CN110305464B - Continuous silicon nitride fiber reinforced resin-based composite wire and preparation method thereof - Google Patents
Continuous silicon nitride fiber reinforced resin-based composite wire and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a continuous silicon nitride fiber reinforced resin-based composite wire and a preparation method thereof, belonging to the technical field of composite materials. The composite wire is prepared from silicon nitride fibers, a lubricant, resin, a coupling agent, a softening agent and a solvent. The invention aims to reduce the damage of the fiber in the three-dimensional weaving process, the bundling property and the wear resistance of the prepared composite wire rod are obviously improved, and the prepared composite wire rod has better flexibility, can meet the bending deformation requirements of the fabric under different warp density, weft density and thickness, obviously reduces the breakage of the fiber in the three-dimensional weaving process, reduces the yarn breakage and defects in the fabric, and ensures the performance of the fabric.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a continuous silicon nitride fiber reinforced resin matrix composite wire and a preparation method thereof.
Background
The silicon nitride fiber is a ceramic fiber material with excellent performances such as high strength, high hardness, good oxidation resistance, thermal stability, excellent creep resistance, good thermal shock resistance, high electrical insulation and the like. Compared with quartz fiber, silicon nitride fiber has more excellent high temperature resistance, and is an ideal material for preparing ceramic matrix composite fiber reinforcement, so that the silicon nitride fiber has great application potential in the fields of aerospace, national defense industry and the like.
The three-dimensional fabric as a reinforcement has the advantages of good performance in the thickness direction and strong designability of shape, and the application in the aerospace field reaches a certain scale. Although the three-dimensional weaving is technically mature as the most main preparation method of the three-dimensional fabric, in the preparation process, the interweaving movement of the fibers is more frequent than that of the preparation of the plane fabric, so that the fibers are more easily damaged by stretching, bending, friction, shearing, twisting and the like, and the silicon nitride fibers are more hard and have strong brittleness, so that the damage is more serious. And the fiber is easy to break after being damaged, so that the continuity of the fiber in the fabric is reduced, broken yarns and defects in the fabric are increased, the performance of the fabric is greatly damaged, and even the preparation efficiency of the fabric is influenced. Therefore, the damage resistance of the silicon nitride fiber is improved, the damage to the silicon nitride fiber in the three-dimensional weaving process is reduced, and the preparation method has very important significance for accelerating the preparation of the silicon nitride fiber fabric reinforcement.
In order to improve weaving suitability and fiber damage resistance, it is often necessary to size or surface treat the fibers. However, the research on the silicon nitride fiber is relatively late, the silicon nitride element content of the silicon nitride fiber is high, the affinity to the organic polymer matrix is weak, and the preparation of the sizing agent and the surface treatment agent of the silicon nitride fiber is difficult. Although there are some reports on sizing agents or surface treatment agents for silicon nitride fibers, there are some problems. For example, patent with application number CN201710182433 proposes a silicon nitride fiber sizing agent, which improves strength of tows and reduces filoplume and broken filaments, but the sizing film has weak protection to the fibers when the fiber sizing rate is low, the fibers still can be damaged in a large area along with the process of three-dimensional weaving, and when the sizing rate is increased, brittleness and flexibility of the fibers can be increased, and when the warp and weft density or thickness of the fabric is increased, the fabric is very easy to break; the nitride fiber sizing agent proposed in the patent application No. CN201710887481 has a certain protection effect and improved performance on the fiber, but the production efficiency is low, and is not suitable for mass production. Therefore, it is difficult to improve the three-dimensional weaving suitability of the silicon nitride fiber by reducing the damage of the silicon nitride fiber from the viewpoint of the sizing agent or the surface treatment agent.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a continuous silicon nitride fiber reinforced resin-based composite wire and a preparation method thereof, and the composite wire is used as a three-dimensional weaving yarn to prepare a three-dimensional fabric, so that the problem that the silicon nitride fiber is greatly damaged in the manufacturing process of the three-dimensional fabric with the reinforcement is solved.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a continuous silicon nitride fiber reinforced resin-based composite wire is prepared from the following components in parts by weight:
60-80 parts of modified resin solution;
0.5-2 parts of a lubricant;
25-45 parts of silicon nitride fiber.
Preferably, the modified resin solution is prepared from resin, a softening agent, a silane coupling agent and a solvent, and comprises the following components in parts by weight:
wherein the lubricant is dimethyl silicone oil.
Preferably, the viscosity of the dimethylsilicone fluid is not higher than 300.
Wherein the resin is one of thermoplastic polyurethane and polylactic acid.
Wherein the softening agent is one or more of ethylene glycol, polyethylene glycol, polypropylene glycol and polyvinylpyrrolidone.
Preferably, the molecular weight of the polyethylene glycol is not more than 3000 in order to ensure the stability of the solution.
Wherein the solvent is one or two of dimethylformamide, ethyl acetate, acetone and butanone.
Wherein the coupling agent is a silane coupling agent.
In order to reduce the friction effect during the three-dimensional weaving, the composite wire needs to be lubricated, and the lubricant has low solubility in the solution system, so the lubricant of the invention is impregnated after the fiber is impregnated with the resin solution.
The invention also introduces a preparation method of the continuous silicon nitride fiber reinforced resin-based composite wire, which comprises the following steps:
(1) weighing the following raw materials in parts by weight:
(2) adding 10-20 parts by weight of solvent and 0.3-2 parts by weight of coupling agent into a preparation container, heating in water bath to 20-30 ℃, and stirring for 5-10 minutes to prepare coupling agent diluent;
(3) adding 60-70 parts by weight of solvent, 2-15 parts by weight of softening agent and 8-20 parts by weight of resin into the coupling agent diluent prepared in the step (2), heating in a water bath to 30-45 ℃, and stirring until the resin is completely dissolved to prepare a modified resin solution;
(4) adding the modified resin solution prepared in the steps (1) - (3) into a solution tank, adding 0.5-2 parts by weight of lubricant into a lubricant tank, placing 25-45 parts by weight of silicon nitride fiber on a bobbin creel, leading the fiber to be sequentially pulled to pass through the solution tank, a drying pipe I, the lubricant tank and a drying pipe II provided with a pipeline fan, and then winding and collecting the fiber by a winding machine to obtain the unidirectional continuous silicon nitride fiber resin-reinforced composite wire.
Further, in order to accelerate the evaporation of the solvent and avoid the softening of the polymer caused by the over-high temperature, the drying area is divided into two sections with different temperatures, preferably, the temperature of the drying pipe I is 120-150 ℃, and the temperature of the drying pipe II is 50-80 ℃.
Further, in order to accelerate the drying of the composite wire and reduce the disturbance of the air flow to the fiber, it is preferable that the air flow rate of the duct fan is in the range of 5 to 10m3/min。
Further, in view of the production rate and quality stability of the composite wire rod, it is preferable that the winding speed of the winder is 5 to 12 m/min.
It should be noted that the main purpose of the present invention is to improve the damage resistance of the fibers during the preparation of the silicon nitride fiber reinforced ceramic matrix composite, so that the silicon nitride fiber reinforced ceramic matrix composite needs to be calcined at high temperature in the preparation pretreatment process of the silicon nitride fiber reinforced ceramic matrix composite, and all the organic components in the fiber bundles are decomposed, so that the method of the present invention does not affect the next preparation process of the silicon nitride fiber reinforced ceramic matrix composite.
Compared with the prior art, the invention has the beneficial effects that on the background of solving the three-dimensional weaving problem of the silicon nitride fiber, the unidirectional continuous silicon nitride fiber reinforced resin matrix composite wire is prepared, and the invention has the following beneficial effects:
firstly, the continuous silicon nitride fiber reinforced resin matrix composite wire rod can be prepared without complex chemical reaction, has simple production process and can be suitable for production;
secondly, the continuous silicon nitride fiber reinforced resin-based composite wire is beneficial to reducing the breakage in the three-dimensional weaving process, thereby reducing the yarn breakage and defects in the fabric and ensuring the performance stability and production continuity of the fabric;
thirdly, the resin can effectively coat the fibers, reduce the hairiness on the surfaces of the fibers, remarkably improve the wear resistance and the bundling property, reduce the friction on the fibers during three-dimensional weaving and reduce the fiber damage of the prepared continuous silicon nitride fiber reinforced resin-based composite wire;
fourthly, the continuous silicon nitride fiber reinforced resin-based composite wire prepared by the invention can keep better flexibility even along with the increase of the resin content, does not become brittle and hard, and can meet the bending deformation requirement of the wire under the condition of preparing fabrics with larger warp density, weft density or thickness;
fifthly, the continuous silicon nitride fiber reinforced resin-based composite wire prepared by the invention can be used for three-dimensional weaving, and can also be used as a suture line for sewing and a braided wire.
Drawings
FIG. 1 is a schematic diagram of a preparation process and a device of a preparation method of a continuous silicon nitride fiber reinforced resin-based composite wire rod.
FIG. 2 is an electron microscope image of the composite wire obtained in example 3 of the present invention.
Detailed Description
Specific examples of the present invention are given below. The specific examples are only intended to illustrate the invention in further detail and do not limit the scope of protection of the claims of the present application.
Some of the raw materials used in the examples were as follows:
dimethyl silicone oil with the product trade name of Dow Corning PMX-200 and the viscosity of 50; the softening agent is PEG-400 and PE6-600 from Malaysia national oil company; the coupling agent is KH-550 from Nanjing chemical auxiliary agent Limited; the resin was a thermoplastic polyurethane, designated as bayer F165A.
In the following examples, a single strand of fiber is used for all fibers.
Example 1
A continuous silicon nitride fiber reinforced resin-based composite wire is prepared according to the following method:
(1) weighing the following raw materials in parts by weight:
wherein the solvent is acetone;
(2) adding 10 parts by weight of solvent and 1 part by weight of coupling agent into a preparation container, heating the mixture to 20 ℃ in a water bath, and stirring the mixture for 5 minutes to prepare coupling agent diluent;
(3) adding 76 parts by weight of solvent, 5 parts by weight of softening agent PEG-400 and 8 parts by weight of resin into the coupling agent diluent prepared in the step (2), heating the mixture in a water bath to 40 ℃, and stirring the mixture until the resin is completely dissolved to prepare a modified resin solution;
(4) adding the modified resin solution prepared in the steps (1) - (3) into a solution tank, adding 1 part by weight of lubricant into a lubricant tank, placing 40 parts by weight of silicon nitride fiber on a bobbin creel, sequentially drawing the fiber through the solution tank, a drying pipe I, the lubricant tank and a drying pipe II with a pipeline fan, and winding and collecting the fiber through a winding machine to obtain the continuous silicon nitride fiber reinforced resin-based composite wire.
Wherein the temperature of the drying pipe I is 130 ℃, and the air flow of the pipeline fan is 6m3And/min, the temperature of the drying pipe II is 50 ℃, and the winding speed of the winding machine is 10 m/min.
Example 2
A continuous silicon nitride fiber reinforced resin-based composite wire is prepared according to the following method:
(1) weighing the following raw materials in parts by weight:
wherein the solvent is acetone;
(2) adding 10 parts by weight of solvent and 1 part by weight of coupling agent into a preparation container, heating the mixture to 20 ℃ in a water bath, and stirring the mixture for 5 minutes to prepare coupling agent diluent;
(3) adding 70 parts by weight of solvent, 4 parts by weight of mixed softener of PEG-400 and 4 parts by weight of PEG-800 and 12 parts by weight of resin into the coupling agent diluent prepared in the step (2), heating the mixture to 40 ℃ in a water bath, and stirring the mixture until the resin is completely dissolved to prepare a modified resin solution;
(4) adding the modified resin solution prepared in the steps (1) - (3) into a solution tank, adding 2 parts by weight of a lubricant into a lubricant tank, placing 30 parts by weight of silicon nitride fiber on a bobbin creel, sequentially drawing the fiber through the solution tank, a drying pipe I, the lubricant tank and a drying pipe II with a pipeline fan, and winding and collecting the fiber through a winding machine to obtain the continuous silicon nitride fiber reinforced resin-based composite wire.
Wherein the temperature of the drying pipe I is 130 ℃, and the air flow of the pipeline fan is 8m3And/min, the temperature of the drying pipe II is 50 ℃, and the winding speed of the winding machine is 8 m/min.
Example 3
A continuous silicon nitride fiber reinforced resin-based composite wire is prepared according to the following method:
(1) weighing the following raw materials in parts by weight:
wherein the solvent is acetone;
(2) adding 20 parts by weight of solvent and 1 part by weight of coupling agent into a preparation container, heating the mixture to 20 ℃ in a water bath, and stirring the mixture for 5 minutes to prepare coupling agent diluent;
(3) adding 54 parts by weight of solvent, 10 parts by weight of softening agent PEG-800 and 15 parts by weight of resin into the coupling agent diluent prepared in the step (2), heating the mixture in a water bath to 40 ℃, and stirring the mixture until the resin is completely dissolved to prepare a modified resin solution;
(4) adding the modified resin solution prepared in the steps (1) - (3) into a solution tank, adding 2 parts by weight of a lubricant into a lubricant tank, placing 25 parts by weight of silicon nitride fiber on a bobbin creel, sequentially drawing the fiber through the solution tank, a drying pipe I, the lubricant tank and a drying pipe II with a pipeline fan, and winding and collecting the fiber through a winding machine to obtain the continuous silicon nitride fiber reinforced resin-based composite wire.
Wherein the temperature of the drying pipe I is 140 ℃, and the air flow of the pipeline fan is 8m3And/min, the temperature of the drying pipe II is 60 ℃, and the winding speed of the winding machine is 5 m/min.
Comparative example
To further illustrate the flexibility properties of the composite wire of the present invention, a comparative example was provided on the basis of the above-described examples. The composite wires of comparative examples 1 to 3 were produced by removing the softening agents of production steps 1 and 3 from the composite wires of examples 1 to 3.
Test example
Examples 1 to 3 and comparative examples 1 to 3 were tested for stiffness and abrasion resistance, the stiffness being a reference value for illustrating the flexibility of the composite wire, and the greater the stiffness value, the lower the flexibility of the composite wire, the weaker the ability to adapt to bending deformation of three-dimensional weaving, and the more easily damaged the composite wire during three-dimensional weaving. The abrasion resistance is a reference value of abrasion resistance when the composite wire is subjected to three-dimensional weaving through testing the times of the composite wire rubbing to fracture, and the test results are shown in table 1.
The test basis of the stiffness is as follows: GB/T7690.4-2013 reinforcing material yarn test method part 4: measurement of stiffness
The abrasion resistance was tested according to the following criteria: FZ/T01058-1999 yarn wear resistance test method reciprocating type grinding roller method
Table 1 test results for different composite wires
As can be seen from the results of the stiffness test, the stiffness of the composite wires according to examples 1 to 3, to which the softening agent was added, was decreased and the flexibility was improved, which helps the composite wires to adapt to bending deformation during three-dimensional weaving and reduce fiber damage, as compared to the composite wires according to comparative examples 1 to 3, to which the softening agent was not added.
From the results of the abrasion resistance test, it can be seen that the abrasion resistance of the composite wire is stronger than that of the untreated fiber, and from the comparison between examples 1 to 3 and comparative examples 1 to 3, the addition of the softening agent does not significantly reduce the abrasion resistance of the composite wire, and the enhancement of the abrasion resistance can further protect the fiber during the three-dimensional weaving.
Claims (2)
1. A preparation method of a continuous silicon nitride fiber reinforced resin-based composite wire is characterized by comprising the following steps:
1) weighing the following raw materials in parts by weight:
2) adding 10-20 parts by weight of acetone solvent and 0.3-2 parts by weight of coupling agent into a preparation container, heating in water bath to 20-30 ℃, and stirring for 5-10 minutes to prepare coupling agent diluent;
3) adding 60-70 parts by weight of acetone solvent, 2-15 parts by weight of polyethylene glycol softener and 8-20 parts by weight of thermoplastic polyurethane resin into the prepared coupling agent diluent, heating in a water bath to 30-45 ℃, and stirring until the resin is completely dissolved to prepare a modified resin solution;
4) adding 60-80 parts of modified resin solution into a solution tank, simultaneously adding 0.5-2 parts by weight of dimethyl silicone oil lubricant into a lubricant tank, placing 20-45 parts of silicon nitride fiber on a bobbin cradle, leading the fiber to sequentially pass through the solution tank, a drying pipe I, the lubricant tank and a drying pipe II provided with a pipeline fan, and then winding and collecting the fiber by a winding machine to obtain the continuous silicon nitride fiber reinforced resin matrix composite wire.
2. The method for preparing the silicon nitride fiber reinforced resin-based composite wire according to claim 1, wherein the temperature range set by the drying tube I is 120-150 ℃, and the airflow range set by the duct fan set by the drying tube II provided with the duct fan is 5-10m3And/min, the temperature range of the drying pipe II is 50-80 ℃, and the winding speed of the winding machine is 5-12 m/min.
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| JPS592814A (en) * | 1982-06-30 | 1984-01-09 | Fuji Fiber Glass Kk | Manufacture of sheet molding compound |
| JP2002088229A (en) * | 2000-09-18 | 2002-03-27 | Asahi Denka Kogyo Kk | Aqueous resin composition |
| JPWO2013042367A1 (en) * | 2011-09-22 | 2015-03-26 | 三洋化成工業株式会社 | Fiber sizing agent composition |
| JP5512030B1 (en) * | 2013-10-15 | 2014-06-04 | ユニチカ株式会社 | Water-based sizing agent, and glass fiber and glass fiber cloth using the same |
| CN105503200A (en) * | 2016-01-12 | 2016-04-20 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon nitride fiber filtration material |
| CN106543707B (en) * | 2016-10-28 | 2018-02-02 | 上海耐特复合材料制品有限公司 | Low temperature resistant ultra-tough nylon composite materials and preparation method thereof |
| CN106948176A (en) * | 2017-03-24 | 2017-07-14 | 武汉龙图新材料科技有限公司 | A kind of silicon nitride fiber sizing agent and preparation method thereof |
| CN107620208B (en) * | 2017-09-27 | 2019-07-19 | 中国人民解放军国防科技大学 | Nitride fiber impregnating compound and coating method thereof |
| CN108755123A (en) * | 2018-05-15 | 2018-11-06 | 天津工业大学 | A kind of silicon nitride fiber surface conditioning agent and preparation method thereof |
| CN109626845A (en) * | 2019-01-18 | 2019-04-16 | 河南光远新材料股份有限公司 | A kind of enhancing textile size of alkali-free glass fibre |
| CN109853238A (en) * | 2019-03-06 | 2019-06-07 | 福建立亚新材有限公司 | A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application |
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