CN106903909B - Ultrathin prepreg and preparation method thereof - Google Patents
Ultrathin prepreg and preparation method thereof Download PDFInfo
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- CN106903909B CN106903909B CN201710130226.7A CN201710130226A CN106903909B CN 106903909 B CN106903909 B CN 106903909B CN 201710130226 A CN201710130226 A CN 201710130226A CN 106903909 B CN106903909 B CN 106903909B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
- B29C70/504—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands
Abstract
The invention provides a preparation method of an ultrathin prepreg, which comprises the steps of fiber layer preparation, resin layer preparation, ultrathin prepreg preparation and the like. The invention also provides the ultrathin prepreg prepared by the preparation method, and the composite laminated board prepared by the ultrathin prepreg has good mechanical property.
Description
Technical Field
The invention relates to the field of prepregs, in particular to an ultrathin prepreg and a preparation method thereof.
Background
The preparation method of the laminated composite material is generally to prepare unidirectional or fabric fiber prepregs firstly and then stack the prepregs into the laminated composite material according to a certain laying mode and a certain laying angle. The performance of the laminated composite material and the structure thereof can be changed through the design of a layering mode and a layering angle, but the thickness of the conventional fiber prepreg is usually 0.125-0.25 mm, and when some composite material structures, particularly thin-wall composite material structures are designed, the allowable layering quantity is limited, so that the design space is greatly reduced, and the bearing requirement of the composite material structure in each direction is difficult to meet.
Therefore, the thin-layer process greatly expands the space and the degree of freedom when the composite material structure is designed, reduces the thickness of the unidirectional fiber prepreg, is convenient for increasing the number of layers of the paving layer under the specified structure thickness, and achieves the requirement of realizing the bearing of the structure in all directions by adopting different paving angles. In addition, the increase of the interlaminar interface enables the expansion of microcracks and delamination damage in the material to be effectively inhibited, the fiber microbending in the conventional prepreg paving layer is effectively eliminated, and various properties of the composite material are improved.
Ultra-thin prepregs generally mean that the areal density of the fibres is not more than 40g/m2And the thickness of the prepreg is not more than 0.04mm, the designability of the composite material in the laying direction can be enhanced, and the prepreg has important significance in the field of high-end composite materials. However, the preparation of the ultrathin prepreg is always the key and difficult point in the prepreg field, and the preparation thereof has the following technical problems: firstly, the ultrathin prepreg with larger size has more splicing seams, large appearance defects and low qualification rate; secondly, the fiber layer of the ultrathin prepreg is usually expanded by small tow fibers, so that the expansion rate is low, the production cost is high, and the production efficiency is low; thirdly, the preparation difficulty of the high-quality ultrathin prepreg is high, and the mechanical property of the composite material is low.
Disclosure of Invention
The present invention is directed to solving the problems described above. The invention aims to provide a preparation method of an ultrathin prepreg and the ultrathin prepreg prepared by the preparation method, wherein the preparation method comprises three steps of fiber layer preparation, resin layer preparation and ultrathin prepreg preparation, the process control of each step is studied, the ultrathin prepreg with high quality and large size can be prepared, the prepared prepreg has good appearance quality and low production cost, and the composite material prepared by the prepreg has good mechanical property.
The invention provides a preparation method of an ultrathin prepreg, which comprises the following steps:
1S fiber layer preparation: fixing N yarn drums on a creel, and finally widening fiber filaments contained in N spindle tows into a fiber layer with a preset width by sequentially passing the tows through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein N is an integer and is more than 2 and less than or equal to 25, and the preparation speed of the fiber layer is 5-7 m/min;
2S resin layer preparation: heating and melting resin, and uniformly coating the colloidal resin on release paper by using a glue coater to prepare a resin layer, wherein the coating temperature is controlled to be 60-90 ℃, and the coating speed is controlled to be 5-20 m/min;
3S preparation of ultrathin prepreg: and (3) respectively arranging the two groups of resin layers prepared in the step (2) above and below the fiber layer, and enabling the two resin layers to penetrate through the gap of a heating and pressing device to infiltrate into the fiber layer to prepare the ultrathin prepreg, wherein the rolling temperature is controlled to be 55-110 ℃, the gap of the heating and pressing device is controlled to be 5-75 mu m, and the preparation speed of the prepreg is controlled to be 4-7 m/min.
In the step 1S, the N-ingot filament bundle widening mode is merging widening, the yarn spreading device is an ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 30-315 MHz, and the medium in the ultrasonic groove comprises water.
In the step 2S, the gluing part of the gluing machine comprises a rubber wheel, a fixed wheel and an adjusting wheel, the coating temperature is controlled to be 70-80 ℃, the coating speed is controlled to be 10-15 m/min, the speed ratio of the fixed wheel is controlled to be 80-100%, and the speed ratio of the adjusting wheel is controlled to be 60-90%.
Wherein in the step 3S, the surface density of the resin layer is controlled to be 7.5-20 g/m2。
Wherein in the step 3S, the surface density of the resin layer is controlled to be 8.2-12.2 g/m2。
In the step 1S, the N-spindle tow widening mode is combined widening, the prepared fiber layer is laid on kraft paper for rolling, the yarn unwinding tension of the yarn drum is 8-15N, the unwinding tension of the kraft paper is 30-50N, and the winding tension of the fiber layer is 130-170N.
In the step 2S, the tension of the release paper is 200-300N, and the pressure of the rubber wheel is controlled to be 0.5-1 MPa.
In the step 3S, the heating and rolling device comprises four groups of heating and rolling equipment, the gap of the heating and rolling equipment is controlled to be 10-60 mu m, and the temperature of the four groups of heating and rolling equipment is sequentially controlled to be 80-100 ℃, 80-105 ℃ and 55-75 ℃.
In the step 3S, a first hot plate is further included between the first and second groups of heating and rolling devices, a second hot plate is further included between the second and third groups of heating and rolling devices, the temperature of the first hot plate is controlled to be 80-95 ℃, and the temperature of the second hot plate is controlled to be 80-95 ℃.
And after the resin layer and the fiber layer are heated and pressed, the resin layer and the fiber layer are cooled and stripped by a cooling plate to obtain the ultrathin prepreg, wherein the temperature of the cooling plate is controlled to be 10-20 ℃.
In the step 1S, the yarn spreading device is an ultrasonic yarn spreading device, the width of the prepared fiber layer is controlled to be 500mm, in the step 3S, the fiber layer is formed by splicing two groups of fiber layers prepared in the step 1S in parallel, and the width is controlled to be 1000 mm.
The invention also provides an ultrathin prepreg prepared by using the preparation method of the ultrathin prepreg, wherein the fiber layer is one of a carbon fiber layer, a glass fiber layer, an aramid fiber layer, a polyethylene fiber layer and a polyimide fiber layer;
the resin layer is one of an epoxy resin layer, a polyurethane resin layer, a cyanate resin layer and a polyimide resin layer;
and the mass of the fiber layer accounts for 45-70% of the total mass of the prepreg.
Wherein the fiber layer is made of carbon fiber tows with the mark number of T700SC-12K, M30 SC-18K.
The fiber layer is a carbon fiber layer, the resin layer is an epoxy resin layer, the width of the ultrathin prepreg is 1000mm, and the fiber surface density is 20-40 g/m2The density of the resin layer surface is 8.2-12.2 g/m2The thickness is 0.02-0.04 mm.
According to the preparation method of the ultrathin prepreg provided by the invention, the main innovation point is that the ultrathin prepreg with high quality and large size can be prepared by researching the process control of each step, the prepared prepreg has good appearance quality and low production cost, and the composite material prepared by using the prepreg has good mechanical property.
Specifically, the preparation method provided by the invention comprises three steps of fiber layer preparation, resin layer preparation and ultrathin prepreg preparation:
the preparation method of the fiber layer mainly comprises the steps of expanding and merging N spindle tows into the fiber layer with the preset width, specifically, N yarn drums are fixed on a creel, fiber filaments contained in each yarn drum pass through a yarn releasing device, a yarn unfolding device, a drying device and a winding device and are finally expanded into the fiber layer with the preset width, wherein N is an integer, N is more than 2 and less than or equal to 25, in the step, the preparation speed of the fiber layer is controlled to be 5-7 m/min, and the uniformity and the width of the fiber layer are effectively controlled while the production efficiency is guaranteed. In order to further reduce the appearance defects of the ultrathin prepreg and improve the mechanical property, the widening mode is preferably combined widening, namely the widening tows are combined simultaneously in the process of widening the N spindle tows, and the mode can reduce the gaps among different spindle widening yarns to the maximum extent and combine the widening of the N spindle tows into a uniform fiber layer.
Preferably, the yarn spreading device is an ultrasonic yarn spreading device. Further, in order to ensure the widening multiplying power and the combining effect of the fibers, the liquid medium in the ultrasonic groove is controlled to be mainly industrial-grade purified water, and the frequency of the ultrasonic generator is 30-315 MHz. Under the operating condition, the fiber bundle widening and thinning effect is better.
Furthermore, the fiber layer is laid on kraft paper for rolling, and the control of yarn unwinding tension of a yarn drum, the kraft paper unwinding tension and the fiber layer rolling tension and the matching of the frequency of an ultrasonic generator and an ultrasonic medium are the key points for widening and combining the multi-spindle fiber bundle.
The yarn spreading method commonly adopted in the prior art is a rolling method, an air flow method and an ultrasonic method, but the three methods are usually used for spreading fiber bundles and then directly collecting the fiber bundles, namely N spindle fiber bundles are spread and respectively collected to obtain N spindle spread fiber bundles, and the possibility that gaps exist in a fiber layer during subsequent process compounding is high, so that the appearance defects of an ultrathin prepreg product are more.
According to the invention, preferably, the yarn unwinding tension of the yarn bobbin is controlled to be 8-15N, the unwinding tension of kraft paper is controlled to be 30-50N, the winding tension of the fiber layer is controlled to be 130-170N, the N spindle fiber bundles can be combined while being widened through the matching of the parameters, the combination and the widening can be carried out simultaneously, and finally, the uniform fiber layer is prepared, so that the damage to the fiber bundles is effectively reduced, and the prepared fiber layer is flat and uniform in winding.
The preparation method of the resin layer comprises the steps of heating resin to be sol, and uniformly coating the sol on release paper to obtain the resin layer, wherein the release paper passes through a gap between the rubber wheel and the fixed wheel, and the fixed wheel coats the resin on the release paper in the movement process of the release paper. In the process, the coating temperature is controlled to be 60-90 ℃, the coating temperature has great influence on the quality of the resin layer, the viscosity of resin sol is easily reduced due to overhigh temperature, the resin quantity of the resin layer is influenced, the viscosity is easily increased due to overlow coating temperature, the uniformity of the resin layer is influenced, and preferably, the coating temperature is controlled to be 70-80 ℃. The coating speed is another key factor influencing the quality of the resin layer, the speed specifically refers to the running speed of the release paper, and the coating speed is controlled to be 5-20 m/min, preferably 10-15 m/min.
In order to better control the resin layer quality, the invention further studies the operating parameters of the fixed wheel and the regulating wheel, in particular the ratio of the running speed of each wheel to the coating speed. The ratio of the fixed wheel speed to the coating speed is defined as a fixed wheel speed ratio, which is controlled to be 80 to 100%, and similarly the ratio of the adjustable wheel speed to the coating speed is controlled to be 60 to 90%, which parameters are controlled to maintain the stability of the resin content and the resin layer density.
Preferably, the surface density of the resin layer is controlled to be 7.5 to 20g/m2The resin layer with the surface density can be effectively infiltrated with the fiber layer, and the prepared ultrathin prepreg is thin, low in resin content and better in mechanical property. More preferably, the surface density of the resin layer is controlled to be 8.2 to 12.2g/m2。
Furthermore, the tension of the release paper is controlled to be 200-300N, and the pressure of the rubber wheel is controlled to be 0.5-1 Mpa. The tension control of the release paper influences the stable operation of the release paper, and further influences the uniformity of the resin layer; the surface density and the integral uniformity of the resin layer are further ensured by controlling the pressure of the rubber wheel, and the quality of the resin layer can be further improved by controlling the parameters.
The preparation method of the ultrathin prepreg mainly comprises the steps of infiltrating two resin layers into a fiber layer to form the ultrathin prepreg, and heating and rolling a blank formed by the resin layers and the fiber layer in the process to finally prepare the prepreg with uniformly distributed fibers. Specifically, the heating and pressing device includes corresponding rolling devices up and down, and the gap between the corresponding devices in the direction perpendicular to the movement direction of the prepreg is adjustable, and the temperature and pressure are applied to the prepreg while the prepreg passes through the gap to produce the prepreg.
The temperature in the preparation process is controlled to be 55-110 ℃, the gap of a heating and pressing device is controlled to be 5-75 mu m, the preparation speed of the prepreg is controlled to be 4-7 m/min, the resin layer can be better soaked into the fiber layer under the process parameters, and the thickness of the prepreg is effectively controlled.
Preferably, the heating and rolling device specifically comprises four groups of heating and rolling devices, and the gap between the four groups of heating and rolling devices is controlled to be 10-60 μm. Preferably, the temperatures of the four groups of heating and rolling equipment are sequentially controlled to be 80-100 ℃, 80-105 ℃ and 55-75 ℃, and the design ensures that the blanks are subjected to multiple heating and rolling processes, so that the uniform distribution of resin and cellosilk in the blanks is promoted, the thickness of the prepregs is further reduced, particularly, the temperature of the blanks is reduced to a certain extent when the blanks pass through the fourth group of heating and rolling equipment, and the subsequent cooling and stripping operation of the prepregs is facilitated. The quality of the ultrathin prepreg and the mechanical property of the prepared laminated board are effectively improved by the cooperation of the four groups of heating and rolling equipment.
More preferably, a first hot plate is further arranged between the first group of heating and rolling equipment and a second hot plate is further arranged between the second group of heating and rolling equipment and the third group of heating and rolling equipment, the hot plates heat the prepreg but do not apply pressure, the temperature of the first hot plate is controlled to be 80-95 ℃, the temperature of the second hot plate is controlled to be 80-95 ℃, the fluidity of resin is further promoted, the quality of the prepreg is improved, and particularly, when the prepreg passes through the first three groups of heating and rolling equipment, the prepreg is subjected to the processes of heating and rolling by the hot plates, so that the resin and the fiber yarns are uniformly distributed, and the performance of the ultrathin prepreg is.
And after the blank passes through the heating roller device, the blank also passes through the cooling plate, the temperature is reduced, and the release paper on the upper resin layer is peeled off, wherein the temperature is controlled to be 10-20 ℃, and the control process further increases the beneficial effects.
Widening and thinning the fiber layer into a uniform whole and preparing the resin layer are difficult points of producing the ultrathin prepreg, and therefore, the preparation process of the fiber layer and the resin layer needs to be strictly controlled in quality. The preparation method provided by the invention can be used for preparing ultrathin prepreg with larger size and has no splicing seam.
Specifically, the width of the fiber layer obtained after merging and widening in the step 1S is controlled to be 500mm, two rolls of fiber layers are spliced in parallel in the process of preparing the ultrathin prepreg, and then the width of the prepreg is controlled to be 1000mm, only one splicing seam is theoretically generated in the process, but the splicing seam can be controlled to be invisible to naked eyes in the process of preparing the prepreg.
On the other hand, the quality needs to be strictly controlled in the preparation process of the resin layer. Furthermore, after the resin layer is prepared by following the preparation method of the resin layer, 5 samples are taken from the layer to measure the surface density, and whether the uniformity and the surface density of the resin layer reach the standard or not is evaluated. And controlling the surface density of the resin layer to be 8.2-12.2 g/m2。
The resin layer with the use quality meeting the standard can be better infiltrated with the fiber layer with the width of 1000mm, and the operation mode only needs two rolls of fiber layers in the preparation process of the prepreg, the width of the prepreg can reach 1000mm, fiber spindles do not need to be frequently replaced, theoretically, only one splicing seam exists, the splicing seam is invisible to naked eyes after the prepreg preparation step is carried out, the ultrathin prepreg with good appearance quality and performance is prepared, the production efficiency of the ultrathin prepreg is effectively improved, and the cost is reduced.
As a preferred example of the present invention, the method for preparing the ultra-thin prepreg includes the steps of:
1S fiber layer preparation: fixing N yarn drums on a creel, enabling tows to sequentially pass through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn drums is 8-15N, finally combining and spreading fiber yarns contained in N spindle tows into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding, wherein N is an integer and is more than 2 and less than or equal to 25;
the yarn spreading device is an ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 30-315 MHz, a medium in an ultrasonic groove comprises water, the unreeling tension of kraft paper is 30-50N, the reeling tension of a fiber layer is 130-170N, and the preparation speed of the fiber layer is 5-7 m/min;
2S resin layer preparation: heating and melting resin, and uniformly coating the colloidal resin on release paper by using a glue spreader to obtain a resin layer, wherein the coating temperature is controlled to be 70-80 ℃, the coating speed is controlled to be 10-15 m/min, the fixed wheel speed ratio is controlled to be 80-100%, the adjusting wheel speed ratio is controlled to be 60-90%, the tension of the release paper is 200-300N, and the pressure of a rubber wheel is controlled to be 0.5-1 MPa;
3S preparation of ultrathin prepreg: two groups of resin layers prepared in the step 2S are respectively arranged above and below the fiber layer, wherein the two groups of resin layers penetrate through the gap of a heating and pressing device to enable the two resin layers to be soaked into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 7.5-20 g/m2；
Wherein the rolling temperature is controlled to be 55-110 ℃, the gap of a heating and pressing device is controlled to be 5-75 mu m, and the preparation speed of the prepreg is controlled to be 4-7 m/min.
As a preferred example of the present invention, the method for preparing the ultra-thin prepreg includes the steps of:
1S fiber layer preparation: fixing N yarn drums on a creel, enabling tows to sequentially pass through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn drums is 8-15N, finally combining and spreading fiber yarns contained in N spindle tows into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding, wherein N is an integer and is more than 2 and less than or equal to 25;
the yarn spreading device is an ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 30-315 MHz, a medium in an ultrasonic groove comprises water, the unreeling tension of kraft paper is 30-50N, the reeling tension of a fiber layer is 130-170N, and the preparation speed of the fiber layer is 5-7 m/min;
2S resin layer preparation: heating and melting resin, and uniformly coating the colloidal resin on release paper by using a glue spreader to obtain a resin layer, wherein the coating temperature is controlled to be 70-80 ℃, the coating speed is controlled to be 10-15 m/min, the fixed wheel speed ratio is controlled to be 80-100%, the adjusting wheel speed ratio is controlled to be 60-90%, the tension of the release paper is 200-300N, and the pressure of a rubber wheel is controlled to be 0.5-1 MPa;
3S preparation of ultrathin prepreg: two groups of resin layers prepared in the step 2S are respectively arranged above and below the fiber layer, wherein the two groups of resin layers penetrate through the gap of a heating and pressing device to enable the two resin layers to be soaked into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 8.2-12.2 g/m2；
The heating and rolling device comprises four groups of heating and rolling devices, a first hot plate is arranged between the first group of heating and rolling devices, a second hot plate is arranged between the second group of heating and rolling devices and the third group of heating and rolling devices, the temperatures of the heating and rolling devices and the hot plates are sequentially controlled to be 80-100 ℃, 80-105 ℃ and 55-75 ℃, the temperature of the first hot plate is controlled to be 80-95 ℃, the temperature of the second hot plate is controlled to be 80-95 ℃, the gap of the heating and rolling devices is controlled to be 10-60 mu m, the resin layer and the fiber layer pass through a heating roller after being pressed, and then are cooled and stripped by release paper to prepare the ultrathin prepreg, wherein the temperature of the cooling plate is controlled to be 10-20 ℃, and the preparation speed of the prepreg is controlled to be 4-7 m/min.
According to another aspect of the present invention, there is provided an ultra-thin prepreg manufactured using the above manufacturing method. Specifically, the fiber layer is one of a carbon fiber layer, a glass fiber layer, an aramid fiber layer, a polyethylene fiber layer and a polyimide fiber layer;
the resin layer is one of an epoxy resin layer, a polyurethane resin layer, a cyanate resin layer and a polyimide resin layer; the weight of the fiber layer is controlled to be 45-70% of the total weight of the prepreg, and the high fiber content can effectively increase the tensile strength of the material after the composite material is prepared.
Furthermore, the preparation method provided by the invention is very suitable for preparing carbon fiber prepregs, and is particularly suitable for carbon fiber tows of large tows with the brands of T700SC-12K and M30 SC-18K. Because the price of the small tows is higher, the cost can be reduced by using the large-tow carbon fiber as a raw material to prepare the ultrathin prepreg, and the mechanical properties of the ultrathin prepreg and the laminated plate can be further improved. More preferably, the resin layer of the prepreg is an epoxy resin layer.
Particularly, the invention claims a large-size ultrathin prepreg prepared by the preparation method, the width of the prepreg is 1000mm, and the fiber surface density is 20-40 g/m2The density of the resin layer surface is 8.2-12.2 g/m2The thickness is 0.02-0.04 mm.
The invention researches the process control of each step, and compared with the prior art, the invention has the following beneficial effects:
firstly, the invention has more control parameters, the quality control of the fiber layer, the resin layer and the prepreg in the preparation process is stable, and the technical problem of high difficulty in preparing high-quality ultrathin prepreg is effectively solved.
Secondly, the ultrathin prepreg prepared by the invention can realize the preparation of the ultrathin prepreg with larger size, effectively reduces the appearance defects, and has good quality and high qualification rate.
Thirdly, the preparation of the ultrathin prepreg can be carried out by using the large tow fiber bundle, so that the mechanical property of the laminated plate prepared from the prepreg is effectively improved, the production efficiency is effectively improved, and the production cost is greatly reduced.
The method for preparing the ultrathin prepreg and the beneficial effects of the ultrathin prepreg provided by the invention are illustrated by specific experimental data given by examples.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention, in which like reference numerals are used to designate like elements, and the drawings in the following description are some, but not all embodiments of the invention, and will enable one of ordinary skill in the art to make and use the invention.
Fig. 1 shows a flow chart for preparing an ultra-thin prepreg according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
Example 1
1S fiber layer preparation: fixing a 25-spindle carbon fiber bobbin with the trademark of T700SC-12K on a creel, sequentially passing tows through a yarn releasing device, a yarn spreading device, a drying device and a winding device, and finally spreading the fibers contained in the 25-spindle tows to form a fiber layer with the width of 500mm, wherein the preparation speed of the fiber layer is 5 m/min;
2S resin layer preparation: after adding hot melt adhesive into epoxy resin, uniformly coating the colloidal resin on release paper by using a glue coater to prepare a resin layer, wherein the coating temperature is controlled to be 70 ℃, and the coating speed is controlled to be 10 m/min;
3S preparation of ultrathin prepreg: and (3) respectively arranging the two groups of resin layers prepared in the step (2) above and below the fiber layer, and penetrating the resin layers through the gap of a heating and pressing device to infiltrate the two resin layers into the fiber layer to prepare the ultrathin prepreg, wherein the rolling temperature is controlled to be 80 ℃, the gap of the heating and pressing device is controlled to be about 60 mu m, and the preparation speed of the prepreg is controlled to be 4 m/min.
The width of the prepared ultrathin prepreg is 1000mm, and the fiber surface density is 40g/m2The thickness is 0.04 mm.
Example 2
1S fiber layer preparation: fixing a 19-spindle carbon fiber yarn bobbin with the brand number of T700SC-12K on a creel, and sequentially passing the yarn bundle through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn bobbin is 8N, finally merging and spreading the fiber yarns contained in the 19-spindle yarn bundle into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding;
in the ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 100MHz, the medium in an ultrasonic groove is industrial-grade purified water, the unreeling tension of kraft paper is 30N, the reeling tension of a fiber layer is 130N, and the preparation speed of the fiber layer is 6 m/min;
2S resin layer preparation: after adding hot melt adhesive into epoxy resin, uniformly coating colloidal resin on release paper by using a glue spreader to prepare a resin layer, wherein the coating temperature is controlled to be 70 ℃, the coating speed is controlled to be 15m/min, the speed ratio of a fixed wheel is controlled to be 80%, the speed ratio of an adjusting wheel is controlled to be 60%, the tension of the release paper is 200N, and the pressure of a glue wheel is controlled to be 0.5 MPa;
3S preparation of ultrathin prepreg: arranging two groups of resin layers prepared in the step 2S above and below the fiber layer respectively, wherein the two groups of resin layers penetrate through a gap of a heating and pressing device to be infiltrated into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 10g/m2；
Wherein the rolling temperature is controlled to be 90 ℃, the gap of a heating and pressing device is controlled to be about 50 mu m, and the preparation speed of the prepreg is controlled to be 7 m/min.
The width of the prepared ultrathin prepreg is 1000mm, and the fiber surface density is 30g/m2The thickness is 0.03 mm.
Example 3
1S fiber layer preparation: fixing 14-spindle carbon fiber yarn bobbins with the brand number of T700SC-12K on a creel, and sequentially passing tows through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn bobbins is 15N, finally merging and spreading the fiber yarns contained in the 14-spindle tows into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding;
in the ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 100MHz, the medium in an ultrasonic groove is industrial-grade purified water, the unreeling tension of kraft paper is 30N, the reeling tension of a fiber layer is 150N, and the preparation speed of the fiber layer is 7 m/min;
2S resin layer preparation: after adding hot melt adhesive into epoxy resin, uniformly coating the colloidal resin on release paper by using a glue spreader to prepare a resin layer, wherein the coating temperature is controlled to be 75 ℃, the coating speed is controlled to be 12m/min, the fixed wheel speed ratio is controlled to be 95%, the wheel speed ratio is adjusted to be 74%, the tension of the release paper is 260N, and the pressure of a rubber wheel is controlled to be 0.75 MPa;
3S preparation of ultrathin prepreg: arranging two groups of resin layers prepared in the step 2S above and below the fiber layer respectively, wherein the two groups of resin layers penetrate through a gap of a heating and pressing device to be infiltrated into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 12.2g/m2；
The heating and rolling device comprises four groups of heating and rolling devices, a first hot plate is arranged between the first group of heating and rolling devices, a second hot plate is arranged between the second group of heating and rolling devices and the third group of heating and rolling devices, the temperatures of the heating and rolling devices are sequentially controlled to be 80 ℃, 100 ℃, 95 ℃ and 72 ℃, the temperatures of the first hot plate and the second hot plate are both 95 ℃, the gap of the heating and rolling devices is controlled to be about 45 mu m, the resin layer and the fiber layer are cooled and stripped of upper release paper through a cooling plate after being subjected to heating and rolling devices, and the ultrathin prepreg is prepared, wherein the temperature of the cooling roller is controlled to be 20 ℃, and the preparation speed of the prepreg is controlled to be 5 m/min.
The width of the prepared ultrathin prepreg is 1000mm, and the fiber surface density is 22.4g/m2The thickness is 0.022 mm.
Example 4
1S fiber layer preparation: fixing a 15-spindle carbon fiber yarn bobbin with the trademark of T700SC-12K on a creel, and sequentially passing the tows through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn bobbin is 10N, finally merging and spreading the fibers contained in the 15-spindle tow into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding;
in the ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 200MHz, the medium in an ultrasonic groove is industrial-grade purified water, the unreeling tension of kraft paper is 50N, the reeling tension of a fiber layer is 170N, and the preparation speed of the fiber layer is 5 m/min;
2S resin layer preparation: after adding hot melt adhesive into epoxy resin, uniformly coating colloidal resin on release paper by using a glue spreader to prepare a resin layer, wherein the coating temperature is controlled to be 72 ℃, the coating speed is controlled to be 10m/min, the speed ratio of a fixed wheel is controlled to be 90%, the speed ratio of an adjusting wheel is controlled to be 72%, the tension of the release paper is 240N, and the pressure of a rubber wheel is controlled to be 0.72 MPa;
3S preparation of ultrathin prepreg: arranging two groups of resin layers prepared in the step 2S above and below the fiber layer respectively, wherein the two groups of resin layers penetrate through a gap of a heating and pressing device to be infiltrated into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 9.8g/m2；
The heating and rolling device comprises four groups of heating and rolling devices, a first hot plate is arranged between the first group of heating and rolling devices, a second hot plate is arranged between the second group of heating and rolling devices and the third group of heating and rolling devices, the temperatures of the heating and rolling devices are sequentially controlled to be 90 ℃, 105 ℃, 80 ℃ and 60 ℃, the temperatures of the first hot plate and the second hot plate are both 90 ℃, the gap of the heating and rolling devices is controlled to be about 48 mu m, the resin layer and the fiber layer are cooled and stripped of upper release paper through a cooling plate after being subjected to heating and rolling, and the ultrathin prepreg is prepared, wherein the temperature of the cooling roller is controlled to be 15 ℃, and the preparation speed of the prepreg is controlled to be 6 m/min.
The width of the prepared ultrathin prepreg is 1000mm, and the fiber surface density is 24g/m2The thickness is 0.024 mm.
Example 5
1S fiber layer preparation: fixing a 13-spindle carbon fiber yarn bobbin with the trademark of T700SC-12K on a creel, and sequentially passing the yarn bundle through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein the yarn releasing tension of the yarn bobbin is 12N, finally merging and spreading the fiber yarns contained in the 13-spindle yarn bundle into a fiber layer with the width of 500mm, and laying the fiber layer on kraft paper for winding;
in the ultrasonic yarn spreading device, the frequency of an ultrasonic generator is 200MHz, the medium in an ultrasonic groove is industrial-grade purified water, the unreeling tension of kraft paper is 45N, the reeling tension of a fiber layer is 155N, and the preparation speed of the fiber layer is 5.5 m/min;
2S resin layer preparation: after adding hot melt adhesive into epoxy resin, uniformly coating the colloidal resin on release paper by using a glue spreader to prepare a resin layer, wherein the coating temperature is controlled to be 80 ℃, the coating speed is controlled to be 15m/min, the speed ratio of a fixed wheel is controlled to be 100%, the speed ratio of an adjusting wheel is controlled to be 90%, the tension of the release paper is 300N, and the pressure of a glue wheel is controlled to be 0.7 MPa;
3S preparation of ultrathin prepreg: arranging two groups of resin layers prepared in the step 2S above and below the fiber layer respectively, wherein the two groups of resin layers penetrate through a gap of a heating and pressing device to be infiltrated into the fiber layer to prepare the ultrathin prepreg, the fiber layer is formed by splicing the two groups of fiber layers prepared in the step 1S in parallel, the width is controlled to be 1000mm, and the areal density of the resin layers is controlled to be 8.2g/m2；
The heating and rolling device comprises four groups of heating and rolling devices, a first hot plate is arranged between the first group of heating and rolling devices, a second hot plate is arranged between the second group of heating and rolling devices and the third group of heating and rolling devices, the temperatures of the heating and rolling devices are sequentially controlled to be 100 ℃, 80 ℃, 105 ℃ and 65 ℃, the temperatures of the first hot plate and the second hot plate are both 85 ℃, the gap of the heating and rolling devices is controlled to be about 30 mu m, the resin layer and the fiber layer are cooled and stripped of upper release paper through a cooling plate after being subjected to heating and rolling, and the ultrathin prepreg is prepared, wherein the temperature of the cooling roller is controlled to be 10 ℃, and the preparation speed of the prepreg is controlled to be 5 m/min.
The width of the prepared ultrathin prepreg is 1000mm, and the fiber surface density is 20g/m2The thickness is 0.02 mm.
Comparative example
To further illustrate the beneficial effects of the present invention, an ultra-thin prepreg of 1000mm width produced by the prior art was selected as a comparative example, whichThe fiber surface density is 20g/m2And the thickness of the ultra-thin prepreg is 0.02mm, and the ultra-thin prepreg is produced by adopting a T300-3k carbon fiber tow and epoxy resin.
Test example
The ultra-thin prepregs of examples 1-5 and comparative examples were applied to the preparation of laminates, and the final composite products were subjected to performance tests, respectively, with the following results:
TABLE 1 Performance test results for ultra-thin prepreg composite articles of different specifications
| Testing performance | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Tensile Strength (MPa) | 2037 | 2135 | 2241 | 2210 | 2245 | 1545 |
| Compressive Strength (MPa) | 874 | 897 | 1015 | 1007 | 1020 | 807 |
| Flexural Strength (MPa) | 1231 | 1403 | 1431 | 1421 | 1444 | 1228 |
| Interlaminar shear strength (MPa) | 78 | 79 | 88 | 89 | 88 | 74 |
As can be seen from the above test examples, the mechanical properties of examples 1-5 are much higher than those of comparative examples, specifically, the average tensile strength of examples 1-5 is 2173.6MPa, which is 40.7% higher than that of 1545MPa of comparative examples; the average compressive strength is 962.6MPa, which is improved by 19.3 percent compared with 807MPa of a comparative example; the average bending strength is 1386MPa, which is improved by 12.9 percent compared with 1228MPa of a comparative example; the average interlaminar shear strength was 84.4MPa, an increase of 14.1% over the comparative example of 74 MPa. The ultra-thin prepreg provided by the invention has better performance, and the prepared laminated plate has excellent performance.
In summary, the invention has the following beneficial effects:
firstly, the invention has more control parameters, the quality control of the fiber layer, the resin layer and the prepreg in the preparation process is stable, and the technical problem of high difficulty in preparing high-quality ultrathin prepreg is effectively solved.
Secondly, the ultrathin prepreg prepared by the invention can realize the preparation of the ultrathin prepreg with larger size, effectively reduces the appearance defects, and has good quality and high qualification rate.
Thirdly, the preparation of the ultrathin prepreg can be carried out by using the large tow fiber bundle, so that the mechanical property of the laminated plate prepared from the prepreg is effectively improved, the production efficiency is effectively improved, and the production cost is greatly reduced.
Finally, it should be noted that: in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A preparation method of an ultrathin prepreg is characterized by comprising the following steps:
1S fiber layer preparation: fixing N yarn drums on a creel, and finally widening fiber filaments contained in N spindle tows into a fiber layer with a preset width by sequentially passing the tows through a yarn releasing device, a yarn spreading device, a drying device and a winding device, wherein N is an integer and is more than 2 and less than or equal to 25, and the preparation speed of the fiber layer is 5-7 m/min;
2S resin layer preparation: heating and melting resin, and uniformly coating the colloidal resin on release paper by using a glue coater to prepare a resin layer, wherein the coating temperature is controlled to be 70-80 ℃, and the coating speed is controlled to be 10-15 m/min; the surface density of the resin layer is controlled to be 7.5-20 g/m2；
3S preparation of ultrathin prepreg: arranging two groups of resin layers prepared in the step 2S above and below the fiber layer respectively, and enabling the two resin layers to penetrate through the gap of a heating and pressing device to infiltrate into the fiber layer to prepare the ultrathin prepreg, wherein the rolling temperature is controlled to be 55-110 ℃, the gap of the heating and pressing device is controlled to be 5-75 mu m, and the preparation speed of the prepreg is controlled to be 4-7 m/min;
in the step 1S, the N-ingot tow widening mode is combined widening, the prepared fiber layer is laid on kraft paper for rolling, the yarn unwinding tension of the yarn drum is 8-15N, the unwinding tension of the kraft paper is 30-50N, and the winding tension of the fiber layer is 130-170N;
the yarn spreading device is an ultrasonic yarn spreading device, wherein the frequency of an ultrasonic generator is 30-315 MHz, and a medium in an ultrasonic groove comprises water;
in the step 2S, the gluing part of the gluing machine comprises a rubber wheel, a fixed wheel and an adjusting wheel, the speed ratio of the fixed wheel is controlled to be 80-100%, and the speed ratio of the adjusting wheel is controlled to be 60-90%; wherein, the fixed wheel speed ratio refers to the ratio of the fixed wheel speed to the coating speed, and the adjusting wheel speed ratio refers to the ratio of the adjusting wheel speed to the coating speed;
the tension of the release paper is 200-300N, and the pressure of the rubber wheel is controlled to be 0.5-1 MPa;
in the step 3S, the heating and rolling device comprises four groups of heating and rolling equipment, the gap of the heating and rolling equipment is controlled to be 10-60 mu m, and the temperature of the four groups of heating and rolling equipment is sequentially controlled to be 80-100 ℃, 80-105 ℃ and 55-75 ℃;
a first hot plate is arranged between the first group of heating rolling equipment and the second group of heating rolling equipment, a second hot plate is arranged between the second group of heating rolling equipment and the third group of heating rolling equipment, the temperature of the first hot plate is controlled to be 80-95 ℃, and the temperature of the second hot plate is controlled to be 80-95 ℃;
after the resin layer and the fiber layer are pressed by a heating roller, the resin layer and the fiber layer are cooled by a cooling plate, and the upper delamination type paper is peeled off to prepare the ultrathin prepreg, wherein the temperature of the cooling plate is controlled to be 10-20 ℃;
in the step 3S, the fiber layers are formed by splicing two groups of fiber layers prepared in the step 1S in parallel, and the width of the ultrathin prepreg is 2 times that of the fiber layers prepared in the step 1S.
2. A method for preparing an ultra-thin prepreg according to claim 1, wherein in the step 1S, the width of the fiber layer is 500 m;
in the step 3S, the fiber layers are formed by splicing two groups of fiber layers prepared in the step 1S in parallel, and the width of the ultrathin prepreg is 1000 m.
3. An ultra-thin prepreg produced using the method for producing an ultra-thin prepreg according to claim 1 or 2,
the fiber layer is one of a carbon fiber layer, a glass fiber layer, an aramid fiber layer, a polyethylene fiber layer and a polyimide fiber layer;
the resin layer is one of an epoxy resin layer, a polyurethane resin layer, a cyanate resin layer and a polyimide resin layer; and the mass of the fiber layer accounts for 45-70% of the total mass of the prepreg.
4. The ultra-thin prepreg of claim 3, wherein the fiber layer is made of carbon fiber tow having a designation T700SC-12K, M30 SC-18K.
5. The ultra-thin prepreg of claim 3, wherein the fiber layer is a carbon fiber layer and the resin layer is a ringThe width of the ultrathin prepreg is 1000mm, and the fiber surface density is 20-40 g/m2The density of the resin layer surface is 8.2-12.2 g/m2The thickness is 0.02-0.04 mm.
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| CN105038142A (en) * | 2015-06-30 | 2015-11-11 | 航天材料及工艺研究所 | Preparing method of hot-melt prepreg of novolac epoxy resin |
| CN105150404A (en) * | 2015-07-15 | 2015-12-16 | 北京昂林贸烽科技有限公司 | Method for processing carbon fiber tow |
| CN105904611A (en) * | 2016-04-14 | 2016-08-31 | 北京航空航天大学 | Ultrathin continuous fiber reinforced thermoplastic resin prepreg and preparation method thereof |
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| CN105038142A (en) * | 2015-06-30 | 2015-11-11 | 航天材料及工艺研究所 | Preparing method of hot-melt prepreg of novolac epoxy resin |
| CN105150404A (en) * | 2015-07-15 | 2015-12-16 | 北京昂林贸烽科技有限公司 | Method for processing carbon fiber tow |
| CN105904611A (en) * | 2016-04-14 | 2016-08-31 | 北京航空航天大学 | Ultrathin continuous fiber reinforced thermoplastic resin prepreg and preparation method thereof |
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