Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof

A silicon oxidation polyimide, polyimide technology, applied in the direction of chemical instruments and methods, flat products, other household appliances, etc., can solve the problem of increased material adhesion, cold welding phenomenon has not been better resolved, and affects Problems such as the normal function of the spacecraft mechanism, to achieve the effect of excellent product performance and controllable process conditions

Active Publication Date: 2018-03-06
JILIN UNIV
4 Cites 8 Cited by

AI-Extracted Technical Summary

Problems solved by technology

The occurrence of cold welding seriously affects the normal function of the spacecraft mechanism, and even leads to flight accidents
[0004] In recent years, Japan has developed polyimide-co-siloxane anti-atomic oxygen mat...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Method used

Fig. 1 is the sectional view of surface silicon oxidation polyimide-co-siloxane film 1; Fig. 2 is the difference of surface silicon oxidation polyimide-co-siloxane film 1 in embodiment 1 Scanning calorimetry (DSC) figure; Figure 3 is the X-ray photoelectron spectrum (XPS) figure of surface silicon oxidation polyimide-co-siloxane film 1; Figure 4 is surface silicon oxidation polyimide-co-silicon The scanning electron microscope (SEM) photograph of oxane thin film 1; Fig. 5 is the Si content variation trend figure of surface silicon oxidation polyimide-co-siloxane thin film 1; Table 1 is polyimide-co-siloxane Quantitative analysis results of Si XPS spectrum of thin film alkane 1 and surface silicon oxide polyimide siloxane thin film 1. It can be seen from FIG. 1 that the surface silicon oxide polyimide-co-siloxane film 1 is composed of a glass layer, a transition layer and a base layer. The glass layer is mainly composed of a silicon-oxygen stru...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Abstract

The invention discloses a surface silicon oxidation polyimide-co-silane thin film and a preparation method and belongs to the technical field of polyimide preparation. The invention provides the surface silicon oxidation polyimide-co-silane thin film. The preparation method comprises the following steps: firstly, preparing polyimide-co-silane by adopting a temperature raising and pressurizing method on the basis of a traditional two-step preparation method; and secondly, forming a glass-like functional layer on the surface by controlling conditions and adopting atomic oxygen equipment. The surface silicon oxidation polyimide-co-silane thin film consists of three parts, namely a glass layer, a transition layer and a substrate layer, wherein the glass layer consists of a silicon-oxygen structure, the transition layer consists of the silicon-oxygen structure and the polyimide-co-silane and the substrate layer consists of the polyimide-co-silane. The surface silicon oxidation polyimide-co-silane thin film, disclosed by the invention, has the advantages of excellent atomic oxygen resistance and capability of self-healing. The glass-like functional layer avoids the occurrence of a cold welding phenomenon.

Application Domain

Technology Topic

Atomic oxygenSilicon oxygen +7

Image

  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof
  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof
  • Surface silicon oxidation polyimide-co-silane thin film and preparation method thereof

Examples

  • Experimental program(10)

Example Embodiment

[0027] Example 1
[0028] (1) Dissolve 2.94g 3,3,4',4'-bipyromellitic dianhydride in 55.86g N,N-dimethylformamide (DMF) under the protection of nitrogen at room temperature. The solid content is 5%, stir for 5 hours to obtain 3,3,4',4'-bipyromellitic dianhydride solution;
[0029] (2) Under the protection of nitrogen, dissolve 0.78g of diaminopolysiloxane with a molecular weight of 860 in 14.82g of tetrahydrofuran, with a solid content of 5%, and stir for 5 hours to obtain a diaminopolysiloxane tetrahydrofuran solution;
[0030] (3) The diaminopolysiloxane tetrahydrofuran solution was slowly added dropwise to the 3,3,4',4'-bipyromellitic dianhydride solution, and after stirring for 6 hours, 1.82g 4,4 '-Diaminodiphenyl ether and 34.58g N,N-dimethylformamide (DMF), stirred for 4 hours to obtain oligomeric polyamic acid siloxane solution 1;
[0031] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 1 into an autoclave, replace the air with nitrogen, pressurize it to 0.14 MPa, keep it at 40°C for 1 hour and 80°C for 1 hour, Cool to room temperature to obtain viscous polyamic acid-co-siloxane solution 1;
[0032] (5) The polyamic acid-co-siloxane solution 1 is temperature-programmed as follows: 40°C, 4 hours; 60°C, 4 hours; 80°C, 1 hour; 100°C, 1 hour; 120°C, 2 Hours; 200°C, 1 hour; 250°C, 1 hour; 300°C, 0.5 hours; After cooling to room temperature, soak in deionized water, wash with ethanol, and dry to obtain polyimide-co-siloxane film 1 ;
[0033] (6) Use ground atomic oxygen equipment to irradiate the surface of polyimide-co-siloxane film 1 to obtain surface silicon-oxidized polyimide-co-siloxane film 1; the irradiation conditions are: temperature 253K , Energy 4.5eV, cumulative flux is 1.33×10 20 atoms/cm 2.
[0034] figure 1 It is a cross-sectional view of surface silicon oxidized polyimide-co-siloxane film 1; figure 2 Is the differential scanning calorimetry (DSC) chart of the surface silicon-oxidized polyimide-co-siloxane film 1 in Example 1; image 3 X-ray electron spectroscopy (XPS) image of surface silicon-oxidized polyimide-co-siloxane film 1; Figure 4 It is a scanning electron microscope (SEM) photo of the surface silicon oxide polyimide-co-siloxane film 1; Figure 5 It is the change trend graph of Si content of surface silicon-oxidized polyimide-co-siloxane film 1; Table 1 is polyimide-co-siloxane film 1 and surface silicon-oxidized polyimidesiloxane film 1 Si XPS spectrum quantitative analysis results. by figure 1 It can be seen that the surface silicon oxide polyimide-co-siloxane film 1 is composed of a glass layer, a transition layer and a base layer. The glass layer is mainly composed of a silicon-oxygen structure composed of a glass-like structure, the transition layer is composed of a silicon-oxygen structure and a polyimide-co-siloxane structure; the base layer is composed of a polyimide-co-siloxane structure. The glass layer acts as a functional layer to resist atomic oxygen erosion; the transition layer connects the glass layer and the base layer; the base layer plays the role of supporting the glass layer and the transition layer. by figure 2 It can be seen that the glass transition temperature of the polyimide-co-siloxane 1 prepared in Example 1 is 245°C, and it has good heat resistance; image 3 It can be seen that the peak value of XPS is 103.3eV, which is Si 4+ The characteristic peaks indicate that SiO is formed on the irradiated surface of atomic oxygen x;by Figure 4 It can be seen that the surface of the silicon-oxidized polyimide-co-siloxane film 1 prepared in Example 1 is smooth and has no obvious defects. As can be seen from Table 1, polyamide
[0035] Table 1 Quantitative analysis results of Si XPS spectra of polyimide-co-siloxane film 1 and surface silicon-oxidized polyimide-co-siloxane film 1
[0036]
[0037] The quantitative analysis results of the Si XPS spectrum of the imine-co-siloxane film 1 and the surface silicon oxide polyimide-co-siloxane film 1 show that the treatment of atomic oxygen causes the methylsiloxane on the surface of the material to change to SiO x Conversion, the conversion percentage is as high as 99%. Figure 5 It can be seen that the silicon oxide layer on the surface of the material is about 100nm, and as the depth of the film changes, SiO x The content of silicon in the battery shows a downward trend. By weighing the mass change before and after the atomic oxygen treatment, it can be seen that the outgassing volume of the material in Example 1 is 0.078mg/cm 2.

Example Embodiment

[0038] Example 2
[0039] (1) Dissolve 2.94g 3,3,4',4'-bipyromellitic dianhydride in 14.70g N,N-dimethylacetamide (DMAc) under the protection of nitrogen at room temperature. The solid content is 20%, stirring under nitrogen for 3 hours to obtain 3,3,4',4'-bipyromellitic dianhydride solution;
[0040] (2) Under the protection of nitrogen, dissolve 21 g of diaminopolysiloxane with a molecular weight of 2100 in 84 g of tetrahydrofuran, with a solid content of 20%, and stir under nitrogen for 3 hours to obtain a diaminopolysiloxane tetrahydrofuran solution;
[0041] (3) Slowly adding the diaminopolysiloxane tetrahydrofuran solution dropwise to the aromatic tetraacid dianhydride solution to obtain the oligomeric polyamic acid-co-siloxane solution 2;
[0042] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 2 to an autoclave, replace the air with nitrogen, pressurize it to 0.14 MPa, keep it at 60°C for 3 hours and 100°C for 3 hours, Cool to room temperature to obtain viscous polyamic acid-co-siloxane solution 2;
[0043] (5) The polyamic acid-co-siloxane solution 2 is temperature-programmed as follows: 40°C, 8 hours; 60°C, 8 hours; 80°C, 3 hours; 100°C, 3 hours; 120°C, 4 Hours; 200°C, 2 hours; 250°C, 2 hours; 300°C, 1 hour. After cooling down to room temperature, soak in deionized water and wash with acetone to obtain polyimide-co-siloxane film 2;
[0044] (6) Use ground atomic oxygen equipment to irradiate the surface of the polyimide-co-siloxane film 2 to obtain the surface silicon-oxidized polyimide-co-siloxane film 2; the irradiation conditions are: temperature 353K ; Energy 1.1eV; Cumulative flux 1×10 21 atoms/cm 2.
[0045] The characterization result of the surface silicon-oxidized polyimide-co-siloxane film 2 is similar to that of the surface silicon-oxidized polyimide-co-siloxane film 1.

Example Embodiment

[0046] Example 3
[0047] (1) At room temperature and under the protection of nitrogen, 2.18g pyromellitic dianhydride was dissolved in 19.08g N-methylpyrrolidone (NMP) with a solid content of 10%. Stir under nitrogen for 4h to obtain a pyromellitic dianhydride solution ;
[0048] (2) Under the protection of nitrogen, dissolve 1.48g of diaminopolysiloxane with a molecular weight of 950 in 13.32g of tetrahydrofuran, with a solid content of 10%, and stir under nitrogen for 4 hours to obtain a diaminopolysiloxane tetrahydrofuran solution ;
[0049] (3) The diaminopolysiloxane tetrahydrofuran solution was slowly added dropwise to the aromatic tetraacid dianhydride solution, and after stirring for 4 hours, 3.46g of 2,2-bis[4-(4-aminobenzene) was added. (Oxy)phenyl]propane and 31.14g of N-methylpyrrolidone (NMP), stirred for 4 hours to obtain oligomeric polyamic acid-co-siloxane solution 3;
[0050] (4) Transfer the oligomeric polyamic acid-co-siloxane solution 3 to an autoclave, replace the air with nitrogen, pressurize it to 0.14 MPa, keep it at 60°C for 3 hours and 100°C for 3 hours, Cool to room temperature to obtain viscous polyamic acid-co-siloxane solution 3;
[0051] (5) The polyamic acid-co-siloxane solution 3 is temperature-programmed as follows: 40°C, 6 hours; 60°C, 6 hours; 80°C, 2 hours; 100°C, 2 hours; 120°C, 3 Hours; 200°C, 1.5 hours; 250°C, 1.5 hours; 300°C, 0.75 hours; after cooling to room temperature, soak in deionized water, wash with ethanol, and dry to obtain polyimide-co-siloxane film 3 ;
[0052] (6) Use ground atomic oxygen equipment to irradiate the surface of the polyimide-co-siloxane film 3 to obtain the surface silicon-oxidized polyimide-co-siloxane film 3; the irradiation conditions are: temperature 283K ; Energy 3.5eV; Cumulative flux 5×10 20 atoms/cm 2.
[0053] The characterization result of the surface silicon-oxidized polyimide-co-siloxane film 3 is similar to that of the surface silicon-oxidized polyimide-co-siloxane film 1.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

no PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Similar technology patents

Classification and recommendation of technical efficacy words

Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products