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Preparation method of ionic type negative photosensitive polyimide material

A photosensitive polyimide and ion-type technology, applied in the field of polyimide materials, can solve the problems of difficult molecular weight control, troublesome semiconductor process application, cumbersome steps, etc., and achieve highly controllable production process, high yield, and reaction The effect of simple steps

Inactive Publication Date: 2014-02-05
倚顿新材料(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the existing photosensitive polyimide preparation methods use covalent bond synthesis method, the steps are quite cumbersome, and the molecular weight is not easy to control
Some synthetic process engineering will introduce chloride ions, which will bring trouble to the application of semiconductor process

Method used

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  • Preparation method of ionic type negative photosensitive polyimide material
  • Preparation method of ionic type negative photosensitive polyimide material
  • Preparation method of ionic type negative photosensitive polyimide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1 Preparation method of the present invention (1)

[0040] At room temperature, add a certain amount of solvent 1-methyl-2-pyrrolidone (NMP) into a 250 mL three-necked flask, and blow nitrogen gas for half an hour to remove oxygen in the flask. Using the positive addition method, accurately weigh 2g (0.01mol) of 4,4’-diaminodiphenyl ether (ODA) into a three-necked flask, and stir for 20 minutes until completely dissolved. Then accurately weighed 3.087g (0.0105mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) into the three-necked flask in batches, and mechanically stirred for 8 hours to obtain polyimide (PI) precursor—polyamic acid (polyamide acid, PAA) solution. During the whole preparation process, a certain amount of NMP was added in good time to keep the solid content at 15%.

[0041] Weigh 3.297g (0.021mol) of 2-(dimethylamino)ethyl methacrylate, add it into the light yellow viscous PAA solution under the condition of avoiding light, conti...

Embodiment 2

[0047] At room temperature, add a certain amount of solvent N,N-dimethylformamide (DMF) into a 250mL three-necked flask, and blow nitrogen gas for half an hour to remove oxygen in the flask. Using the positive addition method, accurately weigh 2g (0.01mol) of 4,4’-diaminodiphenyl ether (ODA) into a three-necked flask, and stir for 20 minutes until completely dissolved. Then, accurately weighed 2.289g (0.0105mol) of pyromellitic anhydride (PMDA) was added to the three-necked flask in batches, and mechanically stirred for 8 hours to obtain the precursor of polyimide (PI) - polyamic acid (PAA ) solution. During the whole preparation process, a certain amount of DMF was added in time to keep the solid content at 15%.

[0048] Weigh 3.297g (0.021mol) of 2-(dimethylamino)ethyl methacrylate, add it into the light yellow viscous PAA solution under the condition of avoiding light, continue to stir the reaction for 5 hours, and dissolve in DMF The ionic negative photosensitive polyimi...

Embodiment 3

[0052] At room temperature, add a certain amount of solvent N,N-dimethylacetamide (DMAc) into a 250mL three-necked flask, and blow nitrogen gas for half an hour to remove oxygen in the flask. Using the positive addition method, accurately weigh 2g (0.01mol) of 4,4’-diaminodiphenyl ether (ODA) into a three-necked flask, and stir for 20 minutes until completely dissolved. Then accurately weighed 3.255g (0.0105mol) of 4,4'-oxydiphthalic anhydride (ODPA) into the three-necked flask in batches, and mechanically stirred for 8 hours to obtain the precursor of polyimide (PI) Body - polyamic acid (PAA) solution. During the whole preparation process, a certain amount of DMAc was added in time to keep the solid content at 10%.

[0053] Weigh 3.003g (0.021mol) of 2-(dimethylamino)ethyl acrylate, add it into the light yellow viscous PAA solution under the condition of avoiding light, continue to stir the reaction for 5 hours, and dissolve it in the DMAc solution The yield of ionic photos...

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Abstract

The invention relates to a preparation method of an ionic type negative photosensitive polyimide material. The preparation method comprises the following steps: a) dissolving aromatic diamine into a proper amount of organic solvent; after the aromatic diamine is completely dissolved, adding aromatic tetradianhydride in a solid suspension polymerization mode; and mechanically stirring, and reacting at room temperature to obtain a polyamide acid solution, wherein the substance amount ratio of the aromatic diamine to the aromatic tetradianhydride is 1:1.04-1:1.06; and b) in a light-shielded condition, adding photosensitive tertiary-amine small molecules into the obtained polyamide acid solution. mechanically stirring and reacting at room temperature to obtain an ionic type negative photosensitive polyamide glue solution, wherein the substance amount ratio of the photosensitive tertiary-amine small molecules to the aromatic diamine in the step a) is 2.1:1, and in the reaction process of the step a) and step b), a proper amount of organic solvent is added to ensure that the solid content of the system is 10-20%. The reaction steps of the preparation method are simple, the yield is high and close to 100%, the production process is highly controllable, and the preparation method is suitable for industrialization.

Description

technical field [0001] The invention relates to a polyimide material, in particular to a preparation method of an ion-type negative photosensitive polyimide material. Background technique [0002] Polyimide (polyimide, PI) refers to a class of polymers containing imide rings in the main chain, and is generally formed by polycondensation of aromatic diamines and aliphatic dianhydrides or aromatic dianhydrides. Due to its semi-trapezoidal and trapezoidal main chain structure and the resonance effect of the aromatic ring, it has excellent thermal stability, chemical stability, electrical insulation and high mechanical strength, and has become a high-performance material with wide application. In addition, it also has the characteristics of good adhesion to the substrate and good matching with the semiconductor process, so it has been widely used in the field of microelectronics in recent years as an insulating layer, passivation layer or stress buffer for microelectronic device...

Claims

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Application Information

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IPC IPC(8): C08G73/10G03F7/038
Inventor 路庆华闵瑞
Owner 倚顿新材料(苏州)有限公司
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