(2,4,6-trimethylphenyl)amine], N,N'-diphenyl-N,N'-bis(1-naphthyl)-1,1'-biphenyl-4,4"-diamine, N,N'-diphenyl-N,N'-bis(3-methylphenyl)-(1,1'-biphenyl)-4,4'-diamine, poly(N,N'-bis(4-butylphenyl)-N,N'-bis(phenyl)benzidine), N,N'-bis(4-(N,N'-diphenyl-amino)phenyl)-N,N'-diphenylbiphenyl amine, 4,4',4'-tri(N-carbazolyl)-triphenylamine, 4,4',4'-tri(N-3-methylphenyl-N-phenylamino)triphenylamine, poly[(9,9'-dioctylfluorene-2,7-diyl)-co-(4,4'-(N-(4-sec-butylphenyl)diphenylamine))], poly(N-vinylcarbazole) and its derivatives, N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4-4'-diamine, poly(phenylene vinylene), poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylene vinylene], poly[ 2-methoxy-5-(3',7'-dimethyloctyloxy)-1,4-phenylene vinylene], 2,2',7,7'-tetrakis[N,N-di(4-methoxyphenyl)amino]-9,9'-spirobifluorene, 4,4'-cyclohexylbis[N,N-di(4-methylphenyl)aniline], 1,3-bis(carbazol-9-yl)benzene, polyaniline, polypyrrole, poly(p-phenylene vinylene), aromatic tertiary amines, polynuclear aromatic tertiary amines, 4,4'-bis(p-carbazyl)-1,1'-biphenyl compounds, N,N,N',N'-tetraarylbenzidine, poly(3,4-ethylenedioxythiophene) At least one of poly(vinyl)sulfonic acid and its derivatives, poly(methacrylate) and its derivatives, poly(9,9-octylfluorene) and its derivatives, polyspirofluorene and its derivatives, polythiophene and its derivatives, poly(3,4-ethylenedioxythiophene)-polystyrenesulfonic acid and its derivatives, copper phthalocyanine, 2,3,6,7,10,11-hexacyano-1,4,5,8,9,12-hexaazatriphenylene, poly(dioxyethylthiophene), 4,4',4'-tris(N-3-methylphenyl-N-phenylamino)triphenylamine, tetracyanoquinodimethane, transition metal oxides and transition metal sulfur compounds; and / or The N-type semiconductor material includes at least one of metal oxide, doped metal oxide, II-VI semiconductor material, III-V semiconductor material and I-III-VI semiconductor material, and the metal oxide is selected from ZnO, BaO, TiO 2 SnO 2 At least one of the following; the metal oxide in the doped metal oxide is selected from ZnO, TiO 2 SnO 2 At least one of the doping elements is selected from at least one of Al, Mg, Li, In, and Ga; the II-VI semiconductor group material is selected from at least one of ZnS, ZnSe, and CdS; the III-V semiconductor group material is selected from at least one of InP and GaP; the I-III-VI semiconductor material is selected from at least one of CuInS and CuGaS.

9. A film, It is characterized in that The film is prepared by the method for preparing the film according to any one of claims 1 to 8.

10. A light emitting device, It is characterized in that include: a first electrode; a second electrode, arranged opposite to the first electrode; A functional film layer is arranged between the first electrode and the second electrode, and the functional film layer includes a functional sub-film layer, and the functional sub-film layer is prepared by the method for preparing a thin film according to any one of claims 1-8.

11. The light emitting device according to claim 10, It is characterized in that When the first electrode is an anode and the second electrode is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer and an electron functional layer stacked in sequence in a direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electron functional layer is a thin film prepared by the method for preparing a thin film according to any one of claims 1 to 8; and / or When the first electrode is a cathode and the second electrode is an anode, the functional film layer includes an electronic functional layer, a light-emitting layer, and a hole functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electronic functional layer is a thin film prepared by the method for preparing a thin film according to any one of claims 1 to 8.

12. A method for preparing a light emitting device, It is characterized in that include: Providing a light-emitting device preform, wherein the light-emitting device preform comprises a first electrode; Preparing a functional film layer on the light-emitting device preform, wherein the functional film layer is prepared by the method for preparing a thin film according to any one of claims 1 to 8; A second electrode is formed on the functional film layer to obtain a light-emitting device.

13. The method for preparing a light emitting device according to claim 12, It is characterized in that When the first electrode is an anode and the second electrode is a cathode, the functional film layer includes a hole functional layer, a light-emitting layer and an electron functional layer stacked in sequence in a direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electron functional layer is prepared by the method for preparing a thin film according to any one of claims 1 to 8; and / or When the first electrode is a cathode and the second electrode is an anode, the functional film layer includes an electronic functional layer, a light-emitting layer, and a hole functional layer stacked in sequence in the direction from the first electrode to the second electrode, and at least one of the hole functional layer, the light-emitting layer and the electronic functional layer is prepared by the thin film preparation method described in any one of claims 1 to 8.

14. A display device, It is characterized in that A light-emitting device comprising the light-emitting device according to claim 10 or 11 or a light-emitting device manufactured by the method for manufacturing the light-emitting device according to claim 12 or 13.