CN110760310A - Method for improving mechanical property of liquid crystal polymer product - Google Patents
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Abstract
The invention discloses a method for improving the mechanical property of a liquid crystal polymer product, belonging to the technical field of polymer composite materials, the method comprises the steps of carrying out heat treatment on the liquid crystal polymer product under the protective atmosphere, wherein the heat treatment temperature is 250 ℃, and the time is 6 h; in the heat treatment temperature rise process, when the environmental temperature is below 100 ℃, the temperature rise is carried out at the speed of 5 ℃/min, when the temperature is 100 ℃ and 200 ℃, the temperature rise is carried out at the speed of 2 ℃/min, when the temperature is 200 ℃ and 250 ℃, the temperature rise is carried out at the speed of 1 ℃/min; in the heat treatment and temperature reduction process, when the ambient temperature is 250-50 ℃, the temperature is reduced at the speed of 1 ℃/min. The method is simple and easy to operate, can improve the crystallization nonuniformity of polymer molecules, can obtain the LCP product with a stable crystallization structure, can eliminate the internal stress of the product, enables the product not to be easily brittle or mechanically damaged in the using process, and improves the mechanical property of the LCP product.
Description
Technical Field
The invention belongs to the technical field of high-molecular composite materials, and particularly relates to a method for improving the mechanical property of a liquid crystal polymer product.
Background
A Liquid Crystal Polymer (LCP) is a high molecular substance that is composed of a rigid molecular chain and a flexible molecular chain, and has both Liquid fluidity and crystalline physical properties, and anisotropy, under certain physical conditions. The material has excellent heat resistance and forming processing performance. Liquid crystal polymers can be further classified into lyotropic liquid crystal polymers and thermotropic liquid crystal polymers. The former is in a liquid crystal state in a solvent, and the latter is in a liquid crystal state due to a change in temperature. The liquid crystal polymer has compact molecular packing and high orientation during molding, so that it has small linear expansion coefficient, low molding shrinkage, outstanding strength and elastic modulus and excellent heat resistance, and has relatively high load deformation temperature, some of which may reach 340 deg.c.
Due to its unique molecular chain rigidity, the LCP has little entanglement phenomenon peculiar to a polymer, and is very significant in orientation in the flow direction, unlike a general thermoplastic resin. The molecular chain orientation relaxation time is long, and the orientation in the flow direction can be kept and cured when injection molding and heating molding are carried out, so that the LCP has large anisotropy from the aspects of mechanical properties and other properties, and the orientation of liquid crystal molecules is avoided as much as possible in the LCP film molding process.
The literature at home and abroad reports that various methods change the molecular orientation of LCP (liquid Crystal Polymer) molecules, for example, a static mixing device is added in a die head, polymer molecules are interwoven together at a specific angle in a multi-layer co-extrusion mode, or a rotary die head blow molding mode is adopted, but the above schemes are implemented by improving equipment or selecting processes in the preparation process of the LCP, and the literature or patents of LCP products (thick products or thin films) are rarely reported in a post-treatment mode after sample preparation is finished, and the phenomena of uneven heating and over-fast cooling of the products are difficult to avoid in the preparation process of the products, so that the service performance of the products is influenced.
LCP is excellent in dimensional stability, electrical insulation, heat resistance, thermal stability, chemical resistance and is widely used as a functional part or a structural member. Therefore, how to effectively improve the mechanical properties of LCP products by post-treatment means is a problem that must be considered in the industry.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: a method for improving the mechanical properties of liquid crystal polymer articles by post-treatment, annealing, is provided.
In order to solve the technical problems, the invention adopts the technical scheme that: a method of improving the mechanical properties of a liquid crystalline polymer article comprising the steps of: carrying out heat treatment on the liquid crystal polymer product under the protective atmosphere, wherein the temperature of the heat treatment is 250 ℃, and the time is 6 h;
in the heat treatment temperature rise process, when the environmental temperature is below 100 ℃, the temperature rise is carried out at the speed of 5 ℃/min, when the temperature is 100 ℃ and 200 ℃, the temperature rise is carried out at the speed of 2 ℃/min, when the temperature is 200 ℃ and 250 ℃, the temperature rise is carried out at the speed of 1 ℃/min;
in the heat treatment and temperature reduction process, when the ambient temperature is 250-50 ℃, the temperature is reduced at the speed of 1 ℃/min.
The invention has the beneficial effects that: the method for improving the mechanical property of the liquid crystal polymer product solves the problems that the liquid crystal polymer product has different orientation degrees and crystallinities in all directions due to the fact that molecules are very easy to rapidly freeze and crystallize in the cooling process, the orientation of the product in different directions is obvious, and the brittleness is high. The method starts from post-treatment, and does not need to improve the equipment end, so that enterprises do not need to change or improve a large amount of equipment in the actual production process, the product quality is improved, the cost required by modification is greatly reduced, the product is improved and the product performance is improved in a more convenient mode, and the operation is simpler.
Drawings
FIG. 1 is a schematic representation of a stack of liquid crystal polymer films according to an embodiment of the present invention;
FIG. 2 is a process parameter diagram illustrating a heat treatment according to an embodiment of the present invention.
Detailed Description
In order to explain technical contents, achieved objects, and effects of the present invention in detail, the following description is made with reference to the accompanying drawings in combination with the embodiments.
The most key concept of the invention is as follows: annealing the processed liquid crystal polymer product, and strictly controlling the annealing temperature, the annealing time and the temperature rise and fall process, thereby improving the mechanical property of the liquid crystal polymer product.
The method for improving the mechanical property of the liquid crystal polymer product comprises the following steps:
carrying out heat treatment on the liquid crystal polymer product under the protective atmosphere, wherein the temperature of the heat treatment is T3 ℃, and the time is 6 h;
in the heat treatment temperature rise process, when the environmental temperature is below T1, the temperature is raised at the speed of 5 ℃/min, when the temperature is T1-T2, the temperature is raised at the speed of 2 ℃/min, when the temperature is T2-T3, the temperature is raised at the speed of 1 ℃/min;
in the heat treatment cooling process, when the ambient temperature is T3-50 ℃, cooling at the speed of 1 ℃/min;
here, the heat treatment temperature (T3) is selected to be 20-40 ℃ below the melting point Tm, T1 is around the glass transition temperature Tg of LCP, T2 is 80-100 ℃ below the melting point Tm of LCP, and the values of T1, T2 and T3 and the optimal value of T3 depend on the material characteristics.
Specifically, the liquid crystal polymer product is subjected to heat treatment under the protective atmosphere, the temperature of the heat treatment is 250 ℃, and the time is 6 hours;
in the heat treatment temperature rise process, when the environmental temperature is below 100 ℃, the temperature rise is carried out at the speed of 5 ℃/min, when the temperature is 100 ℃ and 200 ℃, the temperature rise is carried out at the speed of 2 ℃/min, when the temperature is 200 ℃ and 250 ℃, the temperature rise is carried out at the speed of 1 ℃/min;
in the heat treatment and temperature reduction process, when the ambient temperature is 250-50 ℃, the temperature is reduced at the speed of 1 ℃/min.
From the above description, the beneficial effects of the present invention are: aiming at the problems that molecules are very easy to rapidly freeze and crystallize in the cooling process of a liquid crystal polymer, so that the degree of orientation and crystallinity in all directions are different, the orientation of the product in different directions is obvious, and the brittleness is high, the method for improving the mechanical property of a liquid crystal polymer product improves the problem of crystallization nonuniformity of the liquid crystal polymer product by annealing (heat treatment) the liquid crystal polymer product and strictly controlling the temperature of the heat treatment and the temperature rise and drop processes in the heat treatment;
according to the method, the crystallization nonuniformity of polymer molecules is improved in a mode of annealing post-treatment, so that the LCP product with a stable crystalline structure is obtained; the internal stress of the product is eliminated through a simple post-treatment mode, so that the product is not easy to crack or mechanically damage in the using process; by means of slow cooling and annealing treatment, the mechanical properties (tensile modulus and elastic modulus) of the LCP product are improved, and the toughness is improved;
the method starts from post-treatment, can directly improve the mechanical property of the existing LCP product, does not need to replace or readjust equipment or process to prepare the product, is simple and efficient, enables enterprises to avoid replacing or improving a large amount of equipment in the actual production process, improves the product quality and greatly reduces the cost required by modification.
Further, the liquid crystal polymer article is a liquid crystal polymer film.
Furthermore, the liquid crystal polymer product can also be liquid crystal polymer products in various forms such as liquid crystal polymer sheets, particles and the like.
Furthermore, before the liquid crystal polymer film is subjected to heat treatment, protective films are respectively added on the upper part and the lower part of the liquid crystal polymer film for covering.
From the above description, when the liquid crystal polymer article is a liquid crystal polymer film, by adding a protective film and applying a minute weight to the edge, curling of the film when heated at high temperature can be effectively prevented.
Further, the protective film is a solid polyimide protective film.
Furthermore, the material of the liquid crystal polymer product is aromatic-containing liquid crystal polymer resin.
Further, the liquid crystal polymer product is made of an LCP resin synthesized by copolymerizing polycyclic rigid molecular monomers, introducing naphthalene rings into the molecular structure, and using aliphatic segments in the molecular chain.
Furthermore, the material of the liquid crystal polymer product is other crystallizable polymers, such as polyvinylidene fluoride and polyethylene terephthalate.
Further, the protective atmosphere is a nitrogen atmosphere or an argon atmosphere.
Further, the equipment for carrying out heat treatment is a vacuum drying oven, a silicon-molybdenum sintering furnace or an oil bath pan.
Furthermore, the maximum temperature of the high-temperature annealing equipment for heat treatment needs to be heated to more than 300 ℃, and the temperature can be controlled by a program.
Example 1 is:
the method for improving the mechanical property of the liquid crystal polymer product comprises the following specific steps:
1) respectively adding protective films, namely thermosetting polyimide films (shown in figure 1) on and under the liquid crystal polymer film, wherein the area of the thermosetting polyimide films is larger than that of the liquid crystal polymer film, and tiny weights are applied to the edges of the thermosetting polyimide films;
2) putting the liquid crystal polymer film covered with the protective film into a vacuum drying oven for heat treatment in nitrogen atmosphere, before heating, vacuumizing, injecting nitrogen, vacuumizing and injecting nitrogen into the vacuum drying oven, repeating the steps for 5 times until the air remained in the vacuum drying oven is replaced by the nitrogen atmosphere, and completely filling the drying oven with the nitrogen atmosphere; then, heating to carry out heat treatment (see figure 2), wherein the temperature of the heat treatment is 250 ℃, and the time is 6 h;
in the heat treatment heating process, when the temperature in the vacuum oven is below 100 ℃, the temperature is heated at the speed of 5 ℃/min, when the temperature is increased at 100 ℃ and 200 ℃, the temperature is increased at the speed of 2 ℃/min, when the temperature is increased at 200 ℃ and 250 ℃, the temperature is increased at the speed of 1 ℃/min; in the heat treatment cooling process, when the temperature in the vacuum oven is 250-50 ℃, cooling at the speed of 1 ℃/min, stopping controlling the temperature when the temperature is below 50 ℃, naturally cooling to room temperature, taking out the liquid crystal polymer film covered with the protective film, and separating the protective film to obtain the treated liquid crystal polymer film;
the liquid crystal polymer film is an LCP film prepared by blow molding.
Example 2 is:
the method for improving the mechanical property of the liquid crystal polymer product comprises the following specific steps:
1) respectively adding protective films, namely thermosetting polyimide films, on the upper and lower sides of the liquid crystal polymer film, wherein the area of each thermosetting polyimide film is larger than that of the liquid crystal polymer film, and a tiny weight is applied to the edge of each thermosetting polyimide film;
2) putting the liquid crystal polymer film covered with the protective film into a vacuum drying oven for heat treatment in nitrogen atmosphere, before heating, vacuumizing, injecting nitrogen, vacuumizing and injecting nitrogen into the vacuum drying oven, repeating the steps for 5 times until the air remained in the vacuum drying oven is replaced by the nitrogen atmosphere, and completely filling the drying oven with the nitrogen atmosphere; then, starting to heat up for heat treatment, wherein the heat treatment temperature is 250 ℃ and the time is 6 h;
in the heat treatment heating process, when the temperature in the vacuum oven is below 100 ℃, the temperature is heated at the speed of 5 ℃/min, when the temperature is increased at 100 ℃ and 200 ℃, the temperature is increased at the speed of 2 ℃/min, when the temperature is increased at 200 ℃ and 250 ℃, the temperature is increased at the speed of 1 ℃/min; in the heat treatment cooling process, when the temperature in the vacuum oven is 250-50 ℃, cooling at the speed of 1 ℃/min, stopping controlling the temperature when the temperature is below 50 ℃, naturally cooling to room temperature, taking out the liquid crystal polymer film covered with the protective film, and separating the protective film to obtain the treated liquid crystal polymer film;
the liquid crystal polymer film is an LCP film prepared by a biaxial stretching method.
Example 3 is:
the method for improving the mechanical property of the liquid crystal polymer product comprises the following specific steps:
1) respectively adding protective films, namely thermosetting polyimide films, on the upper and lower sides of the liquid crystal polymer film, wherein the area of each thermosetting polyimide film is larger than that of the liquid crystal polymer film, and a tiny weight is applied to the edge of each thermosetting polyimide film;
2) putting the liquid crystal polymer film covered with the protective film into a vacuum drying oven for heat treatment in nitrogen atmosphere, before heating, vacuumizing, injecting nitrogen, vacuumizing and injecting nitrogen into the vacuum drying oven, repeating the steps for 5 times until the air remained in the vacuum drying oven is replaced by the nitrogen atmosphere, and completely filling the drying oven with the nitrogen atmosphere; then, starting to heat up for heat treatment, wherein the heat treatment temperature is 250 ℃ and the time is 6 h;
in the heat treatment heating process, when the temperature in the vacuum oven is below 100 ℃, the temperature is heated at the speed of 5 ℃/min, when the temperature is increased at 100 ℃ and 200 ℃, the temperature is increased at the speed of 2 ℃/min, when the temperature is increased at 200 ℃ and 250 ℃, the temperature is increased at the speed of 1 ℃/min; in the heat treatment cooling process, when the temperature in the vacuum oven is 250-50 ℃, cooling at the speed of 1 ℃/min, stopping controlling the temperature when the temperature is below 50 ℃, naturally cooling to room temperature, taking out the liquid crystal polymer film covered with the protective film, and separating the protective film to obtain the treated liquid crystal polymer film;
the liquid crystal polymer film is an LCP film prepared by a hot pressing method.
Example 4 is:
the method for improving the mechanical property of the liquid crystal polymer product comprises the following specific steps:
placing the liquid crystal polymer sheet in a silicon-molybdenum sintering furnace to carry out heat treatment in an argon atmosphere (see figure 2), and continuously introducing argon into the silicon-molybdenum sintering furnace, wherein the heat treatment temperature is 250 ℃ and the time is 6 hours;
in the heat treatment heating process, when the temperature in the silicon-molybdenum sintering furnace is below 100 ℃, the temperature is raised at the speed of 5 ℃/min, when the temperature is raised to 100 ℃ and 200 ℃, the temperature is raised at the speed of 2 ℃/min, when the temperature is raised to 200 ℃ and 250 ℃, the temperature is raised at the speed of 1 ℃/min;
in the heat treatment cooling process, when the temperature in the silicon-molybdenum sintering furnace is 250-50 ℃, cooling at the speed of 1 ℃/min, stopping controlling the temperature when the temperature is below 50 ℃, naturally cooling to room temperature, and taking out the liquid crystal polymer sheet;
the liquid crystal polymer sheet is made of LCP resin with the melting point of 250-380 ℃.
Experimental example:
the folding endurance of the liquid crystal polymer films of examples 1-3(LCP-1#, LCP-2#, LCP-3#) after annealing treatment was tested, and the results are shown in Table 1.
TABLE 1
It can be seen from the table that after the annealing treatment, the folding resistance of the LCP film is improved, the bending times before repeated bending to fracture are increased, the toughness of the product is obviously improved, and the problems of obvious orientation and large brittleness of the product in different directions are solved.
In summary, the method for improving the mechanical properties of the liquid crystal polymer product provided by the invention solves the problems that the liquid crystal polymer product has different orientation degrees and crystallinities in all directions due to the fact that molecules are very easy to rapidly freeze and crystallize in the cooling process, the orientation properties of the product in different directions are obvious, and the brittleness is high. The method starts from post-treatment, and does not need to improve the equipment end, so that enterprises do not need to change or improve a large amount of equipment in the actual production process, the quality of products is improved, meanwhile, the production cost required by modification is greatly reduced, the products are improved and the performance of the products is improved in a more convenient mode, and the operation is simpler.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to the related technical fields, are included in the scope of the present invention.
Claims (6)
1. A method of improving the mechanical properties of a liquid crystal polymer article comprising the steps of: carrying out heat treatment on the liquid crystal polymer product under the protective atmosphere, wherein the temperature of the heat treatment is 250 ℃, and the time is 6 h;
in the heat treatment temperature rise process, when the environmental temperature is below 100 ℃, the temperature rise is carried out at the speed of 5 ℃/min, when the temperature is 100 ℃ and 200 ℃, the temperature rise is carried out at the speed of 2 ℃/min, when the temperature is 200 ℃ and 250 ℃, the temperature rise is carried out at the speed of 1 ℃/min;
in the heat treatment and temperature reduction process, when the ambient temperature is 250-50 ℃, the temperature is reduced at the speed of 1 ℃/min.
2. The method of improving the mechanical properties of a liquid crystal polymer article of claim 1, wherein the liquid crystal polymer article is a liquid crystal polymer film.
3. The method for improving the mechanical properties of a liquid crystal polymer product according to claim 2, wherein the liquid crystal polymer film is covered with protective films on the top and bottom of the liquid crystal polymer film before the heat treatment.
4. The method of claim 1, wherein the liquid crystal polymer product is made of aromatic liquid crystal polymer resin.
5. The method of improving the mechanical properties of a liquid crystal polymer article of claim 1, wherein the protective atmosphere is a nitrogen atmosphere or an argon atmosphere.
6. The method of claim 1, wherein the heat treatment is carried out in a vacuum oven, a silicon-molybdenum sintering furnace, or an oil bath.
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| CN112351592A (en) * | 2020-11-24 | 2021-02-09 | 中国科学技术大学 | Method for preparing flexible circuit board based on liquid crystal polymer film |
| CN114133603A (en) * | 2021-12-14 | 2022-03-04 | 宁波长阳科技股份有限公司 | Method for improving mechanical property of liquid crystal polymer film and liquid crystal polymer film |
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