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摘要:
机器零部件的磨损是机器失效故障的主要原因，由磨损引发机械故障带来巨大经济损失，有必要开展机械设备的磨损检测. 磨粒检测技术通过磨粒的形状与图像分析，可以认知磨损的机理与磨损过程，实现视情维修，并且实现对机械零部件剩余寿命的预测. 本文中拟从磨粒的检测原理与方法、统计分析、几何分析、图像分割、图像识别与处理、在线铁谱技术与磨粒智能分析，对机械磨损的磨粒检测技术进展进行评述. 铁谱仪的原理有直读式铁谱仪、分析式铁谱仪、旋转式铁谱仪和在线铁谱仪. 基于磨粒的检测原理有铁谱技术、基于霍尔效应的磨粒检测、激光网检测、微流控检测技术、径向磁感应的磨粒检测、静电检测磨粒的方法、超声波反射检测磨粒的方法和并行共振激励检测等. 本文中介绍了铁谱技术的统计分析、几何形态分析、分形分析、图像分割研究、基于图像的铁谱分析、在线铁谱分析和铁谱的人工智能分析进展；另一方面，提出了机械磨损的磨粒检测技术存在的问题与挑战，提出了今后需要研究的问题. 基于机器视觉，自动分析磨粒的大小、边缘形状和表面纹理，得到磨粒的特征参数，用群理论分析磨粒的统计参数，减少对试验分析人员经验的依赖，实现更快、更准确的磨粒特征分析. 基于分形几何理论表征磨粒的几何形态，得到磨粒的尺度不变量. 逆分形分析技术是从小尺度到大尺度，可以对磨粒的几何形态提供新的表征信息. 采用三维磨粒的全信息检测技术，可以提取磨粒的三维几何特征. 针对磨粒几何形态的分形计算，引入粗糙集理论，来提高磨粒图像分割的精度与速度. 新的磨粒产生速率是衡量磨损变化趋势的有效参数，可以预测机械零件的剩余寿命. 两种或者多种检测原理的融合与集成，可以提高监测磨损的准确性，为机器的磨损故障预测提供更高的可信性. 此外，集成不同研究者各自开发的磨粒智能检测分析方法，研制机器磨损故障监测的软件包，实现基于磨粒信息的机械磨损的故障诊断与机械零件剩余磨损寿命的预测.
Abstract:The wear of mechanical parts and elements is the main reason of the failures of machines, and causes enormous economic loss as results of failures of mechanical wear. Thus, the operation conditions of equipment are monitored with respect to wear process and wear state. The wear mechanisms and the wear stages can be studied with the detection techniques in terms of wear debris, and the maintenance based on machine condition and the prediction of the remain service life of mechanical elements and parts can be achieved. The principles of wear debris detection, statistical analysis, morphological analysis, image segmentation and recognition and intelligent examine based on artificial intelligence were reviewed. The ferrography methods have direct reading ferrography, analytical ferrography, rotary ferrography and on-line ferrography. The principles of debris detection are classified as ferrography, Hall-effect, laser net fins, microfluidic detection, radial inductive sensor, electrostatic sensor, ultrasonic echo detection and detection method with parallel resonance structure. The state and the art of measurements using wear debris of above different principles were comparatively reviewed. On the other hand, the challenges and existed problems, which need studied further, of wear debris for detection of mechanical wear are proposed and presented. The automatic analysis of debris size, edge profile and surface texture based on machine vision would obtain its feature parameters. The statistical computation with group theory can avoid the dependence on experience of researchers, and achieve more efficient and accuracy analysis of debris features. The characterization of debris morphology with fractal theory can obtain their scale-invariant parameters, and the inverse fractal analysis from small scale to larger scale can provide new information for the debris morphology. The morphological feature extraction based on three dimensional view images for wear debris analysis can present full description of the wear debris. The introduction of the rough set theory to the fractal analysis debris morphology can improve the efficiency and accuracy of the segmentation of wear debris. The birth rate of new wear debris is an effective parameter to assess the wear stage and its tendency, with which remain service lives of mechanical elements can be predicted. The integration of different principal methods can improve the accuracy of wear monitoring, and provide more reliable prediction results for the wear failure of machines. Moreover, an exited problem and useful topic is the integration of the intelligent analysis methods presented by different researchers, and develop one software for the monitoring of wear failure of machines, which is a trend of monitoring method of mechanical wear. The final goals are the automatic failure diagnosis of mechanical wear based on the information of wear debris, and the prediction of remain service life of mechanical elements as results of mechanical wear.
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我国盾构机整机研制能力已达到世界先进水平，但是影响盾构机整机可靠性和安全性的主驱动密封关键核心零部件几乎全部依赖进口，核心技术被欧美国家垄断，加之受愈演愈烈俄乌战争局势和复杂多变国际形势影响，加剧了对国内盾构机企业关键核心零部件的封锁制裁[1-4]. 受制于关键零部件“卡脖子”问题，我国高端盾构机技术水平与国外仍存在较大差距，特别是国内缺乏高性能的主驱动橡胶密封件，表现在国产密封材料加工性能差，压变性和耐磨性不足，导致盾构机主驱动橡胶密封件长期依赖进口材料，严重制约了我国盾构机产业的高质量发展，危及盾构机产业安全[5-10].
大型盾构机主驱动橡胶密封件直径可达7 m以上，其截面是1种VD型异形密封结构，橡胶材料的加工性能在其精细结构成型过程中发挥着举足轻重的作用，而焦烧时间和门尼黏度是影响橡胶材料加工性能的关键因素[11]. 焦烧时间越短，加工过程中越容易发生橡胶早期硫化现象，导致密封件唇口精细结构处出现缺陷；门尼黏度反映橡胶加工性能的好坏和分子量高低及分布范围宽窄，黏度值高，表明橡胶分子量大，可塑性差. 在大型盾构机用异形密封圈的成型过程中，通常要求密封材料门尼黏度ML(1+4)<50，焦烧时间T10>150 s.
针对大型盾构机主驱动橡胶密封的成型工艺对丁腈橡胶加工性能的要求，本研究中以松明油、癸二酸二丁酯和固体古马隆树脂为原料，合成复合增塑剂；并使用高结构炭黑(每100 g炭黑的邻苯二甲酸二丁酯吸收值不低于110 mL)和低结构炭黑(每100 g炭黑的邻苯二甲酸二丁酯吸收值不高于70 mL)并用的补强体系，对NBR密封材料进行加工性能、物理机械性能和摩擦性能的宏观调控，结果表明改性后的NBR在兼具良好力学性能和耐磨性能的同时，加工性能得到显著改善，研制的NBR混炼胶焦烧时间T10可长达168.6 s，门尼黏度值ML(1+4)可低至46.95，满足了大型盾构机主驱动橡胶密封的成型工艺需求，可以推动国内盾构机主驱动密封用NBR复合材料的发展.
1. 试验部分
1.1 原料
丁腈橡胶N21购买于中国石油兰州石化公司；炭黑N220购买于江西黑猫炭黑股份有限公司；槽法炭黑购买于山东德蓝化工有限公司；过氧化二异丙苯(DCP)购买于上海凯茵化工有限公司；古马隆树脂购买于濮阳市恒泰石油化工有限公司；松明油(Pine Tar)购买于衡水帝亿石油化工有限公司；氧化锌、硬脂酸、2-硫醇基苯骈咪唑、2,2,4-三甲基-1,2-二氢化喹啉、癸二酸二丁酯、四甲基秋兰姆二硫化物、硫磺和N，N'-间苯撑双马来酰亚胺均购买于阿拉丁生化科技股份有限公司.
1.2 材料组成
基本组成：NBR (兰化 N21)100份，氧化锌5份，硬脂酸1份，炭黑N220 45份，槽法炭黑15份，2-硫醇基苯骈咪唑2.5份，2,2,4-三甲基-1,2-二氢化喹啉1份，古马隆树脂5份，癸二酸二丁酯2份，四甲基秋兰姆二硫化物1.5份，硫磺1份，过氧化二异丙苯2.5份，N，N'-间苯撑双马来酰亚胺1份. 改变松明油加入量，不同松明油(Pine ar)含量的橡胶材料样品编号列于表1中.
表 1 不同松明油使用量的丁腈橡胶配方设计Table 1. Formulation design of NBR with different amount of pine tarSample Content of pine tar/phr (weight parts per hundred parts of rubber) 1# 0.0 2# 0.3 3# 0.6 4# 0.9 5# 1.2 1.3 NBR硫化胶的制备
首先将烧杯放置在加热炉上，预热至50~80 ℃；加入固体古马隆树脂，升温至100 ℃使其熔化，然后再加入松明油和癸二酸二丁酯，搅拌直至三组份分散均匀；将加热炉缓慢升温到120 ℃，搅拌10~20 min后停止搅拌，将混合液体放置在室温下自然冷却至室温，得到粒状三组份复合增塑剂.
将密炼机预热至40 ℃后投入NBR生胶进行塑炼至生胶包辊，然后向密炼机依次投入三组份复合增塑剂、氧化锌、硬脂酸、炭黑N220、槽法炭黑、2-硫醇基苯骈咪唑和2,2,4-三甲基-1,2-二氢化喹啉，混炼20 min，将所述混炼后的橡胶从密炼机中取出，在室温条件下静置24 h，得到丁腈橡胶混炼胶. 将得到的混炼橡胶置于开炼机中，依次加入硫磺、四甲基秋兰姆二硫化物、过氧化二异丙苯和N,N’-间苯撑双马来酰亚胺，经打三角包3次和打卷3 次后出片，橡胶片在室温条件下静置24 h，得到混炼胶压延片. 将混炼胶压延片置入相应的模具，放入平板硫化机，在160 ℃和8 MPa条件下硫化，硫化时间为20 min，得到NBR硫化胶.
1.4 性能测试
硫化参数测试按照GB/T 1233-2008，采用橡胶加工分析仪(RPA, RPA 2000型, 美国 Alpha 科技有限公司)进行测定，设置测试压力为 10 MPa，角度为±0.5°.
门尼黏度按照 GB/T1232.1-2000，采用门尼黏度仪(MV, MV 2000型, 美国Alpha科技有限公司)进行测定，设置其测试时间为4 min，预热时间为1 min，温度为100 ℃.
硬度按照GB/T 531. 1-2008，采用邵氏A型硬度计进行测试，样品的尺寸为50 mm×50 mm×6 mm.
拉伸性能按照GB/T 528-2009中的1型试样，采用万能电子拉伸试验机(Shimadzu，AD-X，5 kN)进行测试，拉伸速率为500 mm/min.
压缩永久变形按照 GB/T 7759.1-2015中的方法进行测定，设置温度为100 ℃，保温时间为24 h.
耐磨性能即阿克隆磨耗按照GB/T 1689-2014，采用高温阿克隆磨耗试验机(GT-7012-AH1)进行测试.
摩擦系数按照GB/T 12444-2006，采用高速环块摩擦磨损试验机(MR-H3B型)进行测试，测试条件为载荷132 N，转速70 r/min，样品尺寸为12.32 mm×12.32 mm×19.05 mm，金属对偶为Φ 49.22 mm×13.06 mm尺寸及304不锈钢材质.
2. 结果与讨论
2.1 硫化参数和门尼黏度
采用橡胶加工分析仪(RPA 2000)以及门尼黏度仪(MV 2000)测试了NBR混炼胶的硫化参数和门尼黏度，如图1所示. NBR混炼胶硫化参数的测试结果列于表2中，由表2可看出，当NBR复合增塑剂中的松明油使用量少于0.9 phr时，NBR的焦烧时间T10和门尼黏度ML(1+4)呈现出显著的线性相关性，其中当松明油使用量由0 phr增加到0.9 phr时，T10由130.2 s增加到168.6 s，ML(1+4)由85.55降低到46.95. 图2所示为不同硫化参数的混炼胶加工成盾构机主驱动用VD密封圈唇口图片，由图2可以看出，1#NBR密封件唇口处有明显缺陷，而4#NBR密封件唇口处平整饱满，4#相比于1#，由于焦烧时间的延长和门尼黏度的降低，加工性能得到显著提升，能够满足主驱动VD型橡胶密封件唇口处精细结构的完整成型对橡胶材料加工性能的要求. 这主要是因为，在本研究中合成的三组份复合增塑剂中癸二酸二丁酯对古马隆树脂主体能够发挥溶胀作用，可以增加古马隆树脂中分子的自由体积，增强其分子链段的运动能力，提高橡胶加工时的柔韧性；同时黏稠的松明油中吸附的萜烃类物质可作为再生剂，其间的活性小分子能均匀渗透到古马隆树脂分子中间，使其溶胀，增加分子间的距离及氧的渗透，反应作用机理如图3所示，因此，三组份复合增塑剂在橡胶体系中的分散性和溶解性较高，制备的橡胶密封材料具有较长的焦烧时间和较低的门尼黏度.
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图 1 丁腈橡胶的硫化参数和门尼黏度：(a)丁腈橡胶的硫化曲线；(b)丁腈橡胶的门尼黏度；(c)松明油使用量对T10和ML(1+4)的影响；(d)松明油使用量对T90和(MH-ML)的影响Figure 1. Curing parameters and Mooney viscosity of NBR: (a) vulcanization curve of NBR; (b) Mooney viscosity curve of NBR; (c) effect of pine tar additive on T10 and ML(1+4); (d) effect of pine tar additive on T90 and(MH-ML)表 2 不同松明油使用量丁腈橡胶的硫化参数Table 2. Curing parameters of NBR with different pine tar contentSample T10/s T90/s MH/(dN·m) ML/(dN·m) MH-ML/(dN·m) ML(1+4) 1# 130.2 1 366.8 25.43 2.59 22.84 85.55 2# 142.2 1 202.4 23.95 2.18 21.77 75.18 3# 155.4 1 206.6 23.89 1.85 22.04 59.53 4# 168.6 1 237.2 23.94 2.24 21.70 46.95 5# 148.8 1 263.6 22.48 2.23 20.25 47.51 ![]()
图 2 盾构机用VD型NBR密封件局部图：(a) 1# NBR；(b) 4# NBRFigure 2. Partial drawing of VD type NBR seal for shield tunneling machine: (a) 1# NBR; (b) 4# NBR![]()
图 3 复合增塑剂合成路线及协同作用的机理Figure 3. Synthesis route and synergistic mechanism of composite plasticizer此外，橡胶体系中高结构炭黑和低结构炭黑并用，在填充时产生了颗粒互补效应，提高了胶料的分散度和分子链段的运动能力，延长了胶料在硫化过程中的可流动时间，即焦烧时间，也能够进一步改善胶料的加工性能.
2.2 力学性能
大型盾构机的主驱动密封工况严苛，为了防止密封泄露，要求橡胶密封材料能够承受较高的压强，因此，橡胶密封材料需具备优异的硬度、强度和回弹性. 橡胶材料的拉伸应力应变曲线如图4(a)所示，其具体的物理机械性能参数列于表3中，本研究中不同配方的NBR拉伸强度均大于21 MPa，相比于进口主驱动橡胶密封件材料的拉伸强度(14 MPa)，提升了50%以上. 主要原因是，在本研究中NBR补强体系采用颗粒较小的高结构炭黑和颗粒较大低结构炭黑并用，2种不同结构炭黑的颗粒之间在填充时发生互补，小的炭黑颗粒填充到了大的炭黑聚集体中间，且2种炭黑在分散过程中因表面活性不同促进了炭黑分散性，解决了炭黑容易聚集的难题，增大了炭黑与橡胶分子链之间的微观接触面积，提升了炭黑的补强效果，提高了橡胶材料的强度[12-13].
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图 4 丁腈橡胶的物理机械性能：(a)丁腈橡胶的应力应变曲线；(b)松明油使用量对硬度(邵A)和压缩永久变形的影响Figure 4. Physical and mechanical properties of NBR: (a) stress-strain curve of NBR; (b) effect of pine tar additive on hardness (Shore A) and compression permanent deformation在一定范围内，复合增塑剂中松明油的使用量对NBR强度[图4(a)]和压缩永久变形[图4(b)]影响较小，但随复合增塑剂中松明油的使用量由0 phr增加到1.2 phr，NBR硬度降低了9.5%[图4(b)]，拉断伸长率增长了59.3%，这是因为松明油中含有的有机酸基团，能够降低橡胶分子链间的作用力，提高胶料的黏着性. 此外，古马隆树脂虽然与橡胶的相容性良好，但因其软化点较高，在开炼机和密炼机中都难分散均匀，本研究中将古马隆树脂、松明油和癸二酸二丁酯预先混合制备成三组份复合增塑剂，能够有效降低古马隆树脂的软化点，既保持了三组份原有功能特性，同时又解决了古马隆软化点较高难分散均匀，松明油和癸二酸二丁酯配料困难等问题.
表 3 不同松明油使用量丁腈橡胶的物理机械性能Table 3. Physical and mechanical properties of NBR with different pine tar contentSamples Hardness (Shore A) Tensile strength/MPa Elongation at break/% Compression permanent deformation/% 1# 84 21.77 464.800 23.0 2# 84 22.83 499.000 22.5 3# 82 23.07 546.350 23.1 4# 81 22.51 684.368 22.7 5# 76 21.98 740.563 22.6 2.3 耐磨性能
橡胶材料的耐磨性能是影响盾构机主驱动密封系统寿命和可靠性的关键因素[14-19]. 本研究中通过摩擦系数、磨损率和不同温度下的阿克隆磨耗量和磨损形貌对比分析了三组份复合增塑剂中不同松明油使用量对NBR耐磨性能的影响. 图5(a)所示为不同含量松明油改性NBR的摩擦系数随时间的变化关系图，图5(b)所示为不同配方NBR的摩擦系数和磨损率，随着复合增塑剂中松明油含量的增加，NBR的摩擦系数和磨损率均先降低再升高，在132 N和70 r/min的条件下，与无松明油添加的1#相比，4#的摩擦系数从0.770降低至0.655，降低了14.9%；4#的磨损率从1.6×10−7 cm3/(N·m)降低至6.8×10−8 cm3/(N·m)，降低了57.6%，但当松明油添加量超过0.9 phr时，NBR的摩擦系数和磨损率均大幅度上升. 采用SEM对NBR样品磨损表面微观形貌进行分析，如图6所示，1#和2#摩擦接触表面在交变接触压应力的作用下，循环应力的应力幅超过材料的弹性极限，导致材料表面因疲劳损伤而引起磨损，出现裂纹；当复合增塑剂中松明油添加量在0.6~0.9 phr时，样品表面只有轻微磨痕，无明显磨损，耐磨性能较好；当复合增塑剂中松明油添加量超过0.9 phr时，古马隆树脂在松明油和癸二酸二丁酯的协同作用下，软化点过低，导致胶料的黏着性过高，在摩擦力作用下2个相对滑动的摩擦表面发生塑性变形，橡胶表面和对偶表面发生黏着，橡胶表面因强度较低发生剪切破坏，耐磨性能变差.
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图 5 丁腈橡胶的耐磨性能：(a)丁腈橡胶的环块摩擦试验曲线；(b)丁腈橡胶的摩擦系数和磨损率Figure 5. Abrasion resistance of NBR: (a) ring friction test curve of NBR; (b) friction coefficient and wear rate of NBR![]()
图 6 不同配方丁腈橡胶的环块磨损形貌的SEM照片：(a) 1#；(b) 2#；(c) 3#；(d) 4#；(e) 5#Figure 6. SEM micrographs of wear morphology of ring blocks with different formulations of NBR: (a) 1#; (b) 2#; (c) 3#; (d) 4#; (e) 5#在盾构机实际运行工况中，NBR密封材料的工作环境温度可高达90 ℃，因此本研究中开展了不同温度下的阿克隆磨耗试验，研究了不同温度以及极限温度环境对NBR摩擦磨损性能的影响. 图7所示为不同温度下NBR阿克隆磨耗量的变化趋势，阿克隆磨耗量列于表4中，可以看出，相比于室温条件下NBR的阿克隆磨耗量，60 ℃时NBR的阿克隆磨耗量增幅很小，仅约1%；在90 ℃时，NBR的阿克隆磨耗量相比于室温NBR的阿克隆磨耗增长率约9%，在室温~90 ℃的温度范围内，5种配方NBR的阿克隆磨耗量较平稳，说明材料的耐热性能好，化学稳定性高. 其中4#样品在不同温度下的阿克隆磨耗量皆最小，图8所示为4#样品在不同温度下阿克隆磨耗试验后形貌的SEM照片，可以看出：在室温~90 ℃时，4#样品表面无明显磨损，耐磨性能较好，这主要是因为，在本研究中合成的三组份复合增塑剂中，松明油中含有的松节油是1种天然精油，是以蒎烯为主的多种萜烃类的混合物，有特有的化学活性，其间的活性小分子能均匀渗透到古马隆树脂分子中间，使其溶胀，增加分子间的距离及氧的渗透，在摩擦过程中能够在硫化胶表面形成润滑膜而产生自润滑效果；但当松明油的使用量超过0.9 phr时，在硫化的高温条件下和古马隆树脂分子黏附在一起，使得橡胶分子无法分散均匀，并且会在橡胶分子表面变成黏流态，摩擦表面由于黏附作用使材料堆积变形发生黏着磨损，耐磨性能变差，磨耗量增加.
表 4 不同温度下NBR的阿克隆磨耗量Table 4. Akron wear value of NBR at different temperaturesSamples Akron wear value of NBR/(cm³/1.61 km) Room temperature 60 ℃ 90 ℃ 1# 0.116 1 0.116 3 0.121 3 2# 0.114 0 0.114 9 0.120 7 3# 0.110 8 0.110 9 0.120 2 4# 0.107 1 0.109 1 0.117 6 5# 0.116 5 0.117 4 0.126 8 ![]()
图 7 不同温度下NBR阿克隆磨耗量的变化趋势Figure 7. Change trend of NBR Akron attrition at different temperatures![]()
图 8 4#样品在不同温度下的阿克隆磨耗试验磨损形貌的SEM照片：(a)室温；(b) 60 ℃；(c) 90 ℃Figure 8. SEM micrographs of Akron wear morphology of 4# at different temperatures: (a) room temperature; (b) 60 ℃; (c) 90 ℃本研究中开发的NBR密封材料已经制备成密封件，在盾构机主驱动密封试验台上开展了模拟密封工况下(密封最大压力：1.0 MPa；密封最大压差：0.1 MPa；主驱动轴最大线速度：3.0 m/s；轴径：2.0 m；密封介质：HBW黑油、EP2黄油和320齿轮油)的密封性能考核，考核结果表明NBR密封件能够实现盾构机运行工况下的有效密封，可以满足盾构机掘进长度大于4 km和等效工作天数大于400天的密封寿命要求. 研制的NBR密封材料能够满足目前国内大型盾构机对主驱动密封件的需求.
3. 结论
a. 以古马隆树脂、癸二酸二丁酯和松明油制备的复合增塑剂在橡胶体系中的分散性和溶解性较高，制备的NBR橡胶密封材料具有较长的焦烧时间和较低的门尼黏度，加工性能优异.
b. 松明油能降低固体古马隆树脂的软化点，通过复合增塑剂中三组分的协同作用，能够有效提高橡胶材料的拉断伸长率，增强橡胶材料的柔韧性.
c. 复合增塑体系中加入0.9 phr松明油时，NBR弹性体的摩擦系数和阿克隆磨耗量低，耐磨性能优异，且该材料的耐磨性能在盾构机主驱动模拟试验台中也进行了验证，可以满足盾构机主驱动系统对密封有效性和寿命的需求.
d. 本文中制备的高性能NBR密封材料，在兼具高强度、高韧性、高回复性、高耐热与高耐磨性的基础上，还满足大型盾构机的成型工艺要求，为大型盾构机主驱动密封的设计制备提供材料支撑.
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