CN111844968A - A kind of preparation method of polyimide fiber/polytetrafluoroethylene fiber self-lubricating fabric backing material - Google Patents
A kind of preparation method of polyimide fiber/polytetrafluoroethylene fiber self-lubricating fabric backing material Download PDFInfo
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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Abstract
Description
技术领域technical field
本发明涉及一种聚酰亚胺纤维/聚四氟乙烯纤维自润滑织物衬垫材料的制备方法,主要用于高温、高速等极端服役工况条件下的自润滑关节轴承的加工,属于复合材料制备和固体润滑技术领域。The invention relates to a preparation method of a polyimide fiber/polytetrafluoroethylene fiber self-lubricating fabric lining material, which is mainly used for the processing of self-lubricating spherical plain bearings under extreme service conditions such as high temperature and high speed, and belongs to composite materials The technical field of preparation and solid lubrication.
背景技术Background technique
自润滑关节轴承是一种球面滑动轴承,主要由带有内球面的外圈、外球面的内圈以及自润滑衬垫组成,因其兼具结构紧凑、承载能力强、耐腐蚀和免维护等优点,而被广泛应用于航空航天、精密机械等高端装备润滑领域。自润滑织物衬垫材料作为自润滑关节轴承的关键组件,其摩擦磨损性能直接影响自润滑关节轴承的服役行为和使用寿命。自润滑织物衬垫是以聚四氟乙烯纤维与其它的高性能增强纤维混合编织的薄层织物与聚合物树脂复合而成,使其兼具聚四氟乙烯纤维优异的润滑性能和增强纤维突出的承载能力。Self-lubricating spherical plain bearing is a spherical plain bearing mainly composed of an outer ring with an inner spherical surface, an inner ring with an outer spherical surface and a self-lubricating gasket. Because of its compact structure, strong bearing capacity, corrosion resistance and maintenance-free, etc. It is widely used in aerospace, precision machinery and other high-end equipment lubrication fields. As a key component of self-lubricating spherical plain bearings, self-lubricating fabric backing material directly affects the service behavior and service life of self-lubricating spherical plain bearings. The self-lubricating fabric liner is made of a thin-layer fabric woven with polytetrafluoroethylene fibers and other high-performance reinforcing fibers mixed with polymer resin, making it both have the excellent lubricating properties of polytetrafluoroethylene fibers and the outstanding reinforcement fibers. carrying capacity.
近年来,工程机械装备技术的快速发展对自润滑织物衬垫材料的摩擦磨损性能提出了更高的要求,如要求织物衬垫材料能够在高温、高速等极端工况条件下保持稳定、长效运行。在之前的研究中,聚四氟乙烯/芳纶酚醛树脂基织物衬垫材料因其优异的减摩耐磨性能而得到广泛地应用,但该衬垫材料的热性能较差,难以满足高温、高速等极端工况的要求。因此,提升自润滑织物衬垫的耐高温性能具有重大的意义,同时也面临诸多挑战。In recent years, the rapid development of construction machinery and equipment technology has put forward higher requirements for the friction and wear properties of self-lubricating fabric backing materials, such as requiring fabric backing materials to be stable and long-lasting under extreme working conditions such as high temperature and high speed. run. In previous studies, PTFE/aramid phenolic resin-based fabric lining materials have been widely used because of their excellent anti-friction and wear resistance properties, but the thermal properties of this lining material are poor, and it is difficult to meet high temperature, Requirements for extreme working conditions such as high speed. Therefore, improving the high temperature resistance of self-lubricating fabric liners is of great significance, but also faces many challenges.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种聚酰亚胺纤维/聚四氟乙烯纤维自润滑织物衬垫材料的制备方法和应用。The purpose of the present invention is to provide a preparation method and application of a polyimide fiber/polytetrafluoroethylene fiber self-lubricating fabric backing material.
一、自润滑织物衬垫材料的制备1. Preparation of self-lubricating fabric backing material
本发明自润滑织物衬垫材料的制备,是以聚四氟乙烯纤维作为经纱,聚酰亚胺纤维作为纬纱编织织物,织物先经空气等离子体改性处理,再在聚酰亚胺溶液中浸渍、烘干,并重复浸渍、烘干直至聚酰亚胺树脂在织物中的质量分数达到目标要求;然后用聚酰亚胺树脂将浸渍好的织物衬垫粘贴在金属基材表面,最后经固化反应,得到自润滑织物衬垫材料。The preparation of the self-lubricating fabric lining material of the present invention uses polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns to weave fabrics. The fabrics are first modified by air plasma, and then dipped in polyimide solution. , drying, and repeated impregnation and drying until the mass fraction of polyimide resin in the fabric reaches the target requirement; then the impregnated fabric liner is pasted on the surface of the metal substrate with polyimide resin, and finally cured After the reaction, a self-lubricating fabric backing material was obtained.
所述编织织物的组织结构为平纹、斜纹、缎纹中的一种或联合使用几种组织。The weave structure of the woven fabric is one of plain weave, twill weave and satin weave, or a combination of several weaves.
所述空气等离子体处理的时间为5~20 min,功率为50~200 W。The time of the air plasma treatment is 5-20 min, and the power is 50-200 W.
所述聚酰亚胺树脂在织物衬垫材料中的质量分数为20~30%。The mass fraction of the polyimide resin in the fabric backing material is 20-30%.
所述金属基材为金属基材为9Cr18Mo、9Cr18MoV、9Cr18、4Cr13、17-4PH中的一种。The metal base material is one of 9Cr18Mo, 9Cr18MoV, 9Cr18, 4Cr13 and 17-4PH.
所述固化反应,实在施加压力0.1~0.3 MPa的条件下,依次经100、150、200、265 ℃四段,每段保温时间为30~60 min,升温速率为5~10 ℃/min。The curing reaction, under the condition of applying a pressure of 0.1-0.3 MPa, goes through four stages of 100, 150, 200, and 265 °C in sequence, and the holding time of each stage is 30-60 min, and the heating rate is 5-10 °C/min.
二、摩擦磨损性能测试2. Friction and wear performance test
1、高温摩擦学性能1. High temperature tribological properties
测试方法:采用玄武三号摩擦磨损试验机,以直径2 mm的45号钢作为摩擦对偶,在确定的滑动速度、应用载荷、试验时间等条件下,通过配备在摩擦副外部的加热炉调节摩擦试验的环境温度进行摩擦测试。摩擦系数通过连接的计算机处理收集到的数据后,自动输出。利用数显高度仪测量自润滑织物衬垫材料的磨损深度,进而计算织物衬垫的磨损体积。采用K=ΔV/P∙L公式计算织物衬垫材料的比磨损率,K─比磨损率;ΔV─磨损体积;P─应用载荷;L─滑动距离。Test method: Xuanwu No. 3 friction and wear testing machine was used, and No. 45 steel with a diameter of 2 mm was used as the friction pair. Under certain conditions such as sliding speed, applied load, and test time, the friction was adjusted by a heating furnace equipped outside the friction pair. The friction test was carried out at the ambient temperature of the test. The coefficient of friction is automatically output after processing the collected data through a connected computer. Using a digital altimeter to measure the wear depth of the self-lubricating fabric pad material, and then calculate the wear volume of the fabric pad. The specific wear rate of the fabric backing material was calculated using the formula K=ΔV/P∙L, K─specific wear rate; ΔV─wear volume; P─applied load; L─sliding distance.
图1为聚四氟乙烯/聚酰亚胺织物-聚酰亚胺树脂基织物衬垫的摩擦系数(a)和磨损率随环境温度变化的柱状图(b)。图1(a)的结果显示,自润滑织物衬垫在试验温度范围内均能保持优异的润滑性能,且随环境温度的上升,自润滑织物衬垫材料的摩擦系数呈现下降的趋势。当试验环境温度为335 ℃时,织物衬垫材料的摩擦系数为0.0453,呈现出优异的高温润滑性能。图1(b)的结果显示,自润滑织物衬垫的比磨损率随环境温度的上升呈现明显的上升趋势,但在试验温度范围内均能保持突出的耐磨性能。当试验环境温度为335 ℃时,织物衬垫材料的磨损率为22.1×10-14 m3· (N·m)-1,依旧保持在较低的水平,表现出优异的高温抗磨性能。Figure 1 is a bar graph (b) of the coefficient of friction (a) and wear rate of PTFE/polyimide fabric-polyimide resin-based fabric pads as a function of ambient temperature. The results in Figure 1(a) show that the self-lubricating fabric liner can maintain excellent lubricating performance in the test temperature range, and with the increase of the ambient temperature, the friction coefficient of the self-lubricating fabric liner material shows a downward trend. When the test environment temperature is 335 ℃, the friction coefficient of the fabric backing material is 0.0453, showing excellent high temperature lubrication performance. The results in Figure 1(b) show that the specific wear rate of the self-lubricating fabric liner shows an obvious upward trend with the increase of the ambient temperature, but it can maintain outstanding wear resistance in the test temperature range. When the test environment temperature was 335 ℃, the wear rate of the fabric backing material was 22.1×10 -14 m 3 · (N · m) -1 , which remained at a low level, showing excellent high temperature wear resistance.
2、高速摩擦学性能2. High-speed tribological properties
测试方法:采用玄武三号摩擦磨损试验机,以直径2 mm的45号钢作为摩擦对偶,在室温以及确定的应用载荷、试验时间等条件下,通过调节摩擦试验的滑动速度,探索滑动速度对织物衬垫摩擦学性能的影响。摩擦系数通过连接的计算机处理收集到的数据后,自动输出。利用数显高度仪测量自润滑织物衬垫材料的磨损深度,进而计算织物衬垫的磨损体积。采用K=ΔV/P∙L公式计算织物衬垫材料的比磨损率,K─比磨损率;ΔV─磨损体积;P─应用载荷;L─滑动距离。Test method: Xuanwu No. 3 friction and wear testing machine was used, and No. 45 steel with a diameter of 2 mm was used as the friction pair. Under the conditions of room temperature and certain applied load and test time, the sliding speed of the friction test was adjusted to explore the effect of sliding speed on the friction test. Influence of tribological properties of fabric pads. The coefficient of friction is automatically output after processing the collected data through a connected computer. Using a digital altimeter to measure the wear depth of the self-lubricating fabric pad material, and then calculate the wear volume of the fabric pad. The specific wear rate of the fabric backing material was calculated using the formula K=ΔV/P∙L, K─specific wear rate; ΔV─wear volume; P─applied load; L─sliding distance.
图2为聚四氟乙烯/聚酰亚胺织物-聚酰亚胺树脂基织物衬垫的摩擦系数(a)和磨损率随滑动速度变化的柱状图(b)。图2(a)的结果显示,自润滑织物衬垫在试验滑动速度范围内均能保持优异的润滑性能,且随滑动速度的增加,自润滑织物衬垫材料的摩擦系数呈现轻微的下降趋势。当滑动速度为2.73m/s时,织物衬垫材料的摩擦系数为0.1322,依然保持在较低的水平。图2(b)的结果显示,自润滑织物衬垫的比磨损率随滑动速度的上升呈现明显的下降趋势。当试验滑动速度为2.73m/s时,织物衬垫材料的比磨损率为2.3×10-14m3· (N·m)-1,保持在较低的水平,表现出优异的高速摩擦学性能。Figure 2 is a bar graph (b) of the coefficient of friction (a) and wear rate of the PTFE/polyimide fabric-polyimide resin-based fabric pad as a function of sliding speed. The results in Fig. 2(a) show that the self-lubricating fabric liner can maintain excellent lubricating performance in the test sliding speed range, and with the increase of sliding speed, the friction coefficient of the self-lubricating fabric liner material shows a slight downward trend. When the sliding speed is 2.73m/s, the friction coefficient of the fabric backing material is 0.1322, which remains at a low level. The results in Fig. 2(b) show that the specific wear rate of the self-lubricating fabric liner shows a clear downward trend with the increase of the sliding speed. When the test sliding speed is 2.73m/s, the specific wear rate of the fabric backing material is 2.3×10 -14 m 3 · (N · m) -1 , which is kept at a low level, showing excellent high-speed tribology performance.
综上所述,本发明使用聚酰亚胺纤维作为增强纤维,与聚四氟乙烯纤维混纺编织,制得聚四氟乙烯/聚酰亚胺织物-聚酰亚胺树脂基自润滑织物衬垫材料具有较好的浸润性能,使得织物衬垫材料的界面黏附性能良好。同时由于使用的聚酰亚胺纤维及聚酰亚胺树脂均具备突出的热稳定性能,赋予自润滑织物衬垫材料优异的高温、高速摩擦学性能,因此适用于高温、高速等极端服役工况条件,极大地拓展了自润滑关节轴承在高端装备润滑领域的应用范围。To sum up, the present invention uses polyimide fibers as reinforcing fibers, and blends and weaves with polytetrafluoroethylene fibers to prepare polytetrafluoroethylene/polyimide fabric-polyimide resin-based self-lubricating fabric pads The material has good wettability, which makes the interfacial adhesion of the fabric backing material good. At the same time, because the polyimide fiber and polyimide resin used have outstanding thermal stability, they endow the self-lubricating fabric backing material with excellent high temperature and high speed tribological properties, so it is suitable for extreme service conditions such as high temperature and high speed. conditions, which greatly expands the application scope of self-lubricating spherical plain bearings in the field of high-end equipment lubrication.
附图说明Description of drawings
图1为聚四氟乙烯/聚酰亚胺织物-聚酰亚胺树脂基织物衬垫的摩擦系数、磨损率随环境温度变化的柱状图(0.26 m/s, 12.5 MPa)。Figure 1 is a histogram of the friction coefficient and wear rate of PTFE/polyimide fabric-polyimide resin-based fabric liner as a function of ambient temperature (0.26 m/s, 12.5 MPa).
图2为聚四氟乙烯/聚酰亚胺织物-聚酰亚胺树脂基织物衬垫的摩擦系数、磨损率随滑动速度变化的柱状图(室温, 12.5 MPa)。Figure 2 is a histogram of the friction coefficient and wear rate of the PTFE/polyimide fabric-polyimide resin-based fabric pad as a function of sliding speed (room temperature, 12.5 MPa).
具体实施方式Detailed ways
下面通过具体实施例对本发明聚酰亚胺纤维/聚四氟乙烯纤维自润滑织物衬垫材料及其制备方法和应用作进一步说明。The polyimide fiber/polytetrafluoroethylene fiber self-lubricating fabric backing material of the present invention and its preparation method and application will be further described below through specific examples.
实施例1Example 1
以聚四氟乙烯纤维作为经纱,聚酰亚胺纤维作为纬纱,编织破斜纹织物;织物先经空气等离子体改性处理后(10 min,100 W),再在聚酰亚胺溶液中浸渍、烘干,并重复浸渍、烘干直至聚酰亚胺树脂在织物中的质量分数达到30 wt%;然后用聚酰亚胺树脂将浸渍好的织物衬垫粘贴在9Cr18Mo金属基材表面,最后在0.2 MPa压力条件下,依次经20 min升至100 ℃并保温30 min、10 min升至150 ℃并保温60 min、10 min升至200 ℃并保温60 min、10 min升至265 ℃并保温120 min的固化反应,制得自润滑织物衬垫材料。The broken twill fabric was woven with polytetrafluoroethylene fiber as the warp yarn and polyimide fiber as the weft yarn; the fabric was first modified by air plasma (10 min, 100 W), and then dipped in polyimide solution, Drying, and repeated impregnation and drying until the mass fraction of polyimide resin in the fabric reaches 30 wt%; then the impregnated fabric liner is pasted on the surface of the 9Cr18Mo metal substrate with polyimide resin, and finally Under the condition of 0.2 MPa pressure, successively increased to 100 °C for 20 min and held for 30 min, 10 min to 150 °C and held for 60 min, 10 min to 200 °C and held for 60 min, 10 min to 265 °C and held for 120 min. Min curing reaction, produced self-lubricating fabric backing material.
利用玄武三号摩擦磨损试验机评估上述制得自润滑织物衬垫的摩擦学性能,在0.26 m/s, 12.5 MPa条件下,于335 ℃高温环境中的摩擦系数和磨损率分别为0.051,25×10-14 m3· (N·m)-1。The tribological properties of the self-lubricating fabric pads prepared above were evaluated by the Xuanwu No. 3 friction and wear tester. Under the conditions of 0.26 m/s, 12.5 MPa, the friction coefficient and wear rate in a high temperature environment of 335 ℃ were 0.051, 25 ×10 -14 m 3 · (N·m) -1 .
实施例2Example 2
以聚四氟乙烯纤维作为经纱、聚酰亚胺纤维作为纬纱编织缎纹织物;织物先经空气等离子体改性处理(8 min,120 W),再在聚酰亚胺溶液中浸渍、烘干,并重复浸渍、烘干直至聚酰亚胺树脂在织物衬垫材料中的质量分数达到25 wt%;然后用聚酰亚胺树脂将浸渍好的织物粘贴在9Cr18Mo金属基材表面,最后在0.2 MPa压力条件下,依次经20 min升至100 ℃并保温30 min、10 min升至150℃并保温60 min、10 min升至200 ℃并保温60 min、10 min升至265℃并保温120 min的固化反应,制得自润滑织物衬垫材料。The satin fabric was woven with polytetrafluoroethylene fiber as warp yarn and polyimide fiber as weft yarn; the fabric was first modified by air plasma (8 min, 120 W), and then dipped and dried in polyimide solution. , and repeated impregnation and drying until the mass fraction of polyimide resin in the fabric backing material reached 25 wt%; then the impregnated fabric was pasted on the surface of 9Cr18Mo metal substrate with polyimide resin, and finally at 0.2 Under MPa pressure conditions, successively increased to 100 °C for 20 min and held for 30 min, 10 min to 150 °C and held for 60 min, 10 min to 200 °C and held for 60 min, 10 min to 265 °C and held for 120 min The curing reaction of self-lubricating fabric backing material is obtained.
利用玄武三号摩擦磨损试验机评估上述制得自润滑织物衬垫的摩擦学性能,在0.26 m/s,12.5 MPa条件下,于335 ℃高温环境中的摩擦系数和磨损率分别为0.042,19×10-14 m3· (N·m)-1。The tribological properties of the self-lubricating fabric pads prepared above were evaluated by the Xuanwu No. 3 friction and wear testing machine. Under the conditions of 0.26 m/s and 12.5 MPa, the friction coefficient and wear rate in a high temperature environment of 335 ℃ were 0.042, 19 ×10 -14 m 3 · (N·m) -1 .
实施例3Example 3
以聚四氟乙烯纤维作为经纱、聚酰亚胺纤维作为纬纱编织平纹织物;织物先经空气等离子体改性处理后(10 min,100 W),再在聚酰亚胺溶液中浸渍、烘干,并重复浸渍、烘干直至聚酰亚胺树脂在织物衬垫材料中的质量分数达到30 wt%;然后用聚酰亚胺树脂将浸渍好的织物衬垫粘贴在17-4PH金属基材表面,最后在0.2 MPa压力条件下,依次经20 min升至100 ℃并保温60 min、10 min升至150 ℃并保温120 min、10 min升至200 ℃并保温120min、10 min升至265 ℃并保温150 min的固化反应,制得自润滑织物衬垫材料。The plain weave fabric was woven with polytetrafluoroethylene fiber as warp yarn and polyimide fiber as weft yarn; the fabric was first modified by air plasma (10 min, 100 W), and then dipped and dried in polyimide solution. , and repeated impregnation and drying until the mass fraction of polyimide resin in the fabric pad material reaches 30 wt%; then the impregnated fabric pad is pasted on the surface of the 17-4PH metal substrate with polyimide resin , and finally, under the pressure of 0.2 MPa, successively increased to 100 °C for 20 min and held for 60 min, 10 min to 150 °C and held for 120 min, 10 min to 200 °C and held for 120 min, 10 min to 265 °C and then held at 265 °C for 10 min. The curing reaction was kept for 150 min to obtain a self-lubricating fabric backing material.
利用玄武三号摩擦磨损试验机评估上述制得自润滑织物衬垫的摩擦学性能,在0.26 m/s, 12.5 MPa条件下,于335 ℃高温环境中的摩擦系数和磨损率分别为0.06,23×10-14 m3· (N·m)-1。The tribological properties of the self-lubricating fabric linings prepared above were evaluated by the Xuanwu No. 3 friction and wear testing machine. Under the conditions of 0.26 m/s and 12.5 MPa, the friction coefficient and wear rate in a high temperature environment of 335 ℃ were 0.06 and 23, respectively. ×10 -14 m 3 · (N·m) -1 .
实施例4Example 4
以聚四氟乙烯纤维作为经纱、聚酰亚胺纤维作为纬纱编织斜纹织物;织物先经空气等离子体改性处理后(5 min,200 W),再在聚酰亚胺溶液中浸渍、烘干,重复浸渍、烘干直至聚酰亚胺树脂在织物衬垫材料中的质量分数达到20 wt%;然后用聚酰亚胺树脂将浸渍好的织物衬垫粘贴在17-4PH金属基材表面,最后在0.25 MPa压力条件下,依次经25 min升至100℃并保温30 min、15 min升至150 ℃并保温60 min、15 min升至200 ℃并保温60 min、15min升至265 ℃并保温120 min的固化反应,制得自润滑织物衬垫材料。The twill fabric was woven with polytetrafluoroethylene fiber as warp yarn and polyimide fiber as weft yarn; the fabric was first modified by air plasma (5 min, 200 W), and then dipped and dried in polyimide solution. , repeated impregnation and drying until the mass fraction of polyimide resin in the fabric pad material reached 20 wt%; then the impregnated fabric pad was pasted on the surface of the 17-4PH metal substrate with polyimide resin, Finally, under the condition of 0.25 MPa pressure, the temperature was successively increased to 100 °C for 25 min and held for 30 min, 15 min to 150 °C and held for 60 min, 15 min to 200 °C and held for 60 min, 15 min to 265 °C and held for 15 min. After 120 min of curing reaction, a self-lubricating fabric backing material was prepared.
利用玄武三号摩擦磨损试验机评估上述制得自润滑织物衬垫的摩擦学性能,在0.26 m/s, 12.5 MPa条件下,于335 ℃高温环境中的摩擦系数和磨损率分别为0.039,21×10-14 m3· (N·m)-1。The tribological properties of the self-lubricating fabric pads prepared above were evaluated by the Xuanwu No. 3 friction and wear tester. Under the conditions of 0.26 m/s, 12.5 MPa, the friction coefficient and wear rate in a high temperature environment of 335 ℃ were 0.039, 21 ×10 -14 m 3 · (N·m) -1 .
实施例5Example 5
以聚四氟乙烯纤维作为经纱、聚酰亚胺纤维作为纬纱编织斜纹织物,织物先经空气等离子体改性处理后(5 min,200 W),再在聚酰亚胺溶液中浸渍、烘干,并重复浸渍、烘干直至聚酰亚胺树脂在织物衬垫材料中的质量分数达到20 wt%;然后用聚酰亚胺树脂将浸渍好的织物衬垫粘贴在9Cr18金属基材表面,最后在0.25 MPa压力条件下,依次经25 min升至100℃并保温30 min、15 min升至150 ℃并保温60 min、15 min升至200 ℃并保温60 min、15min升至265 ℃并保温120 min的固化反应,制得自润滑织物衬垫材料。The twill fabrics were woven with polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns. The fabrics were first modified by air plasma (5 min, 200 W), and then dipped and dried in polyimide solution. , and repeated impregnation and drying until the mass fraction of polyimide resin in the fabric pad material reached 20 wt%; then the impregnated fabric pad was pasted on the surface of the 9Cr18 metal substrate with polyimide resin, and finally Under the condition of 0.25 MPa pressure, successively increased to 100 °C for 25 min and held for 30 min, 15 min to 150 °C and held for 60 min, 15 min to 200 °C and held for 60 min, 15 min to 265 °C and held for 120 min. Min curing reaction, produced self-lubricating fabric backing material.
利用玄武三号摩擦磨损试验机评估上述制得自润滑织物衬垫的摩擦学性能,在室温, 12.5 MPa条件下,于2.73m/s高速条件下摩擦系数和磨损率分别为0.1322,2.3×10-14m3·(N·m)-1。The tribological properties of the self-lubricating fabric liner prepared above were evaluated by the Xuanwu No. 3 friction and wear tester. -14 m 3 ·(N·m) -1 .
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