Inorganic polysilazane resin

a technology of organic polysilazane and resin, which is applied in the direction of silicon compounds, transportation and packaging, liquid/solution decomposition chemical coatings, etc., to achieve the effect of small residual stress and small shrinkag

Inactive Publication Date: 2015-01-01
AZ ELECTRONICS MATERIALS LUXEMBOURG R L
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0027]As the inorganic polysilazane resin of the present invention has a high content of silicon, a siliceous film formed by using this resin can form a higher density siliceous film in comparison with a film formed by using a conventional polysilazane resin. By this reason, a siliceous film having a smaller shrinkage and a smaller residual stress than those of conventional siliceous films can b

Problems solved by technology

When the shrinkage or residual stress of the film is large, there oc

Method used

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  • Inorganic polysilazane resin
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  • Inorganic polysilazane resin

Examples

Experimental program
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Effect test

example 1

[0071]Three moles (303 g) of dichlorosilane having a purity of 99% or more were injected into a mixed solvent consisting of 1 kg of dehydrated pyridine and 3 kg of dibutyl ether at −30° C. under stirring. While maintaining the temperature of the solution at −30° C., 2 moles (34 g) of ammonia gas having a purity of 99.9% or more were injected into the mixture under stirring. The mixture was reacted for 2 hours while maintaining the temperature at −30° C. to obtain a solution of silazane oligomer containing unreacted Si—Cl. The existence of the unreacted Si—Cl was confirmed by using FTIR, VIR-9450 manufactured by JASCO Corporation.

[0072]The oligomer obtained contains following compounds and the like, and the total number of NH and the total number of Cl in the oligomer are the same.

[0073]In the oligomer formation process, HCl was generated but most of it was reacted immediately with excessive pyridine to form pyridine hydrochloride and the pyridine hydrochloride formed was precipitate...

example 2

[0075]A silazane oligomer solution containing unreacted Si—Cl was prepared by the same process as Example 1. To the silazane oligomer solution obtained, 2 moles (204 g) of N,N,N′,N′-tetramethyldiaminomethane were added and this reaction system was heated gradually to 80° C. under stirring and held at this temperature for one hour, followed by cooling down gradually to the room temperature. Subsequently, 1 mole (17 g) of ammonia gas having a purity of 99.9% was injected again to the mixture under stirring and then the mixture was allowed to stand for 30 minutes. The obtained slurry reaction mixture was filtered with a glass filter to remove pyridine hydrochloride to obtain a filtrate. To the filtrate obtained, dibutyl ether was added and then heated to 50° C., followed by distillation under the reduced pressure of 20 mmHg to remove pyridine at this temperature. Through these processes, Solution B having a concentration of 20% by weight, which contains a resin (Resin B) having a weigh...

example 3

[0076]Three moles (303 g) of dichlorosilane having a purity of 99% or more were injected into a mixed solvent consisting of 300 g of dehydrated pyridine and 3 kg of dibutyl ether under stirring at 0° C. While maintaining the temperature of the solution at 0° C., 3 moles (51 g) of ammonia gas were injected into the mixture under stirring. The mixture was reacted for 2 hours under stirring while maintaining the temperature at 0° C. to obtain a solution of polysilazane polymer. It was confirmed by FTIR, VIR-9450 manufactured by JASCO Corporation that the polymer does not contain the unreacted Si—Cl. The molecular weight of the polymer was 2,300. Pyridine hydrochloride and ammonium chloride, which were formed in the synthesis process of the polysilazane polymer, were removed by filtration with a centrifugal separation filter.

[0077]Subsequently, 1 mole (107 g) of 2,6-lutidine was added to the filtrate and then the reaction system was heated gradually to 90° C., followed by injecting 1 mo...

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Abstract

An inorganic polysilazane resin of the present invention has a Si/N ratio (i.e. a ratio of contained silicon atoms to contained nitrogen atoms) of 1.30 or more. The inorganic polysilazane resin having such a high Si content can be produced by, for example, a method in which an inorganic polysilazane compound containing both Si—NH and Si—Cl is heated to react NH with Cl, a method in which a silazane oligomer (polymer) that leaves no Si—Cl bond is synthesized and a dihalosilane is added to the synthesized silazane oligomer (polymer) to perform a thermal reaction, and the like. A siliceous film can be formed by, for example, applying a coating composition containing the inorganic polysilazane resin onto a base plate and then dried and the dried product is then oxidized by bringing the dried product into contact with water vapor or hydrogen peroxide vapor and water vapor under heated conditions.

Description

FIELD OF THE INVENTION[0001]The present invention relates to an inorganic polysilazane resin, more specifically, to an inorganic polysilazane resin which can be suitably used for forming an insulation film, a passivation film, a planarization film, a protective film, a hard mask, a stress adjusting film, a sacrifice film, and the like of electronic devices such as a semiconductor element, etc. The present invention also relates to a coating composition containing the inorganic polysilazane resin, a method for forming a siliceous film by use of the inorganic polysilazane resin, and a siliceous film formed by the method.BACKGROUND ART[0002]A polysilazane is well known as a compound useful for a precursor of silicon nitride (for example, see Patent literature 1 below). In recent years, it has also attracted attention as a material for forming an insulation film such as an interlayer insulation film, a passivation film, a protective film, a planarization film, and the like of the electr...

Claims

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Application Information

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IPC IPC(8): C01B33/08C09D1/00
CPCC09D1/00C01B33/08C23C18/122C01B21/087H01L21/0217C23C18/1225H01L21/02326C23C18/1212Y10T428/31663H01L21/02282H01L21/02222H01L21/02164C08G77/62C09D183/16C01B33/126C08L83/16H01L21/02323H01L21/02337H01L31/02167Y02E10/50
Inventor FUJIWARA, TAKASHIGROTTENMUELLER, RALPHKANDA, TAKASHINAGAHARA, TATSURO
Owner AZ ELECTRONICS MATERIALS LUXEMBOURG R L
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