WO2020155319A1 - 一种基于动态热屏障的树脂基复合材料加热固化方法 - Google Patents

一种基于动态热屏障的树脂基复合材料加热固化方法 Download PDF

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WO2020155319A1
WO2020155319A1 PCT/CN2019/078084 CN2019078084W WO2020155319A1 WO 2020155319 A1 WO2020155319 A1 WO 2020155319A1 CN 2019078084 W CN2019078084 W CN 2019078084W WO 2020155319 A1 WO2020155319 A1 WO 2020155319A1
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curing
composite material
heating
temperature
barrier
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French (fr)
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李迎光
刘舒霆
周靖
张波
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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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
    • B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
    • 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
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • 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
    • B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
    • B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
    • 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
    • B29C70/88—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced

Definitions

  • the invention relates to a composite material curing technology, in particular to a self-heating curing process method assisted by a composite material dynamic regulation and control thermal barrier. Specifically, it is a method for heating and curing resin matrix composites based on dynamic thermal barriers.
  • Resin-based composite materials have developed into key materials in aerospace and other fields by virtue of their high strength, high modulus, small specific gravity, good thermal stability and strong designability.
  • the curing process of the composite material is the key step that takes the longest time and the highest energy consumption, and plays a decisive role in the final performance of the part.
  • the resin undergoes a chemical cross-linking reaction when heated, and the chemical energy of the resin molecular group or chain segment is transformed during the process of bonding to a long molecular chain or network structure, and finally dissipated to the surrounding environment in the form of heat energy.
  • the composite material is cross-linking.
  • the heat released in the catalyzed reaction further progresses in the positive direction, which exacerbates the uneven temperature distribution.
  • the thermal conductivity of the resin in the composite material is poor, and the heat is mainly transmitted along the fiber direction, resulting in uneven temperature during the curing of the composite material component, especially a large temperature gradient in the thickness direction.
  • the above-mentioned problems cause the difference in the degree of solidification in the thickness direction of the part, and generate thermal stress, which seriously affects the mechanical properties and shape accuracy of the molded part.
  • the heating and curing methods for the material itself as the heat source such as microwave heating, electromagnetic induction heating, electric loss heating, and front-end heating of the resin's own chemical energy. If the curing system is exposed to low-temperature air, the surface of the composite material in contact with the air will dissipate A large amount of heat can easily cause the surface and edge temperature to be lower than the core temperature. For example, in the microwave curing and heat preservation stage of the composite material without any heat insulation layer, the surface of the component is 40°C lower than the center temperature, and the surface cannot be completely cured. In response to this problem, the patent CN201610671002.2 proposes a method for rapid curing of sandwich structure composite materials.
  • a breathable insulation layer is applied to the periphery of the induction heating composite material to insulate the internal heat of the material; in addition, the inventors also mentioned earlier in academic papers It is disclosed that a thermal barrier is applied to a microwave-heated composite material component to control the heat dissipation of the composite material itself.
  • the composite material when the curing reaction temperature is reached, the composite material will emit heat rapidly, forming a strong thermal shock, causing the composite material to be ablated, degraded or even scrapped. Furthermore, in order to release the residual stress to the greatest extent, the cooling rate of the composite material before demolding must be controllable. Therefore, the above method of applying a thermal barrier to the self-heating curing method will make the composite material unable to obtain a large and controllable cooling rate when the heat dissipation capacity needs to be quickly dissipated.
  • the patent mainly invented an adiabatic system that can selectively change the thermal conductivity to adapt to a specific ambient temperature.
  • the patent is mainly aimed at heating and cooling problems in buildings.
  • Boeing was inspired by the above patents and published three patents US14941066, EP16180232.7, and US9952007B2 in May 2017 and April 2018. These three patents mentioned the use of one or more of the self-regulating insulation materials.
  • a thermal brake expands and contracts with changes in the surrounding temperature of the thermal insulation material, and then automatically changes the thermal resistance of the thermal insulation material, so as to respond to temperature changes without control system, power supply and human intervention, and improve the curing quality of composite materials.
  • the above patents are in their respective fields, such as internal combustion engines, construction and other fields, to a certain extent, solve the problem of thermal insulation control.
  • the thermal brake insulation material proposed by Boeing can only provide a passive control method with temperature changes.
  • the above method cannot actively and dynamically adjust the temperature field and release the thermal shock during the composite material curing process, and it is difficult to achieve precise control of the temperature and curing quality of the entire curing process.
  • the purpose of the present invention is to address the poor uniformity of the thickness direction or in-plane temperature during the self-heating curing process of the current resin-based composite material, the serious thermal shock of the curing reaction, which greatly affects the mechanical properties of the composite part, and even causes ablation, degradation and scrap
  • a method for heating and curing resin-based composites based on dynamic thermal barriers is proposed.
  • a flexible thermal barrier with dynamically adjustable heat transfer characteristics is applied to the periphery of the composites and molds, combined with the chemical exothermic characteristics of the resin-based composite curing process.
  • the heat transfer characteristics of the thermal barrier are dynamically adjusted to realize the active control of the thickness direction or in-plane temperature distribution of the composite material.
  • it quickly relieves the exothermic impact of the curing reaction greatly improves the temperature uniformity of the composite material thickness direction, and improves the composite
  • the curing quality of material components reduces curing energy consumption.
  • a method for heating and curing resin-based composite materials based on dynamic thermal barriers which is characterized in that, in view of the self-heating curing characteristics of composite material components, a flexible thermal insulation barrier with dynamically adjustable heat transfer characteristics is applied to the periphery of the composite material and the mold. Based on the chemical exothermic characteristics of the curing process of the composite material, the thickness of the composite material and the temperature of each point in the surface are measured. According to the active temperature uniformization control strategy, the heat transfer characteristics of the thermal insulation barrier are dynamically adjusted during the heating, heat preservation and cooling process to achieve composite Active control of temperature distribution in material thickness direction or in-plane.
  • the main body of the flexible thermal insulation barrier whose heat transfer characteristics can be dynamically adjusted is composed of a flexible material with extremely low heat transfer coefficient.
  • the application method is to tightly wrap the surface of the vacuum bag system of the composite material component to reduce the heat emitted by the composite material component itself. Sealed in a flexible thermal insulation barrier, the flexible material with extremely low heat transfer coefficient is aerogel, polyurethane foam, glass wool or composite silicate felt thermal insulation material, for microwave curing or electromagnetic induction heating curing methods,
  • the flexible insulation barrier shall be made of wave-transmitting materials.
  • the method of dynamically controlling the heat transfer characteristics of the heat insulation barrier adopted by the present invention is a method of physical application-evacuation or changing the heat transfer medium in the heat barrier.
  • the physical application-evacuation method is to use manual or automatic device to dynamically load and evacuate
  • mechanical devices that can operate normally in the high-energy electromagnetic radiation field should be used to dynamically load and evacuate the flexible insulation barriers;
  • the method of changing the heat transfer medium in the thermal barrier is to A powerful cooling fluid with a controllable flow rate and flow rate is passed inside the thermal barrier to enhance the heat absorption and dissipation capacity of the thermal barrier.
  • the mechanical device dynamically loading and evacuating the flexible thermal insulation barrier device is an anti-radiation mechanical arm or gear set.
  • the composite material is cured by self-heating, that is, the composite member itself is used as a curing heating source, and the externally input electric energy is used to heat and solidify the composite material itself, or the composite material can release its own stored chemical energy;
  • the input electric energy heating is microwave curing, electromagnetic induction curing or fiber composite material self-resistance electric heating curing, and the chemical energy heating curing is resin-based front end curing.
  • the active temperature homogenization control strategy is to judge the heating rate and the maximum temperature based on the temperature distribution measured in real time.
  • a thermal barrier with extremely low heat transfer coefficient is applied to achieve zero temperature difference in the thickness direction and in-plane; A reaction exothermic shock occurs in the thickness direction, and the actual average temperature exceeds the set threshold.
  • the advance amount is set to trigger the dynamic evacuation program. The evacuation of the thermal barrier exposes the composite to an open room temperature, or high-speed coolant is used to quickly release the thermal shock. If the temperature difference in the thickness direction exceeds the set threshold, the advance is set to trigger the application program, and the thermal barrier is reapplied to make the composite material return to the zero temperature difference state.
  • the threshold and advance are based on the material, size, curing method, and process curve of the composite material. Choose differently.
  • the present invention clearly proposes for the first time the dynamic thermal barrier of the resin-based composite material's electrical loss self-heating curing technology, which breaks through the limitation that the previous curing process is performed in an unchanging atmosphere, and the uniformity control of the temperature only depends on the regulation of the fed energy ; While ensuring the uniformity of the temperature during the heating of the material, it quickly relieves the exothermic impact of the curing reaction, which can greatly improve the curing quality of composite material components, shorten the curing cycle, and reduce curing energy consumption.
  • Fig. 1 is a schematic diagram of the principle of the curing method of a resin-based composite material based on a dynamic thermal barrier in the present invention
  • FIG. 2 Schematic diagram of the thermal barrier design scheme with water-cooled pipes
  • a method for heating and curing resin-based composite materials based on dynamic thermal barriers It focuses on the self-heating and curing characteristics of composite material components.
  • the composite component itself is used as a heating source, which can be externally input electric energy and other forms of energy through transmission
  • the medium is fed into the composite material and dissipates in the material to generate heat to solidify the composite member, or it can be a chemical energy solidification member that releases the composite material itself.
  • a flexible thermal insulation with dynamically adjustable heat transfer characteristics is applied Barrier, combined with the chemical exothermic characteristics of the curing process of the resin-based composite material, measure the thickness of the composite material and the temperature of each point in the surface, according to the temperature uniformity control strategy, dynamically control the heat transfer characteristics of the thermal barrier during the heating, heat preservation and cooling process, Realize the active control of the thickness direction or in-plane temperature distribution of the composite material.
  • the composite material is self-heated and solidified, that is, the composite member itself is used as a curing heating source, and electric energy can be fed into the composite material through transmission media such as electrodes, cables, and air, and the electrical energy is lost in the material to generate heat and solidify the composite material itself; It can also be that in the chemical cross-linking reaction of the composite material, the resin molecular group or segment is formed in the process of bonding to the long molecular chain or network structure to release the chemical energy stored in the composite material; the external electric energy loss heating can be It is microwave curing, electromagnetic induction curing, or self-resistance electrothermal curing of carbon fiber composite materials.
  • the chemical energy heating curing may be resin-based front end curing.
  • the thermal insulation barrier is composed of a flexible material with extremely low heat transfer coefficient, as shown in Figure 1, it is closely attached to the surface of the vacuum bag system covering the composite material component and the corresponding mold, and blocks the heat emitted by the composite material component itself.
  • the thermal barrier can be aerogel, polyurethane foam, glass wool, composite silicate felt and other thermal insulation materials.
  • the thermal barrier needs to be made of wave-transmitting materials.
  • the above insulation materials generally contain a large amount of dust. When used, use vacuum bags and other high-temperature auxiliary materials to wrap the insulation materials to prevent the dust from falling and interfere with the curing of the composite.
  • the heat transfer characteristics of the thermal barrier can be controlled by the method of physical application-evacuation or changing the heat transfer medium of the material.
  • the physical application-evacuation method is the dynamic loading and evacuation of the thermal barrier by manual or automatic devices.
  • the heating and curing method can use mechanical devices that can operate normally in high-energy electromagnetic and microwave radiation fields and do not interfere with the curing process of composite materials, such as radiation-proof robotic arms, wave-transmitting gear sets, etc., and can be attached with dynamic powerful cooling fluid Different heating environments can be used in different ways.
  • the heat transfer medium can be changed by adding water-cooled pipes to the heat barrier or other devices that can quickly reduce the heat transfer coefficient of the heat barrier to facilitate heat dissipation, as shown in Figure 2. Shown.
  • the temperature homogenization control strategy refers to measuring the thickness direction and surface temperature of the composite material separately during the curing process (contact thermocouple temperature measurement, optical fiber temperature measurement can be used, or non-contact infrared thermal imaging measurement) Temperature), according to the temperature distribution measured in real time, the heating rate and the maximum temperature are judged.
  • a thermal barrier with extremely low heat transfer coefficient is applied to block the heat within the thermal barrier, and the conduction effect of temperature is used to achieve Zero temperature difference between thickness direction and in-plane; for thickness direction reaction exothermic shock, the actual average temperature exceeds the set threshold, set the advance amount to trigger the dynamic evacuation program, evacuate the thermal barrier to expose the composite material to the open room temperature, or pass it at a high speed Coolant quickly releases thermal shock.
  • the advance amount is set to trigger the application program, and the thermal barrier is reapplied to make the composite material return to the zero temperature difference state.
  • the threshold and advance amount are based on the composite material , Size, curing method, process curve, etc. to choose.
  • the method for curing a resin-based composite material component based on a dynamic thermal barrier of the present invention is used to cure a 250 mm ⁇ 250 mm flat plate in a composite material self-resistance electrothermal process.
  • the composite material to be tested is made of carbon fiber reinforced bismaleimide resin-based composite material prepreg T700/QY9611.
  • the layup method is [0°/90°] 10s , a total of 20 layers, single layer
  • the thickness of the prepreg is 0.125mm; the mold is a metal mold, the projection size of the mold profiling surface is 600mm ⁇ 600mm, and the thickness is 3mm; the thermal insulation barrier adopts thermal insulation nano aerogel felt.
  • the specific steps of this embodiment are as follows:
  • Step 1 Material preparation: clean the surface of the mold with a cleaning solvent, take out the roll of Shuangma prepreg from the cold storage, cut into 20 pieces of 250mm ⁇ 250mm prepreg according to the design size of the part, and cut the size of 300mm ⁇ 300mm 1 piece of polyimide film, 1 piece of release cloth with a size of 300mm ⁇ 300mm, 1 piece of air felt with a size of 400mm ⁇ 400mm, and 1 vacuum bag with a size of 600mm ⁇ 600mm.
  • the prepared size is 300mm ⁇ 30mm ⁇ 20 1mm copper electrode sheets are spare;
  • Step 2 Place the prepreg: On the layup workbench, place the prepreg in the 0° direction on the workbench, and place two electrode sheets on the two ends perpendicular to the fiber direction to remove air bubbles. , And then place the prepreg material on it in a direction of 90° to compactly remove air bubbles, repeat the above steps until all 20 layers of prepreg material are laid, and connect the electrode to an external power supply with a maximum current of 300A and a maximum voltage of 10V;
  • Step 3 Material placement: Place the polyimide film on the upper surface of the metal mold for insulation, place the laid prepreg in the center of the polyimide film, and place the release cloth, Air felt, insulation at the connection joints, install the optical fiber fluorescence temperature sensor in the thickness direction of the composite material, lay and encapsulate the vacuum bag, and set the optical fiber fluorescence temperature sensor in 12 roads outside the vacuum bag;
  • Step 4 Arrange the thermal insulation barrier: wrap the nano aerogel felt with strong thermal insulation performance in a vacuum bag, and arrange it closely on the surface of the composite material component vacuum bag system and the back of the mold, so that the heat is blocked in the thermal barrier;
  • Step 5 Composite material curing: The curing process is controlled by PID to proceed in accordance with the corresponding process curve; during the heating process of the composite member, the thermal barrier tightly wraps the composite material, and when the temperature rise end is about to enter the 180°C insulation stage, only the surface
  • the robotic arm lifts the thermal insulation material and removes the thermal barrier to fully release the thermal shock.
  • the robotic arm Put down the insulation material and reapply the thermal barrier to bring the temperature difference of the composite material back to zero.
  • the final composite member completes the curing of the entire material with a small temperature difference, and there is no obvious exothermic shock in the curing exothermic stage, thus achieving the improvement of the curing quality of the composite member.
  • the method for curing a 250mm ⁇ 250mm flat plate based on a dynamic thermal barrier resin-based composite material component of the present invention is used in a composite material microwave process.
  • the composite material to be tested is made of carbon fiber reinforced bismaleimide resin-based composite material prepreg T700/QY9611.
  • the layup method is [0°/90°] 10s , a total of 20 layers, single layer
  • the thickness of the prepreg is 0.125mm;
  • the mold is a glass mold, and the projected size of the profiling surface of the mold is 600mm ⁇ 600mm, and the thickness is 3mm;
  • the thermal insulation barrier is made of thermal insulation nano aerogel felt.
  • Step 1 Material preparation: Clean the surface of the glass mold with a cleaning solvent, take out the roll of Shuangma prepreg from the cold storage and cut it into 20 pieces of 250mm ⁇ 250mm prepreg according to the design size of the part.
  • the cutting size is 300mm ⁇ 300mm 1 piece of polyimide film, 2 pieces of release cloth with a size of 300mm ⁇ 300mm, 1 piece of airfelt with a size of 400mm ⁇ 400mm, and 1 vacuum bag with a size of 600mm ⁇ 600mm for spare;
  • Step 2 Material placement: Lay the release cloth on the upper surface of the glass mold, place the pre-laid prepreg in the center of the release cloth, and place the release cloth and air felt on it in sequence.
  • 1 optical fiber fluorescence temperature measurement sensor is installed in the thickness direction of the composite material, vacuum bag is laid and sealed, and 12 optical fiber fluorescence temperature measurement sensors in the road are set outside the vacuum bag;
  • Step 3 Arrange the thermal insulation barrier: bury the water-cooled pipeline in the nano aerogel felt with strong thermal insulation performance, wrap it in a vacuum bag, and closely fit it on the surface of the vacuum bag system of the composite material and the back of the mold, so that the heat is absorbed Sealed in a thermal barrier;
  • Step 4 Composite material curing: The curing process is controlled by PID to proceed in accordance with the corresponding process curve; during the heating process of the composite member, the thermal barrier tightly wraps the composite material, and when the temperature is about to enter the insulation stage of 180°C, the surface
  • the measured temperature of any one of the 13 optical fiber temperature sensors in the inner and thickness directions exceeds the preset threshold, water is injected into the water-cooled pipeline in the thermal barrier to quickly increase the heat transfer coefficient of the thermal barrier to facilitate heat dissipation and fully release the thermal shock.
  • the heat transfer coefficient is controlled by adjusting the flow and flow rate of the water flow in the water-cooled pipeline. When the temperature drops to 180°C, reduce or slow down the water flow in the water-cooled pipeline or directly turn off the water pump to reduce the heat transfer coefficient of the heat barrier to facilitate heat preservation. Let the temperature difference of the composite material return to zero degrees.

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Abstract

一种基于动态热屏障的树脂基复合材料加热固化方法，针对于复材构件自发热固化方法，在复合材料及模具外围，施加传热特性可动态调控的柔性热屏障，结合树脂基复合材料固化过程的化学放热特性，按照温度均匀化策略动态调控热屏障的传热特性，实现复合材料厚度方向或面内温度分布的主动控制。本发明首次提出树脂基复合材料自加热固化技术动态热屏障，旨在保证材料加热过程中温度均匀性的同时，迅速缓解固化反应放热冲击，可大幅改善复合材料构件固化质量，缩短固化周期，降低固化能耗。

Description

一种基于动态热屏障的树脂基复合材料加热固化方法
技术领域
本发明涉及一种复合材料固化技术，尤其是一种复合材料动态调控热屏障辅助下的自发热固化工艺方法。具体地说是一种基于动态热屏障的树脂基复合材料加热固化方法。
背景技术
树脂基复合材料凭借其高强度、高模量、比重小、热稳定好和可设计性强等优点，已发展成为航空航天等领域的关键材料。复材的固化过程是耗时最长，能耗最高，对零件的最终性能起决定性作用的关键步骤。固化过程中，树脂受热发生化学交联反应，树脂分子团或者链段在键合成分子长链或网络结构的过程中化学能发生转变，最终以热能的形式向周围环境耗散，复合材料在交联反应中放出的热量又进一步催化反应向正向进行，更加剧了温度分布不均。而在复合材料中树脂的热传导性能差，热量主要沿纤维方向传播，造成了复合材料构件固化过程中的温度不均匀，尤其是在厚度方向产生较大的温度梯度。上述问题，造成制件厚度方向固化度的不同，产生热应力，严重影响成型后制件的力学性能和外形精度。
针对材料自身作为热源的加热固化方法，如微波加热，电磁感应加热，电损耗加热，树脂自身化学能前端加热等工艺，若固化系统暴露在低温的空气中，与空气接触的复材表面耗散大量的热，极易造成表面及边缘温度低于中心温度。例如，不施加任何隔热层的复材微波固化保温阶段，构件表面相较于中心温度低40℃，表面无法完全固化。对于该问题，专利CN201610671002.2提出一种夹层结构复合材料快速固化的方法，在感应加热复合材料外围施加透气保温层，用以隔绝材料内部热量；另外，本发明人前期在学术论文中，也公开过向微波加热复合材料构件施加热屏障，以控制复材自身热量耗散。
然而，在达到固化反应温度时，复合材料会急剧放热，形成较强热冲击，造成复合材料的烧蚀、降解甚至报废。再者，为了最大程度的释放残余应力，复材脱模前的降温速率必须可控。因此，上述为自加热固化方法施加热屏障的方法，将使得复材无法在需要迅速耗散热量时，获得较大且可控的降温速率。
目前国内还没有对基于动态热屏障解决复合材料固化过程中温度均匀性和热冲击释放研究的公开资料。经查阅国际文献资料，德国的Reinz Dichtungs GmbH公司于2008年12月取得了EP1905653B1的授权，该专利发明了一种隔热罩，在隔热罩中有一个穿过内外表面的凹槽，凹槽通过一根据温度自动开启和闭合的装置闭合，通过打开闭孔，形成放热通 道从而更好地控制温度。该专利主要面向内燃机等产热机械构件的控温。美国Pittsburgh大学的William等人于2013年公开了US20130081786A1的专利，该专利主要发明了一种可选择性地改变导热性能的绝热系统以适应特定的环境温度。但是该专利主要针对建筑中的供热和制冷问题。波音公司从以上专利中得到启发，先后于2017年5月和2018年4月公开了US14941066、EP16180232.7、US9952007B2三份专利，这三份专利中提及了运用自调节保温材料中一个或多个热制动器随着保温材料周围温度的变化而膨胀和收缩，进而自动改变保温材料的热阻，实现在没有控制系统、电源和人为干预的情况下响应温度变化，提升复合材料固化质量。以上专利都在各自领域内，如内燃机，建筑等领域，一定程度上解决了隔热层控制问题，波音公司所提出的热制动保温材料也只能提供随温度变化实现被动控制方法。针对发生复杂自催化化学反应放热的复合材料固化过程，上述方法无法主动且实时动态的调整复合材料固化过程中温度场和释放热冲击，难以实现整个固化过程温度及固化质量的精确控制。
综上所述，对于树脂基复合材料电损耗加热固化工艺，亟需一种新的实现加热过程温度分布均匀、迅速缓解或消除固化反应热冲击，从而大幅改善复合材料厚度方向温度均匀性，提高复合材料构件固化质量，降低固化能耗的方法。
发明内容
本发明的目的是针对目前树脂基复合材料自加热固化过程中厚度方向或者面内温度均匀性差、固化反应热冲击严重，极大影响复材制件的力学性能，甚至造成烧蚀、降解和报废的问题，提出一种基于动态热屏障树脂基复合材料加热固化方法，在复合材料及模具外围，施加传热特性可动态调控的柔性热屏障，结合树脂基复合材料固化过程的化学放热特性，按照温度均匀化策略动态调控热屏障的传热特性，实现复合材料厚度方向或面内温度分布的主动控制的同时，迅速缓解固化反应放热冲击，大幅改善复合材料厚度方向温度均匀性，提高复合材料构件固化质量，降低固化能耗。
本发明技术方案：
一种基于动态热屏障的树脂基复合材料加热固化方法,其特征在于针对于复合材料构件自发热固化特点，在复合材料及模具外围，施加传热特性可动态调控的柔性隔热屏障，根据树脂基复合材料固化过程的化学放热特性，测量复合材料厚度及面内各点温度，按照主动温度均匀化控制策略，在升温、保温及降温过程中动态调控隔热屏障的传热特性，实现复合材料厚度方向或面内温度分布的主动控制。
所述的传热特性可动态调控的柔性隔热屏障主体由传热系数极低的柔性材料构成， 施加方法为紧密包覆于复合材料构件的真空袋体系表面，将复合材料构件自身发出的热量封锁于柔性隔热屏障内，所述的传热系数极低的柔性材料为气凝胶、聚氨酯泡沫、玻璃棉或复合硅酸盐毡类隔热材料，针对微波固化或电磁感应加热固化方式，柔性隔热屏障应采用透波材料制作。
本发明采用的动态调控隔热屏障的传热特性的方法为物理施加-撤离或改变热屏障内传热介质的方法，所述的物理施加-撤离的方法即采用手动或自动装置动态装载和撤离柔性隔热屏障，采用微波和感应加热固化时，应使用能在高能电磁辐射场中正常运行的机械装置动态装载和撤离柔性隔热屏障；所述的改变热屏障内传热介质的方法为向热屏障内通以流速流量可控的强效冷却流体以提升热屏障的吸热和耗散能力。
所述的机械装置动态装载和撤离柔性隔热屏障装置为防辐射机械臂或齿轮组。
所述的复合材料自发热固化，即复材构件自身作为固化加热源，采用损耗外部输入的电能从而发热并固化复合材料自身，或利用复合材料释放出自身存储的化学能；所述的损耗外部输入的电能加热为微波固化、电磁感应固化或纤维复合材料自阻电热固化，所述的化学能加热固化为树脂基前端固化。
所述的主动温度均匀化控制策略为根据实时测量的温度分布，判断升温速率和最高温度，对于自加热升温阶段，施加传热系数极低的热屏障，实现厚度方向和面内零温差；对于厚度方向发生反应放热冲击，实际平均温度超过设定阈值，设置提前量触发动态撤离程序，热屏障撤离使复材暴露在开敞常温中，或通以高速冷却液，迅速释放热冲击，对于厚度方向温差超过设定阈值，设置提前量触发施加程序，热屏障重新施加，使得复合材料重回零温差状态，所述的阈值及提前量根据复合材料的材料、尺寸、固化方式、工艺曲线的不同进行选择。
本发明的有益效果是：
本发明首次明确提出树脂基复合材料电损耗自加热固化技术动态热屏障，突破了以往固化过程都在不发生改变的氛围中进行，温度的均匀性控制只依赖于对馈入能量的调控的局限；保证材料加热过程中温度均匀性的同时，迅速缓解固化反应放热冲击，可大幅改善复合材料构件固化质量，缩短固化周期，降低固化能耗。
附图说明
图1是本发明中基于动态热屏障树脂基复合材料固化方法原理示意图；
图2带有水冷管的热屏障设计方案示意图
具体实施方式
下面将结合附图和具体实施例对本发明作进一步的阐述。下述实施例仅用于说明本方法的某些实施特例，并不用于限制本发明的保护范围。此外，本发明公开后，本领域技术人员基于本发明中基于动态热屏障树脂基复合材料加热固化的原理做出任何的修改或变化，都属于本申请权利要求书中所限定保护的范围。
如图1-2所示。
一种基于动态热屏障树脂基复合材料加热固化方法,它重点是针对于复合材料构件自发热固化特点，利用复材构件自身作为加热源，可以是外部输入的电能等多种形式的能量经由传输介质馈入复合材料内部，在材料中耗散产生热量固化复材构件，也可以是释放复材自身的化学能固化构件，在复合材料及模具外围，施加传热特性可动态调控的柔性隔热屏障，结合树脂基复合材料固化过程的化学放热特性，测量复合材料厚度及面内各点温度，按照温度均匀化控制策略，在升温、保温及降温过程，动态调控热屏障的传热特性，实现复合材料厚度方向或面内温度分布的主动控制。通过对树脂基复合材料电损耗自加热固化技术施加动态热屏障，突破了以往固化过程都在不发生改变的氛围中进行，温度的均匀性控制只依赖于对馈入能量的调控的局限；保证材料加热过程中温度均匀性的同时，迅速缓解固化反应放热冲击，可大幅改善复合材料构件固化质量，缩短固化周期，降低固化能耗。所述的复合材料自加热固化，即复材构件自身作为固化加热源，可以是通过电极、电缆、空气等传输介质将电能馈入复合材料内部，电能在材料内部损耗发热并固化复合材料自身；也可以是复合材料在化学交联反应中，树脂分子团或者链段在键合成分子长链或网络结构的过程中化学键的形成释放出自身存储的化学能固化复合材料；所述的外部电能损耗加热可以是微波固化，也可以是电磁感应固化，也可以是碳纤维复合材料自阻电热固化，所述的化学能加热固化可以是树脂基前端固化等。所述的绝热屏障由传热系数极低的柔性材料构成，如图1所示，紧密贴合于包覆复合材料构件及相应模具的真空袋体系表面，将复合材料构件自身发出的热量封锁于热屏障内，所述的绝热屏障可以是气凝胶、聚氨酯泡沫、玻璃棉、复合硅酸盐毡等隔热材料，针对微波固化或电磁感应加热等固化方式，热屏障需采用透波材料，以上隔热材料普遍含有大量的粉尘，使用时用真空袋等耐高温的辅助材料包裹隔热材料，防止粉尘掉落，干扰复材固化。所述的调控热屏障的传热特性可通过物理施加-撤离或改变材料传热介质的方法，所述的物理施加-撤离的方法即手动或自动装置动态装载和撤离热屏障，对于微波和感应加热固化方法，可使用在高能电磁、微波辐射场中能正常运行且不干扰复材固化过程的机械装置，如防辐射机械臂、透波的齿轮组等，同时可附以动态强效冷却流体，不同的加热环境中使用的方式可以有所不同，所述的改变材料传热介质可在热屏障中添加水冷管路或者其他可 迅速降低热屏障传热系数以利于散热的装置，如图2所示。所述的温度均匀化控制策略是指在固化过程中，分别测量复合材料厚度方向和表面的温度(可以利用接触式的热电偶测温、光纤测温，也可以是非接触式的红外热成像测温)，根据实时测得的温度分布，判断升温速率和最高温度，对于自加热升温阶段，施加传热系数极低的热屏障，将热量封锁在热屏障之内，利用温度的传导效应，实现厚度方向和面内零温差；对于厚度方向发生反应放热冲击，实际平均温度超过设定阈值，设置提前量触发动态撤离程序，撤离热屏障使复材暴露在开敞常温中，或通以高速冷却液，迅速释放热冲击，对于厚度方向温差超过设定阈值，设置提前量触发施加程序，热屏障重新施加，使得复合材料重回零温差状态，所述的阈值及提前量根据复合材料的材料、尺寸、固化方式、工艺曲线等的不同进行选择。
实施例1。
本实施例是在复合材料自阻电热工艺中利用本发明的基于动态热屏障树脂基复合材料构件固化方法来固化250mm×250mm平板件。所述的待测复合材料由碳纤维增强双马来酰亚胺树脂基复合材料预浸料T700/QY9611铺叠而成，铺层方法为[0°/90°] 10s，共20层，单层预浸料的厚度为0.125mm；所述模具为金属模具，模具靠模面的投影尺寸为600mm×600mm，厚度为3mm；所述的绝热屏障采用的是保温纳米气凝胶毡。本实施例的具体步骤如下：
步骤1：材料准备：用清洁溶剂清洗模具表面，从冷库中取出成卷的双马预浸料根据零件设计尺寸裁成250mm×250mm的预浸料片20片备用，裁剪尺寸为300mm×300mm的聚酰亚胺薄膜1张、尺寸为300mm×300mm的脱模布1块、尺寸为400mm×400mm的透气毡1块以及尺寸为600mm×600mm的真空袋1个备用，准备尺寸为300mm×30mm×1mm的紫铜电极片20片备用；
步骤2：预浸料铺放：在铺层操作台上，将0°方向的预浸料铺放在操作台上，在其上垂直于纤维方向的两端铺放两电极片压实去除气泡，再在其上铺放90°方向预浸料压实去除气泡，重复以上步骤直到全部的20层预浸料铺放完成，将电极与最大电流300A、最大电压10V的外部电源连接起来；
步骤3：材料铺放：在金属模具上表面铺放聚酰亚胺薄膜起绝缘作用，将铺放好的预浸料放置在聚酰亚胺薄膜正中，按顺序依次铺放好脱模布、透气毡，做好连接接头处的绝缘，在复合材料件厚度方向安装光纤荧光测温传感器，铺放并封装真空袋，在真空袋外设置12路面内的光纤荧光测温传感器；
步骤4：布置绝热屏障：将保温性能极强的纳米气凝胶毡用真空袋包裹起来，紧密贴合布置 在复合材料构件真空袋体系的表面和模具背面，使得热量被封锁在热屏障内；
步骤5：复合材料固化：通过PID控制固化过程按照相应的工艺曲线进行；复材构件升温过程中，热屏障紧紧包覆复合材料，在升温末端即将要进入180℃的保温阶段时，只要面内和厚度方向的13路光纤测温传感器的任意一路测量温度超过预设的阈值时，机械手臂抬起保温材料，撤除热屏障，让热冲击充分释放，当温度降至180℃时，机械臂放下保温材料，重新施加热屏障，让复合材料温差回到零度。
上述的实例最终复材构件以较小的温差完成了整个材料的固化，在固化放热阶段也未出现明显的放热冲击，实现了复合材料构件固化质量的提高。
实施例2。
本实施例是在复合材料微波工艺中利用本发明的基于动态热屏障树脂基复合材料构件固化方法来固化250mm×250mm平板件。所述的待测复合材料由碳纤维增强双马来酰亚胺树脂基复合材料预浸料T700/QY9611铺叠而成，铺层方法为[0°/90°] 10s，共20层，单层预浸料的厚度为0.125mm；所述模具为玻璃模具，模具靠模面的投影尺寸为600mm×600mm，厚度为3mm；所述的绝热屏障采用的是保温纳米气凝胶毡。本实施例的具体步骤如下：
步骤1：材料准备：用清洁溶剂清洗玻璃模具表面，从冷库中取出成卷的双马预浸料根据零件设计尺寸裁成250mm×250mm的预浸料片20片备用，裁剪尺寸为300mm×300mm的聚酰亚胺薄膜1张、尺寸为300mm×300mm的脱模布2块、尺寸为400mm×400mm的透气毡1块以及尺寸为600mm×600mm的真空袋1个备用；
步骤2：材料铺放：在玻璃模具上表面铺放脱模布，将预先铺放好的预浸料放置在脱模布正中，其上按顺序依次铺放好脱模布、透气毡，在复合材料件厚度方向安装1路光纤荧光测温传感器，铺放并封装真空袋，在真空袋外设置12路面内的光纤荧光测温传感器；
步骤3：布置绝热屏障：在保温性能极强的纳米气凝胶毡中埋设水冷管路,用真空袋包裹起来，紧密贴合布置在复合材料构件真空袋体系的表面和模具背面，使得热量被封锁在热屏障内；
步骤4：复合材料固化：通过PID控制固化过程按照相应的工艺曲线进行；复材构件升温过程中，热屏障紧紧包覆复合材料，在升温末端即将要进入180℃的保温阶段时，只要面内和厚度方向的13路光纤测温传感器的任意一路测量温度超过预设的阈值时，向热屏障内的水冷管路注水，迅速提高热屏障传热系数以利于散热，让热冲击充分释放，传热系数的控制通过调节水冷管路内水流的流量和流速，当温度降至180℃时，调小、调慢水冷管路的水流或直接关闭水泵，降低热屏障传热系数以利于保温，让复合材料温差回到零度。
本发明未涉及部分与现有技术相同或可采用现有技术加以实现。

Claims (6)

  1. 一种基于动态热屏障的树脂基复合材料加热固化方法,其特征在于针对于复合材料构件自发热固化特点，在复合材料及模具外围，施加传热特性可动态调控的柔性隔热屏障，根据树脂基复合材料固化过程的化学放热特性，测量复合材料厚度及面内各点温度，按照主动温度均匀化控制策略，在升温、保温及降温过程中动态调控隔热屏障的传热特性，实现复合材料厚度方向或面内温度分布的主动控制。
  2. 根据权利要求1所述的方法，其特征在于所述的传热特性可动态调控的柔性隔热屏障主体由传热系数极低的柔性材料构成，施加方法为紧密包覆于复合材料构件的真空袋体系表面，将复合材料构件自身发出的热量封锁于柔性隔热屏障内，所述的传热系数极低的柔性材料为气凝胶、聚氨酯泡沫、玻璃棉或复合硅酸盐毡类隔热材料，针对微波固化或电磁感应加热固化方式，柔性隔热屏障应采用透波材料制作。
  3. 根据权利要求1所述的方法，其特征在于动态调控隔热屏障的传热特性的方法为物理施加-撤离或改变热屏障内传热介质的方法，所述的物理施加-撤离的方法即采用手动或自动装置动态装载和撤离柔性隔热屏障，采用微波和感应加热固化时，应使用能在高能电磁辐射场中正常运行的机械装置动态装载和撤离柔性隔热屏障；所述的改变热屏障内传热介质的方法为向热屏障内通以流速流量可控的强效冷却流体以提升热屏障的吸热和耗散能力。
  4. 根据权利要求3所述的方法，其特征在于所述的机械装置动态装载和撤离柔性隔热屏障装置为防辐射机械臂或齿轮组。
  5. 根据权利要求1所述的方法，其特征在于所述的复合材料自发热固化，即复材构件自身作为固化加热源，采用损耗外部输入的电能从而发热并固化复合材料自身，或利用复合材料释放出自身存储的化学能；所述的损耗外部输入的电能加热为微波固化、电磁感应固化或纤维复合材料自阻电热固化，所述的化学能加热固化为树脂基前端固化。
  6. 根据权利要求1所述的方法，其特征在于所述的主动温度均匀化控制策略为根据实时测量的温度分布，判断升温速率和最高温度，对于自加热升温阶段，施加传热系数极低的热屏障，实现厚度方向和面内零温差；对于厚度方向发生反应放热冲击，实际平均温度超过设定阈值，设置提前量触发动态撤离程序，热屏障撤离使复材暴露在开敞常温中，或通以高速冷却液，迅速释放热冲击，对于厚度方向温差超过设定阈值，设置提前量触发施加程序，热屏障重新施加，使得复合材料重回零温差状态，所述的阈值及提前量根据复合材料的材料、尺寸、固化方式、工艺曲线的不同进行选择。
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