CN214324170U - Film blowing equipment for liquid crystal polymer film - Google Patents
Film blowing equipment for liquid crystal polymer film Download PDFInfo
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- CN214324170U CN214324170U CN202022767237.6U CN202022767237U CN214324170U CN 214324170 U CN214324170 U CN 214324170U CN 202022767237 U CN202022767237 U CN 202022767237U CN 214324170 U CN214324170 U CN 214324170U
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Abstract
A film blowing apparatus for a liquid crystal polymer film, the film blowing apparatus comprising an extruder; the co-extrusion die head is arranged at the tail end of the extruder and comprises a plurality of sub-runners and a co-extrusion runner, and the tail ends of the sub-runners are connected with the starting end of the co-extrusion runner; the number of the sub-runners is more than or equal to 5; the first air ring is connected with a mouth die of the co-extrusion die head; and a second wind ring disposed above the first wind ring. The utility model provides a forming method and blown film equipment of liquid crystal polymer film can be through adjusting inflation ratio, die head temperature, crowded layer combination altogether directly prepare anisotropic continuously adjustable's individual layer or multilayer liquid crystal polymer film, compares with prior art and has substantive characteristics and apparent technological progress.
Description
Technical Field
The utility model relates to a polymer film processing technology field especially relates to a blown film equipment of liquid crystal polymer film.
Background
With the gradual development of communication equipment and technology, the production and preparation of high-performance high-frequency substrate materials become an indispensable part for the development of high-frequency wireless communication. Most of traditional flexible circuit board base materials are polyimide films as insulating base materials of metal-clad plates, but the polyimide films are large in hygroscopicity and poor in high-frequency dielectric property, so that the requirements of the wireless communication industry on high-frequency and high-speed application are difficult to meet. The liquid crystal polymer film can replace the traditional material by virtue of unique properties such as extremely low dielectric constant and dielectric loss (the dielectric constant is about 3 in the frequency range of 1-60 GHz, the dielectric loss is less than 0.003), low hygroscopicity (< 0.04%), excellent dimensional stability and the like, and becomes a key film material in a high-frequency era.
In the prior art, a high-frequency flexible copper clad laminate is generally obtained by laminating and compounding a single-layer liquid crystal polymer film and a copper foil, and preferably, an I-type liquid crystal polymer film with a higher melting point is used as a core layer of a substrate, and a II-type liquid crystal polymer with a lower melting point is used as a bonding layer of the substrate. However, due to the intrinsic high heat resistance and rigid rod structure of liquid crystal polymers, single layer liquid crystal polymer films can generally only be obtained by rotary die blown film, biaxial stretching techniques, laminate stretching or coating methods. If a multilayer liquid crystal polymer substrate with more excellent performance is required to be prepared, different types of liquid crystal polymer films can be subjected to hot-pressing composite forming only through a laminating technology. In addition, the liquid crystal polymer is rapidly solidified when the melting point is lower than the melting point, the lamination phenomenon is easily generated in the thickness direction during the film processing, and the problems of low peeling strength between the single-layer liquid crystal polymer film and a copper foil and the like exist during the copper clad laminate processing.
SUMMERY OF THE UTILITY MODEL
In view of the above, one of the main objects of the present invention is to provide a liquid crystal polymer film blowing apparatus, which is intended to at least partially solve at least one of the above technical problems.
In order to achieve the above object, the present invention provides a liquid crystal polymer film blowing apparatus, comprising:
an extruder;
the co-extrusion die head is arranged at the tail end of the extruder and comprises a plurality of sub-runners and a co-extrusion runner, and the tail ends of the sub-runners are connected with the starting end of the co-extrusion runner; the number of the sub-runners is more than or equal to 5;
the first air ring is connected with a mouth die of the co-extrusion die head; and
and the second wind ring is arranged above the first wind ring.
Based on the above technical solution, the film blowing device for liquid crystal polymer film of the present invention has at least one or a part of the following advantages compared to the prior art:
1. the utility model discloses a homogeneity and continuity when guaranteeing the crowded material altogether that contains liquid crystal polymer and extruding from the bush solve the key of this problem, at first make the plastify effect of crowded material altogether and the homogeneity of fuse-element improve through setting up filtration in the die head, secondly set up suitable coextrusion runner length, realize the homogeneity of material in circumference distribution, solved the problem that inflation broke, the homogeneity is poor and the multilayer is compound difficult in the liquid crystal polymer film preparation process, through regulating and controlling crowded layer material altogether, can obtain different structure types, the accurate adjustable liquid crystal polymer film of anisotropy;
2. because the liquid crystal polymer can be rapidly solidified after being lower than the melting point, the first air ring is arranged at the transverse blowing stage to reduce the influence of cooling air flow on the liquid crystal polymer, the transverse blowing ratio of the film bubble is increased, the plasticity of the liquid crystal polymer is ensured, and when the difference between the crystallization temperature of the liquid crystal polymer material to be processed and the ambient temperature around the film bubble is more than 150 ℃, the temperature of the air flow at the stage is increased; in the film cooling and solidifying stage, the cooling process needs to be accurately adjusted according to the characteristics of materials, so that the defects of folds, deformation and the like of the film caused by rapid cooling are prevented;
3. the utility model provides a liquid crystal polymer film's forming method and blown film equipment can directly prepare anisotropic continuously adjustable individual layer or multilayer liquid crystal polymer film through adjusting inflation ratio, die head temperature, crowded layer combination altogether, has substantive characteristics and apparent technological progress compared with prior art;
4. the utility model provides a liquid crystal polymer film's forming method and blown film equipment, because five layers and the coextrusion technology more than five layers, the liquid crystal polymer layer that is located the intermediate level is under the protection of other coextrudes, its top layer can not cool down the solidification rapidly, the crystallization solidification is more controllable in the thickness direction, has obviously weakened the layering effect of film in the thickness direction, can set up the bond line on the film surface simultaneously, the processing preparation of specially adapted flexible copper-clad plate;
5. the utility model provides a forming method and blown film equipment of liquid crystal polymer film has advantages such as equipment manufacturing is simple, the energy consumption is low, can carry out multiple structure combination according to the user demand simultaneously, has comparatively extensive adaptability, has outstanding industrialization application potentiality.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of five-layer co-extrusion blown film processing provided by an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a multilayer co-extruded liquid crystal polymer composite film prepared according to an embodiment of the present invention.
Description of reference numerals:
1-co-extrusion die head; 2-heating a jacket; 3-7-flow channels; 8-co-extrusion flow channel; 9-the air inlet of the first wind ring; 10-a first wind ring lower disc; 11-first wind ring upper plate; 12-a first wind ring turbulence ring; 13-core air intake; 14-ring die; 15-bubble; 16-the air inlet of the second wind ring; 17-a second wind ring lower disc; 18-a second wind ring upper plate; 19-a second wind ring turbulence ring; 20-herringbone plates; 21-a drawing roll; 22-composite film.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings.
The utility model provides a problem that inflation broke, homogeneity is poor and the compound difficulty of multilayer in the liquid crystal polymer film preparation process, through regulation and control crowded layer material altogether, can obtain different structure types, the accurate adjustable liquid crystal polymer film of anisotropy. The utility model directly obtains single-layer or multi-layer liquid crystal polymer film by using multi-layer co-extrusion film blowing technology; the utility model can accurately regulate and control the anisotropy of the liquid crystal polymer film; the prepared liquid crystal polymer film has good uniformity and unobvious layering in the thickness direction; the utility model discloses the liquid crystal polymer film of preparation has apparent advantage when being compound with the copper foil lamination, preparation flexible copper-clad plate.
The utility model discloses a blown film equipment of liquid crystal polymer film, include:
an extruder;
the co-extrusion die head is arranged at the tail end of the extruder and comprises a plurality of sub-runners and a co-extrusion runner, and the tail ends of the sub-runners are connected with the starting end of the co-extrusion runner; the number of the sub-runners is more than or equal to 5;
the first air ring is connected with a mouth die of the co-extrusion die head; and
and the second wind ring is arranged above the first wind ring.
In some embodiments of the present invention, a filtering structure is disposed at the front end of each of the branch channels;
in some embodiments of the present invention, the ratio of the coextrusion runner to the die diameter is 0.5 to 50.
In some embodiments of the present invention, the co-extrusion die head further comprises a die core, wherein the die core is in a conical-to-cylindrical transition structure;
in some embodiments of the present invention, the film blowing apparatus further comprises a heating jacket for heating the co-extrusion die.
In some embodiments of the present invention, the first air ring is connected to a first temperature control unit for adjusting the temperature of the air flow of the first air ring;
in some embodiments of the present invention, the second air ring is connected to a second temperature control unit for adjusting the temperature of the second air ring airflow.
In some embodiments of the invention, the first wind ring comprises a first wind ring spoiler ring; the first wind ring turbulence ring is of an inverted round platform structure, and the inclination angle alpha of the round platform structure1≤30°；
In some embodiments of the invention, the second wind ring comprises a second wind ring spoiler ring; the second wind ring turbulence ring is of an inverted round platform structure, and the dip angle alpha of the round platform structure2≥45°。
The utility model also discloses a forming method of liquid crystal polymer film adopts as above blown film equipment, include:
setting technological parameters of an extruder;
conveying different materials to a coextrusion runner through different sub-runners respectively;
forming a film bubble by the material passing through the co-extrusion flow channel under the airflow of the mold core;
and drawing the film bubble to enable the film bubble to form the liquid crystal polymer film under the action of the air flow of the first air ring and the air flow of the second air ring.
In some embodiments of the present invention, the crystallization temperature T of the liquid crystal polymer material to be processedcAmbient temperature T of the bubbleaWhen the difference is more than 150 ℃, the temperature of the airflow of the first air ring is set to be Tc-100℃～Tc+30℃；
In some embodiments of the present invention, the temperature of the air flow of the second air ring is Tc-200℃～Tc-120℃；
In some embodiments of the present invention, the step of forming the bubble controls a blow-up ratio of 1.2 to 8.0;
in some embodiments of the present invention, the extrusion pressure of the extruder is set to 0.1 to 15.0 Mpa.
In some embodiments of the present invention, different materials are disposed in the plurality of sub-channels to obtain liquid crystal polymer films with different structures.
In some embodiments of the present invention, the plurality of runners includes at least a first runner, a second runner, a third runner, a fourth runner and a fifth runner, which are sequentially arranged; and liquid crystal polymer material is arranged in the third shunt passage.
In some embodiments of the present invention, the third shunting passage is filled with liquid crystal polymer material, and the other shunting passages are filled with non-liquid crystal polymer material; or,
the third sub-runner is internally made of liquid crystal polymer material, and at least one layer of the second sub-runner and the fourth sub-runner is made of adhesive material; or,
the third sub-runner is internally provided with a liquid crystal polymer material, at least one of the second sub-runner and the fourth sub-runner is provided with a liquid crystal polymer material, and the first sub-runner and the fifth sub-runner are internally provided with an adhesive material; or,
and liquid crystal polymer materials are arranged in the second sub-runner, the third sub-runner and the fourth sub-runner, and at least one of the first sub-runner and the fifth sub-runner is made of an adhesive material.
The utility model discloses a forming method and blown film equipment of liquid crystal polymer film utilizes the method of multilayer coextrusion, realizes the preparation of individual layer and multilayer liquid crystal polymer film, and blown film equipment includes five layers and five above crowded liquid crystal polymer blown film special die heads altogether and supporting shaping, cooling system.
The special die head for multilayer co-extrusion liquid crystal polymer blown film is characterized in that: the front end of the branch runner of the die head is provided with a filtering structure, and solid particles which are not fully plasticized can be filtered before the materials enter the coextrusion runner; the ratio of the length of the co-extrusion flow channel to the diameter of the neck ring mold is 0.5-50, so that the uniformity of the extruded tubular parison is ensured;
the structure of the forming and cooling system comprises a first air ring and a second air ring: multistage forming and cooling equipment, namely a first air ring and a second air ring, is arranged between the outlet of the neck mold and the traction roller, so that transverse blowing, cooling and solidification and the like of film bubbles are gradually realized, the first air ring and the second air ring are respectively provided with a stepless speed regulating fan, the flow speed and the air of air flow can be regulated and controlled, and the temperature of the air flow can be heated or cooled through temperature control equipment; the processing blow-up ratio is 1.2-8.0, more preferably 1.2-6.5, and with the increase of the blow-up ratio, the anisotropy of the film is gradually reduced, and the transverse physical property is gradually improved. The extrusion pressure of the extruder for processing the liquid crystal polymer-containing material is 0.1-15.0 MPa, more preferably 0.5-10.0 MPa, and as the viscosity of the liquid crystal polymer melt is lower, the reflux of the material can be reduced along with the improvement of the extrusion pressure, the extrusion stability of the material is improved, but when the extrusion pressure is too high, the material leakage of the device can be caused, and the processing life of the screw is influenced.
The preparation method of the multilayer co-extruded composite film containing the liquid crystal polymer material is realized by utilizing a multilayer co-extrusion method, wherein the five-layer co-extruded composite film is structurally characterized by IIIA/IIA/I/IIB/IIIB, the layer I is a liquid crystal polymer layer, the layers IIA and IIB are functional layers, and the layers IIIA and IIIB are protective layers; the single-layer liquid crystal polymer film can be obtained by directly stripping the layer I, when the layer IIA and the layer IIB are liquid crystal polymers, the multilayer co-extrusion liquid crystal polymer film can be obtained by stripping the layer IIIA and the layer IIIB, and when the layer IIA and the layer IIB are adhesives, the single-layer liquid crystal polymer film with an adhesive layer can be obtained by stripping the layer IIIA and the layer IIIB; the thickness of the single-layer liquid crystal polymer film is 5-200 mu m, and the thickness of the multi-layer liquid crystal polymer film is 8-500 mu m.
A multilayer co-extrusion composite film containing a liquid crystal polymer film takes five-layer co-extrusion as an example, and is structurally characterized in that III is formedA/IIA/I/IIB/IIIBIn which the layer I is a liquid crystal polymer layer, IIALayer, IIBLayer being a functional layer, IIIALayer IIIBThe layer is a protective layer, and the structural combination of the protective layer can be selected as follows:
a.I layers are liquid crystal polymer layers, and other layers are non-liquid crystal polymer layers, so that a single-layer liquid crystal polymer film can be obtained;
b.I layer is a liquid crystal polymer layer, functional layer IIALayer, IIBAt least one of the layers being of adhesive material, to obtain a beltA monolayer liquid crystalline polymer film of a layer;
c.I layer is a liquid crystal polymer layer, functional layer IIALayer, IIBAt least one layer of the layers is made of liquid crystal polymer material, and two layers or three layers of co-extruded liquid crystal polymer films can be obtained;
d.I layer is a liquid crystal polymer layer, functional layer IIALayer, IIBThe layers are all liquid crystal polymer materials, protective layer IIIALayer IIIBAt least one layer is adhesive material, so that the multilayer co-extruded liquid crystal polymer film with the adhesive layer can be obtained.
When the multilayer co-extruded liquid crystal polymer film is prepared, a layer I and a functional layer IIALayer, IIBThe liquid crystal polymer material of the layers can be the same liquid crystal polymer material or different liquid crystal polymer materials; when seven or more layers are co-extruded, IIIALayer IIIBOutside the layer is provided with IVALayer, IVBMore coextruded layers of layers and more types of structural combinations; the thickness of the single-layer liquid crystal polymer film is 5-200 mu m, and the thickness of the multi-layer liquid crystal polymer film is 8-500 mu m.
In the utility model, the liquid crystal polymer material is a liquid crystal copolyester material which can be processed by melt extrusion and has a melting point of 200-400 ℃; the liquid crystal polymer material may be a pure liquid crystal copolyester material or may comprise a blend of one or more liquid crystal copolyester materials.
Among these liquid crystal copolyesters, preferred are polymers containing at least 2-hydroxy-6-naphthoic acid and/or p-hydroxybenzoic acid as a repeating unit, and particularly preferred are (i) copolymers containing repeating units of 6-hydroxy-2-naphthoic acid and p-hydroxybenzoic acid, (ii) copolymers containing repeating units of at least one aromatic hydroxycarboxylic acid of 2-hydroxy-6-naphthoic acid and p-hydroxybenzoic acid, at least one aromatic diol of 4, 4' -dihydroxybiphenyl and hydroquinone, and at least one aromatic dicarboxylic acid of terephthalic acid, isophthalic acid and 2, 6-naphthalenedicarboxylic acid.
In the liquid crystal copolyester, thermoplastic resins such as fluorine-containing resin, polyphenylene sulfide, polyether ether ketone, polyamide, polyester amide, polyethylene terephthalate and modified resins thereof, polyolefin and the like can be added within the range not affecting the effect of the utility model; various additives such as slipping agents and antioxidants; fillers such as glass and ceramics.
In the utility model, the adhesive material is olefin copolymer or copolymer of olefin and unsaturated carboxylic acid or unsaturated carboxylic acid anhydride; the non-liquid crystal polymer material of the functional layer and the protective layer includes various materials that can be subjected to a film blowing process, such as polyethylene, polypropylene, polybutylene, ethylene/acrylic acid copolymer, ethylene/methacrylic acid copolymer, ethylene/vinyl acetate copolymer, ethylene/vinyl alcohol copolymer, polyvinyl chloride, polystyrene, poly (4-methylpentene), polyethylene terephthalate, nylon, polylactic acid, poly (adipic acid/butylene terephthalate), fluorine-containing resin, and the like; the non-liquid crystalline polymeric material may be one of the aforementioned resins or may be a blend comprising one or more of the aforementioned resins.
The utility model discloses in, carry out the preliminary treatment with the material in the vacuum drying oven before the extrusion moulding, preliminary treatment temperature and time are confirmed according to the nature of processing material.
Referring to fig. 1, a method for forming a liquid crystal polymer film and a film blowing apparatus according to an embodiment of the present invention utilize a multilayer coextrusion method to realize the preparation of single-layer and multilayer liquid crystal polymer films, and the film blowing apparatus includes a special die head for coextrusion of five or more layers of liquid crystal polymer films and a forming and cooling system; the method comprises the steps of respectively adding a liquid crystal polymer material and a protective layer material into an extruder, enabling the liquid crystal polymer material and the protective layer material to enter a co-extrusion die head 1 after being melted and plasticized by the extruder, enabling different processed materials to respectively enter flow channels 3-7 according to the structural combination of a multi-layer co-extrusion composite film, enabling the materials to firstly pass through a layer of filtering structure in each flow channel, filtering insufficiently melted solid particles, enabling the filtering structure to preferably pass through a high-precision filter screen, enabling the mesh number of the filter screen to preferably be 16-100 meshes, enabling filtered melt to finally converge into a co-extrusion flow channel 8, enabling the ratio of the length of the co-extrusion flow channel to the diameter of the die head to be 0.5-50, and adjusting the ratio to adjust the ratio to enable the functional high polymer material to share the same die headThe thickness distribution in the extrusion stage ensures the uniformity of the materials along the circumferential direction, the mold core adopts a structure of conical-to-cylindrical transition, the length of a co-extrusion flow channel is effectively increased under the condition that the height of the mold head is fixed, and the heating sleeve 2 ensures that the filtered processing materials are always in a molten state; the multilayer co-extrusion material is uniformly extruded from an annular neck mold 14, meanwhile, airflow enters a first air ring from an air inlet 9 of the first air ring, the airflow forms uniform and stable airflow through a turbulence channel formed by a first air ring lower plate 10 and a first air ring upper plate 11 and blows towards a film bubble 15, the air ring is connected with a stepless speed regulating fan, the flow speed and the air volume of the airflow can be regulated and controlled, and when the crystallization temperature T of the liquid crystal high polymer material to be processed is higher than the crystallization temperature T of the liquid crystal high polymer material to be processedcAnd the ambient temperature T around the bubbleaWhen the difference value is more than 150 ℃, the temperature of the airflow of the first air ring can be heated through a temperature control device to ensure that the liquid crystal polymer can not be cured immediately and still be in a tensile deformation state, the temperature control device, namely a first temperature control unit is connected between the air inlet 9 of the first air ring and the stepless speed regulating fan, the heating of the airflow generated by the fan is realized by controlling the heating power of a heating element in the first temperature control unit, and the temperature of the heated airflow is Tc-100℃～Tc+30 ℃, the deformability of the bubble is improved with the increase of the temperature of the air flow, but if the temperature is too high, the strength of the bubble is reduced, collapse occurs, and blowing is difficult to perform, the structure of the first air ring turbulent flow ring 12 enables the air flow to quickly disperse to the periphery of the bubble after blowing to the bubble 15, the upward air flow around the bubble 15 is weakened, the influence on transverse blowing is reduced while supporting the forming of the bubble, and the inclination angle alpha of the first air ring turbulent flow ring 12 is reduced1Less than or equal to 30 degrees; blowing air flow enters the film bubble 15 from the mold core air inlet hole 13 to transversely blow the film bubble 15, a traction roller 21 right above the mold head longitudinally pulls the film bubble 15, the film bubble 15 is pulled to a second air ring right above the first air ring, cooling air flow enters the second air ring from an air inlet 16 of the second air ring, the cooling air flows through a turbulent flow channel formed by a lower plate 17 of the second air ring and an upper plate 18 of the second air ring to form uniform and stable air flow to blow the film bubble 15, a second temperature control unit is arranged between an air inlet 16 of the second air ring and the stepless speed regulating fan, and heating elements in the second temperature control unit are controlledThe heating power realizes the control of the temperature of the air flow generated by the fan, and the temperature of the cooling air flow of the second air ring is Tc-200℃～TcAt-120 ℃, the cooling effect of the bubble is improved along with the reduction of the temperature of the airflow, but if the temperature is too low, the cooling among the multiple co-extrusion layers is uneven, and the defects of folds, layering and the like occur, the structure of the second air ring turbulence ring 19 enables the blown bubble to be gradually cooled, and the inclination angle alpha of the second air ring turbulence ring 192The temperature is more than or equal to 45 degrees, and the cooled and solidified film bubble enters a traction roller 21 through a herringbone plate 20, so that a multilayer co-extruded composite film 22 containing the liquid crystal polymer is obtained; the structure of the resulting multilayer coextruded composite film 22 is shown in FIG. 2.
The technical solution of the present invention is further explained by the following specific embodiments with reference to the attached drawings. It should be noted that the following specific examples are only illustrative, and the scope of the present invention is not limited thereto.
The chemicals and raw materials used in the following examples were either commercially available or self-prepared by a known preparation method.
The performance tests in the following examples are specified below:
peel strength
Preparing a peeling test piece with the width of 5mm by using the prepared liquid crystal polymer substrate, uncovering the bonding surface of the liquid crystal polymer film and the metal layer from the edge under the room temperature condition, fixing the liquid crystal polymer film layer on a flat plate by using a double-sided adhesive tape, peeling the metal layer in the 90-degree direction at the speed of 50mm/min, recording the peeling load by using a digital display pull gauge, wherein the peeling length is more than 50mm, and calculating the peeling strength according to the average value of the load in the peeling process.
Mechanical properties and thickness
The utility model discloses use the mechanical properties of universal tester test film, refer to GB/T1040.3-2006 method and test. The utility model discloses use mechanical contact formula calibrator test film thickness, test according to ASTM D645 method.
Example 1
By using the liquid crystal polymer film provided in the above embodimentA film forming method and a film blowing apparatus for preparing a monolayer liquid crystal polymer film of an adhesive layer. The structural combination of the multilayer co-extruded composite film is as follows: IIIA(polyethylene)/IIA(Binder)/I (liquid Crystal Polymer)/IIB(Binder)/IIIB(polyethylene); the liquid crystal polymer material is liquid crystal copolyester of p-hydroxybenzoic acid and 2-hydroxy-6-naphthoic acid, the melting point is 260 ℃, and the crystallization temperature T isc215 ℃, the adhesive material is ethylene/vinyl acetate copolymer, the melting point is 95 ℃, and the polyethylene is low-density polyethylene containing 1% of an opening agent, and the melting point is 112 ℃; before processing, the liquid crystal polymer material is subjected to drying pretreatment in a vacuum drying oven, wherein the drying temperature is 130 ℃, and the drying time is 5 hours. The liquid crystal polymer material, ethylene/vinyl acetate copolymer and polyethylene material after the pretreatment were added to the film blowing apparatus provided in the above example. The extrusion pressure range of an extruder in which the liquid crystal polymer is located is 0.6-3.0 MPa, air rings of a forming and cooling system are adjusted, the air outlet temperature of a first air ring is 245 ℃, the air outlet temperature of a second air ring is 50 ℃, and the bubble is stable when the inflation ratio is 5.0; finally, the polyethylene protective layer of the surface layer is peeled off to obtain the liquid crystal polymer film with the adhesive layers on two surfaces with the total thickness of about 60 mu m, the tensile strength of the film along the drawing direction is 235MPa, the elongation at break is 35%, the tensile strength perpendicular to the drawing direction is 210MPa, and the elongation at break is 33%, which shows that the obtained liquid crystal polymer film has excellent mechanical properties.
Example 2
The embodiment of the present invention is different from embodiment 1 in that the extrusion pressure range is 0.1 to 2.5MPa, the air-out temperature of the first air ring is 200 ℃, the air-out temperature of the second air ring is 50 ℃, the blow-up ratio of the film bubble is 1.2, and finally the liquid crystal polymer film with the adhesive layers on both sides and having a total thickness of about 90 μm is obtained, the tensile strength of the film along the pulling direction is 327MPa, the elongation at break is 21%, the tensile strength perpendicular to the pulling direction is 189MPa, and the elongation at break is 25%, which indicates that the obtained liquid crystal polymer film has excellent mechanical properties.
Example 3
The present example differs from example 1 in that the blow ratio of the bubble is 8, and the liquid crystal polymer film with adhesive layers on both sides of about 35 μm in total thickness is finally obtained, the tensile strength of the film along the drawing direction is 227MPa, the elongation at break is 36%, the tensile strength perpendicular to the drawing direction is 219MPa, and the elongation at break is 35%, indicating that the obtained liquid crystal polymer film has excellent mechanical properties.
Example 4
By using the method for forming a liquid crystal polymer film and the film blowing apparatus provided in the above embodiments, a multilayer liquid crystal polymer film is produced. The structural combination of the multilayer co-extruded composite film is as follows: IIIA(polyethylene)/IIA(polyethylene)/I (liquid Crystal Polymer)/IIB(polyethylene)/IIIB(polyethylene); the liquid crystal polymer material is liquid crystal copolyester of p-hydroxybenzoic acid and 2-hydroxy-6-naphthoic acid, the melting point is 280 ℃, and the crystallization temperature T iscThe temperature is 234 ℃, the polyethylene is low-density polyethylene containing 1% of a shedding agent, the air outlet temperature of the first air ring is 250 ℃, the air outlet temperature of the second air ring is 80 ℃, and the melting point is 112 ℃; before processing, the liquid crystal polymer material is subjected to drying pretreatment in a vacuum drying oven, wherein the drying temperature is 150 ℃ and the drying time is 5 hours. The liquid crystal polymer material and the polyethylene material after the pretreatment were added to the film blowing apparatus provided in the above example. The extrusion pressure range of an extruder in which the liquid crystal polymer is positioned is 0.5-5.0 MPa, and the air ring of a forming and cooling system is adjusted to ensure that the bubble is stable when the blow-up ratio is 4.5; and finally, peeling off the polyethylene protective layer on the surface layer to obtain a single-layer liquid crystal polymer film with the thickness of about 25 microns, and carrying out hot pressing on the obtained liquid crystal polymer film and a copper foil with the thickness of 18 microns for 3min under the conditions that the temperature is 285 ℃ and the pressure is 4MPa to prepare the copper-clad laminated board, wherein the bonding strength of the tested laminated board is 0.85N/mm.
Example 5
Utilize onThe liquid crystal polymer film is formed by a method of forming a liquid crystal polymer film and a film blowing apparatus. The structural combination of the multilayer co-extruded composite film is as follows: IIIA(polyethylene)/IIA(Low melting point liquid crystal polymer)/I (high melting point liquid crystal polymer)/IIB(Low melting liquid Crystal Polymer)/IIIB(polyethylene); the high-melting-point liquid crystal polymer material is liquid crystal copolyester of p-hydroxybenzoic acid, biphenol and terephthalic acid, the melting point is 320 ℃, and the crystallization temperature T isc1The low-melting-point liquid crystal polymer material is liquid crystal copolyester of p-hydroxybenzoic acid and 2-hydroxy-6-naphthoic acid, the melting point is 280 ℃, and the crystallization temperature T is 283 DEG Cc2At 234 ℃, the polyethylene is low-density polyethylene containing 1 percent of opening agent, and the melting point is 112 ℃; before processing, the liquid crystal polymer material is respectively dried and preprocessed in a vacuum drying oven, the drying temperature of the liquid crystal polymer with high melting point is 180 ℃, the drying temperature of the liquid crystal polymer with low melting point is 150 ℃, and the drying time is 5 hours. The liquid crystal polymer material and the polyethylene material after the pretreatment were added to the film blowing apparatus provided in the above example. The extrusion pressure range of an extruder in which the liquid crystal polymer is located is 6.0-10.0 MPa, air rings of a forming and cooling system are adjusted, the air outlet temperature of a first air ring is 290 ℃, the air outlet temperature of a second air ring is 100 ℃, and the bubble is stable when the inflation ratio is 3.0; and finally, peeling the polyethylene protective layer on the surface layer to obtain the three-layer co-extruded liquid crystal polymer film with the total thickness of about 80 mu m.
Example 6
The embodiment is different from the embodiment 5 in that the extrusion pressure range is 8.0-15.0 MPa, the air outlet temperature of the first air ring is 305 ℃, the air outlet temperature of the second air ring is 100 ℃, the blow-up ratio is 8.0, and the total thickness is about 55 μm.
Example 7
The embodiment of the invention is different from the embodiment 5 in that the extrusion pressure range is 0.5 to 5.0MPa, the blow-up ratio is 4.5, and the total thickness is about 70 μm. And hot-pressing the obtained liquid crystal polymer film and a copper foil with the thickness of 18 mu m for 3min at the temperature of 295 ℃ and under the pressure of 4MPa to prepare the copper-clad laminated board, wherein the bonding strength of the tested laminated board is 0.93N/mm.
Comparative example 1
The method for forming the liquid crystal polymer film and the film blowing equipment provided in the above specific embodiment are used for preparing the multilayer co-extruded liquid crystal polymer film, and the difference between the comparative example and the example 5 is that only the first air ring works, and the second air ring stops working; the method is characterized in that tiny wrinkles appear on the surface of a film bubble before the film bubble enters a traction roller in the film blowing processing process of the liquid crystal polymer film, although the blow-up ratio of the film bubble can still reach 3, the stability of the film bubble is poor, phenomena such as stretching resonance, vibration and the like easily occur, the wrinkles on the surface of the finally obtained liquid crystal polymer film are obvious, the obtained three-layer co-extruded liquid crystal polymer film is cut into a strip shape with the width of 5mm, the strip shape is placed in liquid nitrogen for 30s, then brittle fracture is carried out to obtain the section of the film, observation is carried out under the condition that the accelerating voltage is 2kV after surface metal spraying treatment, and remarkable layering appears in the thickness direction of the film.
Comparative example 2
The method for forming the liquid crystal polymer film and the film blowing equipment provided in the above specific embodiment are used for preparing the multilayer co-extruded liquid crystal polymer film, and the difference between the comparative example and the example 5 is that only the second air ring works, and the first air ring stops working; the multilayer polymer parison extruded from the die is rapidly cooled and solidified, the bubble is broken when the blow-up ratio reaches 1.2, the continuous transverse blow-up is difficult to carry out, and the bubble generates severe left and right swing when being longitudinally pulled.
It can be seen from comparative examples 1 and 2 that the first air ring mainly functions to improve the tensile deformation capability of the multi-layer polymer parison, and the air flow does not affect the transverse inflation while supporting the bubble at the transverse inflation stage, so that the bubble has excellent film blowing stability while achieving large inflation; the second air ring has the functions of realizing gradual and controllable cooling of the formed film bubble, preventing wrinkles generated by different forming shrinkage rates of different co-extrusion layer materials and weakening a layered skin-core structure generated by rapid solidification of a liquid crystal polymer; the liquid crystal polymer film with a specific blow-up ratio and excellent film performance can be obtained by the synergistic effect of the first air ring and the second air ring, and the anisotropy of the film can be controllably adjusted through the blow-up ratio, the traction ratio, the air flow temperature and the air flow quantity of the first air ring.
To sum up, the utility model provides a forming method and blown film equipment of liquid crystal polymer film can obtain the single-layer or multilayer liquid crystal polymer film that mechanical properties is excellent, anisotropy is low, can carry out controllable regulation to the anisotropy of liquid crystal polymer film according to different user demands simultaneously; the multilayer liquid crystal polymer film and the copper foil have high bonding strength during hot-pressing compounding, and have important significance for industrially preparing a high-frequency multilayer flexible copper-clad plate.
The details of the present invention not described in detail belong to the known technology in the art.
It should be noted that, although the invention has been shown and described with reference to the specific exemplary embodiments thereof, it should be understood by those skilled in the art that the invention is not limited to the above-mentioned embodiments, and that various changes and modifications may be made without departing from the spirit and scope of the invention, and it is intended to cover such changes and modifications also if they fall within the scope of the claims and their equivalents.
In particular, various combinations and/or combinations of features recited in the various embodiments and/or claims of the present invention can be made without departing from the spirit and teachings of the invention, even if such combinations or combinations are not expressly recited in the present invention. All such combinations and/or associations are within the scope of the present invention. The scope of the invention should, therefore, be determined not with reference to the appended claims, but should instead be determined with reference to the following claims, along with the full scope of equivalents to which such claims are entitled.
Claims (9)
1. An apparatus for blowing a liquid crystal polymer film, comprising:
an extruder;
the co-extrusion die head is arranged at the tail end of the extruder and comprises a plurality of sub-runners and a co-extrusion runner, and the tail ends of the sub-runners are connected with the starting end of the co-extrusion runner; the number of the sub-runners is more than or equal to 5;
the first air ring is connected with a mouth die of the co-extrusion die head; and
and the second wind ring is arranged above the first wind ring.
2. The film blowing apparatus according to claim 1,
and the front end of each sub-runner is provided with a filtering structure.
3. The film blowing apparatus according to claim 1,
the ratio of the diameter of the co-extrusion flow channel to the diameter of the neck mold is 0.5-50.
4. The film blowing apparatus according to claim 1,
the co-extrusion die head further comprises a die core, and the die core is in a conical-to-cylindrical transition structure.
5. The film blowing apparatus according to claim 1,
the film blowing equipment also comprises a heating sleeve for heating the co-extrusion die head.
6. The film blowing apparatus according to claim 1,
the first air ring is connected with a first temperature control unit for adjusting the air flow temperature of the first air ring.
7. The film blowing apparatus according to claim 1,
and the second air ring is connected with a second temperature control unit for adjusting the air flow temperature of the second air ring.
8. The film blowing apparatus according to claim 1,
the first wind ring comprises a first wind ring turbulent flow ring; the first wind ring turbulence ring is of an inverted round platform structure, and the inclination angle alpha of the round platform structure1≤30°。
9. The film blowing apparatus according to claim 1,
the second wind ring comprises a second wind ring turbulent flow ring; the second wind ring turbulence ring is of an inverted round platform structure, and the dip angle alpha of the round platform structure2≥45°。
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