WO2019227735A1 - Oled发光材料的制备方法 - Google Patents

Oled发光材料的制备方法 Download PDF

Info

Publication number
WO2019227735A1
WO2019227735A1 PCT/CN2018/103391 CN2018103391W WO2019227735A1 WO 2019227735 A1 WO2019227735 A1 WO 2019227735A1 CN 2018103391 W CN2018103391 W CN 2018103391W WO 2019227735 A1 WO2019227735 A1 WO 2019227735A1
Authority
WO
WIPO (PCT)
Prior art keywords
emitting material
solution
solvent
light
preparing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2018/103391
Other languages
English (en)
French (fr)
Inventor
易国霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
Original Assignee
Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd filed Critical Wuhan China Star Optoelectronics Semiconductor Display Technology Co Ltd
Priority to US16/091,116 priority Critical patent/US10868259B2/en
Publication of WO2019227735A1 publication Critical patent/WO2019227735A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent materials, e.g. electroluminescent or chemiluminescent
    • C09K11/06—Luminescent materials, e.g. electroluminescent or chemiluminescent containing organic luminescent materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/649—Aromatic compounds comprising a hetero atom
    • H10K85/657—Polycyclic condensed heteroaromatic hydrocarbons
    • H10K85/6572—Polycyclic condensed heteroaromatic hydrocarbons comprising only nitrogen in the heteroaromatic polycondensed ring system, e.g. phenanthroline or carbazole
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
    • C09K2211/10—Non-macromolecular compounds
    • C09K2211/1003—Carbocyclic compounds
    • C09K2211/1007—Non-condensed systems
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
    • C09K2211/10—Non-macromolecular compounds
    • C09K2211/1003—Carbocyclic compounds
    • C09K2211/1014—Carbocyclic compounds bridged by heteroatoms, e.g. N, P, Si or B
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
    • C09K2211/10—Non-macromolecular compounds
    • C09K2211/1018—Heterocyclic compounds
    • C09K2211/1025—Heterocyclic compounds characterised by ligands
    • C09K2211/1029—Heterocyclic compounds characterised by ligands containing one nitrogen atom as the heteroatom

Definitions

  • the invention relates to the technical field of OLED display, in particular to a method for preparing an OLED light-emitting material.
  • the structure of an OLED is mainly composed of an anode, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron input layer, an electron injection layer, and a cathode.
  • the light-emitting layer of the OLED has a concentration quenching effect, that is, the quantum efficiency will decrease when the concentration of the light-emitting material increases. Therefore, if a single light-emitting material is used in the OLED light-emitting layer, the light-emitting efficiency of the light-emitting layer will be greatly reduced.
  • Host material host light-emitting material
  • Dopant material guest light-emitting material
  • the doping ratio is designed based on maximizing the luminous efficiency, but the vaporized atoms or molecules during the evaporation process will cause disproportionate dissipation of the host material and the dopant material during flight, and eventually lead to the luminescent material The change of the doping ratio leads to a decrease in luminous efficiency.
  • the existing OLED light-emitting materials have the problem of non-proportional dissipation of host and guest materials during the evaporation process.
  • the invention provides a method for preparing an OLED light-emitting material, so as to solve the disproportionate dissipation of the Host material and the Dopant material during the evaporation process of the existing OLED light-emitting material, resulting in a change in the doping ratio of the finally prepared light-emitting material. This causes a problem that the luminous efficiency is reduced.
  • the invention provides a method for preparing an OLED light-emitting material, including the following steps:
  • the first solvent is a mixed solution of absolute ethanol and polyethylene glycol
  • the host light-emitting material is a carbazole derivative
  • the second solvent is absolute ethanol.
  • the guest luminescent material is a carbazole derivative.
  • the host luminescent material is first added to the first solvent, and then the mixture is uniformly stirred.
  • the guest luminescent material is first added to the second solvent, and then the mixture is stirred uniformly.
  • the invention also provides a method for preparing an OLED light-emitting material, comprising the following steps:
  • the mixed solution is placed in a reaction kettle and treated at a temperature of 40 to 60 ° C. for 18 to 36 hours to obtain a reaction solution.
  • reaction solution is centrifuged to collect a precipitate
  • the precipitate is dried in a drying box filled with a protective gas to obtain the OLED light-emitting material.
  • the first solvent is a mixed solution of absolute ethanol and polyethylene glycol
  • the host light-emitting material is a carbazole derivative
  • the second solvent is absolute ethanol.
  • the guest luminescent material is a carbazole derivative.
  • the host luminescent material is first added to the first solvent, and then the mixture is uniformly stirred.
  • the first solution and the second solution are mixed in a polytetrafluoroethylene liner, and the mixed solution is in the polytetrafluoroethylene
  • the filling degree in the lining is 75% to 80%.
  • the method before the step S30, the method further includes the following steps:
  • the drying box and the glove box are evacuated before being filled with a protective gas, wherein the protective gas includes any one or more of nitrogen, helium, and argon.
  • the invention provides another method for preparing an OLED light-emitting material, including the following steps:
  • the first solvent is a mixed solution of absolute ethanol and polyethylene glycol
  • the host light-emitting material is a carbazole derivative
  • the second solvent is absolute ethanol.
  • the guest luminescent material is a carbazole derivative.
  • the host luminescent material is first added to the first solvent, and then the mixture is uniformly stirred.
  • the guest luminescent material is first added to the second solvent, and then the mixture is stirred uniformly.
  • the beneficial effect of the present invention is: by uniformly mixing the Host material and the Dopant material to obtain a treated light-emitting layer material, compared with the direct deposition of the Dopant material directly on the Host material in the prior art, not only the Host material and Dopant
  • the material is evaporated according to the designed ratio before evaporation, and the Host material and the Dopant material can be dissipated in the same proportion during the evaporation process, and the optimal doping ratio designed before the evaporation is hardly changed, which reduces the light emission.
  • the effect of efficiency overcomes the defect of low luminous efficiency existing in the prior art.
  • FIG. 1 is a flowchart of a preparation method according to Embodiment 1 of the present invention.
  • FIG. 2 is a flowchart of a preparation method according to a second embodiment of the present invention.
  • the present invention is directed to a liquid crystal display device of the prior art. Since the liquid crystal display panel and the backlight module have an integrated structure, the development of the liquid crystal display device is restricted, and the operation of the backlight module is complicated and the cost is high. This problem can be solved by this embodiment.
  • a method for preparing an OLED light-emitting material includes the following steps:
  • the host light-emitting material is a carbazole derivative.
  • the host light-emitting material may be mCP (1,3-dicarbazole-9-ylbenzene).
  • the molecular structure formula of the mCP is as follows:
  • the guest luminescent material is a carbazole derivative
  • the guest luminescent material is composed of a donor material and an acceptor material
  • the donor material may be DMOC (3,6-diMethoxy-9H-carbazole, 3,6- Dimethoxy-9H-carbazole), DMAC (9,9-DIMETHYL-9,10-DIHYDRO-ACRIDINE, 9,10-dihydro-9,9-dimethylacridine), carbazole, etc.
  • the acceptor material may be DPS (Diphenylsulfo, diphenylsulfone), BP (4,4'-Dimethylbenzophenone, 4,4-dimethylbenzophenone), etc.
  • the guest light emitting material may be DPS-DMOC, DPS -DMAC, BP-DMOC or BP-DMAC, the molecular structure formula of the donor material is as follows:
  • the molecular structure of the acceptor material is as follows:
  • the host (Host) luminescent material used in this embodiment is mCP, and the guest (Dopant) luminescent material is BP-DMAC.
  • the optimal doping ratio of the designed host and guest luminescent materials is 3%, the light-emitting layer has the highest luminous efficiency. Therefore, according to the above-mentioned doping ratio, 5 g of the host material mCP is prepared, 0.15 g of Dopant material BP-DMAC, and 30mL of absolute ethanol and 10mL of polyethylene glycol;
  • step S101 5 g of mCP is first added to 20 mL of the first solvent, and then vigorously stirred with a magnetic stirrer for 10 minutes, and the mixture is uniformly mixed to obtain the first solution.
  • step S102 0.15 g of BP-DMAC is first added to 20 mL of the second solvent, and then stirred with a magnetic stirrer for 10 minutes, and the mixture is uniformly mixed to obtain the second solution.
  • step S103 the first solution is slowly dropped into the second solution under a normal temperature environment to obtain a mixed solution, and the dropping rate is 2 drops / second. If the adding speed is too fast, the mixed solution A precipitate will be formed in the medium, and it is difficult to form a sol, thereby causing uneven dispersion of the first solution and the second solution.
  • step S104 the method further includes the following steps: first forming the mixed solution into a sol, then forming the sol into a wet gel, and then forming the wet gel into a dry gel.
  • the mixed solution is first placed in a constant temperature water bath at 50 ° C, and heated and stirred until a uniform and stable sol is formed, and then the sol is aged. After about 1 hour, the precipitation is complete and the wet coagulation is obtained. Gel, and finally the wet gel is left for 12 to 24 hours. After the first solvent and the second solvent are volatilized, the xerogel is obtained.
  • step S105 the influence of moisture or oxidizing substances in the air on the luminescent material is avoided.
  • the xerogel is placed in a drying box filled with a protective gas for drying treatment, and the xerogel is further dried.
  • the first solvent and the second solvent carried in the glue are removed.
  • the drying temperature of the xerogel is 100 ° C, and the drying time of the xerogel is 8-10 hours.
  • the method further includes the following steps: firstly evacuating the drying box, and then filling nitrogen as a protective gas.
  • the present invention provides a method for preparing an OLED light-emitting material, including the following steps:
  • the mixed solution is placed in a reaction kettle and treated at a temperature of 40 to 60 ° C. for 18 to 36 hours to obtain a reaction solution.
  • the precipitate is placed in a vacuum drying box for drying to obtain the OLED light-emitting material.
  • the host light-emitting material is a carbazole derivative.
  • the host light-emitting material may be mCP (1,3-dicarbazole-9-ylbenzene).
  • the molecular structure formula of the mCP is as follows:
  • the guest luminescent material is a carbazole derivative
  • the guest luminescent material is composed of a donor material and an acceptor material
  • the donor material may be DMOC (3,6-diMethoxy-9H-carbazole, 3,6- Dimethoxy-9H-carbazole), DMAC (9,9-DIMETHYL-9,10-DIHYDRO-ACRIDINE, 9,10-dihydro-9,9-dimethylacridine), carbazole, etc.
  • the acceptor material may be DPS (Diphenylsulfo, diphenylsulfone), BP (4,4'-Dimethylbenzophenone, 4,4-dimethylbenzophenone), etc.
  • the guest light emitting material may be DPS-DMOC, DPS -DMAC, BP-DMOC or BP-DMAC, the molecular structure formula of the donor material is as follows:
  • the molecular structure of the acceptor material is as follows:
  • the host (Host) luminescent material used in this embodiment is mCP and the guest (Dopant) luminescent material is DPS-DMAC.
  • the optimal doping ratio of the designed host and guest luminescent materials is 3%, the light-emitting layer has the highest luminous efficiency. Therefore, according to the above-mentioned doping ratio, 5 g of the host material mCP is prepared, 0.15 g of Dopant material DPS-DMAC, and 30mL of absolute ethanol and 10mL of polyethylene glycol;
  • reaction kettle and lining Before starting the experiment, put the reaction kettle and lining to be used in the glove box in advance, and then evacuate the glove box and drying box, and then introduce nitrogen to form a glove box environment with protective gas.
  • step S203 in a glove box filled with a protective gas, the second solution is added to a 50 mL polytetrafluoroethylene liner, and the first solution is added dropwise to the second solution.
  • the mixture is uniformly mixed to form the mixed liquid, and the degree of filling of the mixed liquid in the polytetrafluoroethylene lining is 75% to 80%, that is, the volume of the mixed liquid is the polytetrafluoroethylene lining 75% to 80% of the volume, preferably, the degree of filling of the mixed liquid in the polytetrafluoroethylene liner is 80%.
  • the reaction kettle is a high-pressure reactor, and the temperature of the high-pressure reactor cannot be too high, so as to prevent the first luminescent material and the second luminescent material from being effectively vaporized, resulting in the inability to evaporate. Plating into luminescent layer.
  • the processing time of the mixed liquid should not be too long, otherwise it will affect the subsequent evaporation process.
  • the reaction temperature of the mixed liquid is 40-55 ° C, and the processing time of the mixed liquid is 20-30 hours. .
  • step S205 centrifugation of the reaction solution is performed in a centrifuge, the rotation speed of the centrifugation is 8000-10000r / min, and the centrifugation time is 5-20min.
  • the host material and the Dopant material are uniformly mixed to obtain a processed light-emitting layer material.
  • the Dopant material is directly deposited on the Host material. , Not only can Host material and Dopant material be vapor-deposited according to the designed ratio before evaporation, but also can make Host material and Dopant material dissipate in the same proportion during the evaporation process, hardly changing the optimal design before evaporation.
  • the doping ratio reduces the influence on the luminous efficiency and overcomes the defect of low luminous efficiency existing in the prior art.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

一种OLED发光材料的制备方法，步骤包括：将主体发光材料与第一溶剂混合，形成第一溶液；将客体发光材料与第二溶剂混合，形成第二溶液；将第一溶液与第二溶液混合，形成混合液；对所述混合液进行胶化处理，形成干凝胶；对所述干凝胶进行干燥处理，形成所述OLED发光材料。

Description

OLED发光材料的制备方法 技术领域
本发明涉及OLED显示技术领域，特别涉及一种OLED发光材料的制备方法。
背景技术
目前OLED的结构主要由阳极、空穴注入层、空穴传输层、发光层、电子传输层、电子输入层、电子注入层、和阴极组成。由于OLED的发光层具有浓度淬熄效应，即当发光材料的浓度增大时量子效率会降低，因此OLED发光层若采用单一发光材料会极大降低发光层的发光效率，目前OLED发光层多采用Host材料(主体发光材料)与Dopant材料(客体发光材料)搭配蒸镀而成。掺杂比例是依据最大程度地增大发光效率而设计的，但是在蒸镀过程中的气化原子或分子在飞行过程中，会致使Host材料和Dopant材料的无比例耗散，最终导致发光材料掺杂比例的变化，从而导致发光效率降低。
综上所述，现有的OLED发光材料在蒸镀过程中存在主客体材料无比例耗散的问题。
技术问题
本发明提供一种OLED发光材料的制备方法，以解决现有的OLED发光材料在蒸镀过程中出现Host材料与Dopant材料的无比例耗散，导致最终制备的发光材料掺杂比例发生变化，进而导致发光效率降低的问题。
技术解决方案
为解决上述问题，本发明提供的技术方案如下：
本发明提供一种OLED发光材料的制备方法，包括以下步骤：
S10，将第一溶剂和主体发光材料混合，形成第一溶液；
S20，将第二溶剂和客体发光材料混合，形成第二溶液；
S30，将所述第一溶液和所述第二溶液混合，形成混合液；
S40，对所述混合液进行胶化处理，形成干凝胶；
S50，对所述干凝胶进行干燥处理，形成所述OLED发光材料，其中，所述干凝胶的干燥温度是100℃，所述干凝胶的干燥时间是8～10小时。
在本发明的至少一种实施例中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。在本发明的至少一种实施例中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
在本发明的至少一种实施例中，所述S20中，先将所述客体发光材料加入到所述第二溶剂中，再搅拌均匀。
本发明还提供一种OLED发光材料的制备方法，包括以下步骤：
S10，将第一溶剂和主体发光材料混合，形成第一溶液；
S20，将第二溶剂和客体发光材料混合，形成第二溶液；
S30，在充有保护气体的手套箱中，将所述第一溶液和所述第二溶液混合，形成混合液；
S40，将所述混合液置于反应釜中，在40～60℃的温度下处理18～36小时，得到反应液；
S50，将所述反应液进行离心处理，收集沉淀；
S60，将所述沉淀置于充有保护气体的干燥箱中进行干燥，得到所述OLED发光材料。
在本发明的至少一种实施例中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体 发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。在本发明的至少一种实施例中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
在本发明的至少一种实施例中，在所述S30中，所述第一溶液与所述第二溶液混合在聚四氟乙烯内衬中，且所述混合液在所述聚四氟乙烯内衬中的填充度为75％～80％。
在本发明的至少一种实施例中，在所述S30之前，还包括以下步骤：
先对干燥箱和手套箱抽真空，再充入保护气体，其中，所述保护气体包括氮气、氦气、氩气中的任意一种或多种的组合。
本发明提供另一种OLED发光材料的制备方法，包括以下步骤：
S10，将第一溶剂和主体发光材料混合，形成第一溶液；
S20，将第二溶剂和客体发光材料混合，形成第二溶液；
S30，将所述第一溶液和所述第二溶液混合，形成混合液；
S40，对所述混合液进行胶化处理，形成干凝胶；
S50，对所述干凝胶进行干燥处理，形成所述OLED发光材料。
在本发明的至少一种实施例中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。在本发明的至少一种实施例中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
在本发明的至少一种实施例中，所述S20中，先将所述客体发光材料加入到所述第二溶剂中，再搅拌均匀。
有益效果
本发明的有益效果为：通过将Host材料与Dopant材料均匀混合，得到处理后的发光层材料，相较于现有技术中直接在Host材料上直接沉积Dopant材料而言，不仅使Host材料和Dopant材料按蒸镀前设计好的比例进行蒸镀，也能使Host材料和Dopant材料在蒸镀过程中同比例地耗散，几乎不改变蒸镀前设计好的最优掺杂比例，减轻对发光效率的影响，克服了现有技术存在的发光效率低的缺陷。
附图说明
为了更清楚地说明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单介绍，显而易见地，下面描述中的附图仅仅是发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例一的制备方法流程图；
图2为本发明实施例二的制备方法流程图。
本发明的最佳实施方式
以下各实施例的说明是参考附加的图示，用以例示本发明可用以实施的特定实施例。本发明所提到的方向用语，例如[上]、[下]、[前]、[后]、[左]、[右]、[内]、[外]、[侧面]等，仅是参考附加图式的方向。因此，使用的方向用语是用以说明及理解本发明，而非用以限制本发明。在图中，结构相似的单元是用以相同标号表示。
本发明针对现有技术的液晶显示装置，由于液晶显示面板与背光模组为一体式结构，制约液晶显示装置向薄型化发展，且针对背光模组进行维修时操作比较复杂，成本较高的技术问题，本实施例能够解决该缺陷。
实施例一
如图1所示，一种OLED发光材料的制备方法，包括以下步骤：
S101，将第一溶剂和主体发光材料混合，形成第一溶液；
S102，将第二溶剂和客体发光材料混合，形成第二溶液；
S103，将所述第一溶液和所述第二溶液混合，形成混合液；
S104，对所述混合液进行胶化处理，形成干凝胶；
S105，对所述干凝胶进行干燥处理，形成所述OLED发光材料。
所述主体发光材料采用咔唑类衍生物，所述主体发光材料可以为mCP(1,3-二咔唑-9-基苯),所述mCP分子结构式如下所示：
Figure PCTCN2018103391-appb-000001
所述客体发光材料采用咔唑类衍生物，所述客体发光材料由供体材料和受体材料组成，所述供体材料可以为DMOC(3,6-diMethoxy-9H-carbazole，3,6-二甲氧基-9H-咔唑)、DMAC(9,9-DIMETHYL-9,10-DIHYDRO-ACRIDINE，9,10-二氢-9,9-二甲基吖啶)、咔唑等，所述受体材料可以为DPS(Diphenylsulfo，二苯砜)、BP(4,4'-Dimethylbenzophenone，4,4-二甲基二苯甲酮)等，所述客体发光材料可以为DPS-DMOC、DPS-DMAC、BP-DMOC或者BP-DMAC,所述供体材料分子结构式如下：
Figure PCTCN2018103391-appb-000002
所述受体材料分子结构式如下：
Figure PCTCN2018103391-appb-000003
本实施例中所用主体(Host)发光材料为mCP、客体(Dopant)发光材料为BP-DMAC。
真空蒸镀前，当设计的主体发光材料和客体发光材料的最优掺杂比例为3％时，发光层的发光效率最高，因此，根据上述的掺杂比例，准备5g的Host材料mCP，0.15g的Dopant材料BP-DMAC，以及无水乙醇30mL、聚乙二醇10mL；
取10mL无水乙醇和10mL聚乙二醇配制成20mL的所述第一溶剂；取20mL无水乙醇配制成20mL的所述第二溶剂。
在所述S101步骤中，先将5g的mCP加入到20mL的所述第一溶剂中，再用磁力搅拌器强力搅拌10min，混合均匀，得到所述第一溶液。
在所述S102步骤中，先将0.15g的BP-DMAC加入到20mL的所述第二溶剂中，再用磁力搅 拌器搅拌10min，混合均匀，得到所述第二溶液。
在所述S103步骤中，在常温环境下，将所述第一溶液缓慢滴入所述第二溶液中，得到混合液，滴加速度为2滴/秒，若加入速度过快，所述混合液中会形成沉淀，很难形成溶胶，进而导致所述第一溶液与所述第二溶液分散不均匀。
在所述S104步骤中，还包括以下步骤：先使所述混合液形成溶胶，再使所述溶胶形成湿凝胶，之后使所述湿凝胶形成干凝胶。
具体地，先将所述混合液置于50℃的恒温水浴中，进行加热搅拌，至形成均匀稳定的溶胶，再将所述溶胶进行陈化，约1小时后，待沉淀完全，得到湿凝胶，最后将所述湿凝胶，静置12～24小时，待所述第一溶剂、第二溶剂挥发后，得到所述干凝胶。
在所述S105步骤中，避免空气中水分或氧化性物质对发光材料的影响，优选地，将所述干凝胶放置在充有保护气体的干燥箱中进行干燥处理，进一步将所述干凝胶中带有的所述第一溶剂、第二溶剂去除掉。优选地，所述干凝胶的干燥温度是100℃，所述干凝胶的干燥时间是8～10小时。
在所述S105步骤之前，还包括以下步骤：先对干燥箱抽真空，再充入氮气作为保护气体。
实施例二
如图2所示，本发明提供一种OLED发光材料的制备方法，包括以下步骤：
S201，将第一溶剂和主体发光材料混合，形成第一溶液；
S202，将第二溶剂和客体发光材料混合，形成第二溶液；
S203，将所述第一溶液和所述第二溶液混合，形成混合液；
S204，将所述混合液置于反应釜中，在40～60℃的温度下处理18～36小时，得到反应液；
S205，将所述反应液进行离心，收集沉淀；
S206，将所述沉淀置于真空干燥箱中进行干燥，得到所述OLED发光材料。
所述主体发光材料采用咔唑类衍生物，所述主体发光材料可以为mCP(1,3-二咔唑-9-基苯),所述mCP分子结构式如下所示：
Figure PCTCN2018103391-appb-000004
所述客体发光材料采用咔唑类衍生物，所述客体发光材料由供体材料和受体材料组成，所述供体材料可以为DMOC(3,6-diMethoxy-9H-carbazole，3,6-二甲氧基-9H-咔唑)、DMAC(9,9-DIMETHYL-9,10-DIHYDRO-ACRIDINE，9,10-二氢-9,9-二甲基吖啶)、咔唑等，所述受体材料可以为DPS(Diphenylsulfo，二苯砜)、BP(4,4'-Dimethylbenzophenone，4,4-二甲基二苯甲酮)等，所述客体发光材料可以为DPS-DMOC、DPS-DMAC、BP-DMOC或者BP-DMAC,所述供体材料分子结构式如下：
Figure PCTCN2018103391-appb-000005
所述受体材料分子结构式如下：
Figure PCTCN2018103391-appb-000006
本实施例中所用主体(Host)发光材料为mCP、客体(Dopant)发光材料为DPS-DMAC。
真空蒸镀前，当设计的主体发光材料和客体发光材料的最优掺杂比例为3％时，发光层的发光效率最高，因此，根据上述的掺杂比例，准备5g的Host材料mCP，0.15g的Dopant材料DPS-DMAC，以及无水乙醇30mL、聚乙二醇10mL；
取10mL无水乙醇和10mL聚乙二醇配制成20mL的所述第一溶剂；取20mL无水乙醇配制成20mL的所述第二溶剂。
在实验开始之前，将待使用的反应釜、内衬等均事先放入到手套箱中，之后对手套箱和干燥箱抽真空，再通入氮气，形成一通有保护气体的手套箱环境。
在所述S203步骤中，在充有保护气体的手套箱中，将所述第二溶液加入到50mL的聚四氟乙烯内衬中，再将所述第一溶液滴加到所述第二溶液中，混合均匀，形成所述混合液，所述混合液在所述聚四氟乙烯内衬中的填充度为75％～80％，即所述混合液体积是所述聚四氟乙烯内衬体积的75％～80％，优选地，所述混合液在所述聚四氟乙烯内衬中的填充度为80％。在所述S204步骤中，所述反应釜选择高压反应釜，所述高压反应釜的温度不能太高，以免所述第一发光材料和所述第二发光材料不能有效气化，从而导致不能蒸镀成发光层。所述混合液的处理时间也不能太长，否则也会影响后续的蒸镀工艺，优选地，所述混合液的反应温度为40～55℃，所述混合液的处理时间为20～30小时。
在S205步骤中，所述反应液的离心在离心机中进行，所述离心的转速为8000～10000r/min，离心时间为5～20min。
有益效果：本发明所提供的OLED发光材料的制备方法，将Host材料与Dopant材料均匀混合，得到处理后的发光层材料，相较于现有技术中直接在Host材料上直接沉积Dopant材料而言，不仅使Host材料和Dopant材料按蒸镀前设计好的比例进行蒸镀，也能使Host材料和Dopant材料在蒸镀过程中同比例地耗散，几乎不改变蒸镀前设计好的最优掺杂比例，减轻对发光效率的影响，克服了现有技术存在的发光效率低的缺陷。
综上所述，虽然本发明已以优选实施例揭露如上，但上述优选实施例并非用以限制本发明，本领域的普通技术人员，在不脱离本发明的精神和范围内，均可作各种更动与润饰，因此本发明的保护范围以权利要求界定的范围为准。

Claims (13)

  1. 一种OLED发光材料的制备方法，其中，包括以下步骤：
    S10，将第一溶剂和主体发光材料混合，形成第一溶液；
    S20，将第二溶剂和客体发光材料混合，形成第二溶液；
    S30，将所述第一溶液和所述第二溶液混合，形成混合液；
    S40，对所述混合液进行胶化处理，形成干凝胶；
    S50，对所述干凝胶进行干燥处理，形成所述OLED发光材料，其中，所述干凝胶的干燥温度是100℃，所述干凝胶的干燥时间是8～10小时。
  2. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。
  3. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
  4. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述S20中，先将所述客体发光材料加入到所述第二溶剂中，再搅拌均匀。
  5. 一种OLED发光材料的制备方法，其中，包括以下步骤：
    S10，将第一溶剂和主体发光材料混合，形成第一溶液；
    S20，将第二溶剂和客体发光材料混合，形成第二溶液；
    S30，在充有保护气体的手套箱中，将所述第一溶液和所述第二溶液混合，形成混合液；
    S40，将所述混合液置于反应釜中，在40～60℃的温度下处理18～36小时，得到反应液；
    S50，将所述反应液进行离心处理，收集沉淀；
    S60，将所述沉淀置于充有保护气体的干燥箱中进行干燥，得到所述OLED发光材料。
  6. 根据权利要求5所述的OLED发光材料的制备方法，其中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。
  7. 根据权利要求5所述的OLED发光材料的制备方法，其中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
  8. 根据权利要求5所述的OLED发光材料的制备方法，其中，在所述S30中，所述第一溶液与所述第二溶液混合在聚四氟乙烯内衬中，且所述混合液在所述聚四氟乙烯内衬中的填充度为75％～80％。
  9. 根据权利要求5所述的OLED发光材料的制备方法，其中，在所述S30步骤之前，还包括以下步骤：
    先对干燥箱和手套箱抽真空，再充入保护气体，其中，所述保护气体包括氮气、氦气、氩气中的任意一种或多种的组合。
  10. 一种OLED发光材料的制备方法，其中，包括以下步骤：
    S10，将第一溶剂和主体发光材料混合，形成第一溶液；
    S20，将第二溶剂和客体发光材料混合，形成第二溶液；
    S30，将所述第一溶液和所述第二溶液混合，形成混合液；
    S40，对所述混合液进行胶化处理，形成干凝胶；
    S50，对所述干凝胶进行干燥处理，形成所述OLED发光材料。
  11. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述第一溶剂为无水乙醇和聚乙二醇的混合溶液，所述主体发光材料为咔唑类衍生物；所述第二溶剂为无水乙醇，所述客体发光材料为咔唑类衍生物。
  12. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述S10中，先将所述主体发光材料加入到所述第一溶剂中，再搅拌均匀。
  13. 根据权利要求1所述的OLED发光材料的制备方法，其中，所述S20中，先将所述客体发光材料加入到所述第二溶剂中，再搅拌均匀。
PCT/CN2018/103391 2018-05-30 2018-08-31 Oled发光材料的制备方法 Ceased WO2019227735A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US16/091,116 US10868259B2 (en) 2018-05-30 2018-08-31 Method for manufacturing OLED light-emitting material

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201810536530.6A CN108641707B (zh) 2018-05-30 2018-05-30 Oled发光材料的制备方法
CN201810536530.6 2018-05-30

Publications (1)

Publication Number Publication Date
WO2019227735A1 true WO2019227735A1 (zh) 2019-12-05

Family

ID=63758502

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2018/103391 Ceased WO2019227735A1 (zh) 2018-05-30 2018-08-31 Oled发光材料的制备方法

Country Status (2)

Country Link
CN (1) CN108641707B (zh)
WO (1) WO2019227735A1 (zh)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110854302B (zh) 2019-10-31 2021-02-26 深圳市华星光电半导体显示技术有限公司 Oled显示面板及其制备方法、oled显示装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106340594A (zh) * 2016-09-30 2017-01-18 南京邮电大学 一种白光有机电致发光器件及其制备方法
CN106816541A (zh) * 2017-01-11 2017-06-09 瑞声科技（南京）有限公司 磷光蓝有机发光二极管装置
CN106920900A (zh) * 2017-04-05 2017-07-04 武汉华星光电技术有限公司 一种oled中发光层原料的处理方法及应用

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101222802A (zh) * 2007-01-11 2008-07-16 株式会社藤仓 有机电致发光元件以及光布线模块
CN102659846B (zh) * 2012-03-30 2015-07-15 中国科学院宁波材料技术与工程研究所 N-取代苯基苯并咪唑类三价铱有机金属配合物、其制备方法与用途
CN102867920A (zh) * 2012-08-28 2013-01-09 李崇 白色oled发光体
CN103413893A (zh) * 2013-08-01 2013-11-27 中国航空工业集团公司北京航空材料研究院 一种oled器件
CN103474584B (zh) * 2013-09-29 2016-01-06 京东方科技集团股份有限公司 有机电致发光器件及其制备方法、显示装置
CN105870347A (zh) * 2016-04-15 2016-08-17 京东方科技集团股份有限公司 量子点发光器件及其制备方法、显示基板和显示装置
CN107403870B (zh) * 2017-06-21 2019-10-01 武汉华星光电半导体显示技术有限公司 Woled器件

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106340594A (zh) * 2016-09-30 2017-01-18 南京邮电大学 一种白光有机电致发光器件及其制备方法
CN106816541A (zh) * 2017-01-11 2017-06-09 瑞声科技（南京）有限公司 磷光蓝有机发光二极管装置
CN106920900A (zh) * 2017-04-05 2017-07-04 武汉华星光电技术有限公司 一种oled中发光层原料的处理方法及应用

Also Published As

Publication number Publication date
CN108641707A (zh) 2018-10-12
CN108641707B (zh) 2020-04-10

Similar Documents

Publication Publication Date Title
Chu et al. Perovskite light‐emitting diodes with external quantum efficiency exceeding 22% via small‐molecule passivation
CN109135725B (zh) 一种钙钛矿量子点复合膜及其制备方法
Zhang et al. High comprehensive circularly polarized electroluminescence performance improved by chiral coassembled host materials
WO2020037856A1 (zh) 热活化延迟荧光材料及其合成方法
CN107177239A (zh) 墨水配方、光电器件以及光电器件的功能层的制备方法
WO2019075866A1 (zh) 电子传输层喷墨打印墨水及其制备方法
CN110886017A (zh) 一种全无机铯铅卤族钙钛矿纳米晶薄膜的制备方法
CN110845976B (zh) 一种钙钛矿量子点胶水的制备方法
Xu et al. Solution-processed pure blue thermally activated delayed fluorescence emitter organic light-emitting diodes with narrowband emission
WO2020098114A1 (zh) 绿光热活化延迟荧光材料及其合成方法、电致发光器件
WO2020113789A1 (zh) 绿光热活化延迟荧光材料及其合成方法、电致发光器件
CN107342348B (zh) 一种led器件的制备方法
Wang et al. In Situ Green Preparation of Highly Stable CsPbBr3–Polyimide Films for Flexible Liquid Crystal Displays
WO2019227735A1 (zh) Oled发光材料的制备方法
WO2015192480A1 (zh) 有机水氧阻隔材料、oled显示装置及其制备方法
TWI781319B (zh) 發光裝置及其製作方法
Yao et al. Room temperature high-efficiency welding of an ultra-long silver nanowire network for flexible transparent electrodes
CN107546340A (zh) 红光全无机杂化钙钛矿量子点墨水及其柔性发光二极管的制备方法
CN106920900B (zh) 一种oled中发光层原料的处理方法及应用
US11549057B2 (en) Quantum dot luminescent material an method of producing thereof
WO2020134204A1 (zh) 量子点发光二极管的制备方法
CN110055062A (zh) 一种二氧化硅/氧化铝包覆量子点及其制备方法及量子点薄膜的制备方法
Zhou et al. Improving the efficiency and stability of green-light perovskite CsPbBr3 LEDs via low-temperature annealing
US10868259B2 (en) Method for manufacturing OLED light-emitting material
US11404681B2 (en) Display panel, manufacturing method thereof, and display device

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 18920661

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 18920661

Country of ref document: EP

Kind code of ref document: A1