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DIAGNOSIS OF CAUSES OF FAILURE OF COMPONENTS AND SUBASSEMBLIES OF CHEMICAL EQUIPMENT M. B. Chizhmakov and M. B. Shapiro UDC 66.023:620.193:660.077 A diagnosis of the character and causes of failure of the chemical industry equipment working at high temperatures and pressure, under the action of aggressive media, requires the adoption of contemporary methods of the physicochemical investigation of metals. A correct determination of the causes of failure of components and subassemblies of the chemi- cal equipment makes possible for the designer to follow whether the structural material chosen by him and the calculation method of the equipment are suitable for the service con- ditions. The technologist, using these results, can introduce changes in the technological pro- cess of equipment manufacture, if the cause of failure was the deviation from the recommended technology or imperfect technology. For the users the investigation results of the causes of failure make it possible to arrive at conclusions concerning the methods of operation and the process parameters. In addition an analysis of the character and causes of failure of machines and equipment makes possible to predict their service life. As an investigation of the causes of equipment failure in the chemical industry of one of the foreign firms, failure of material takes place above all on account of local corrosion \[i\]. An analysis of equipment failure has shown that 27.5% is caused by general corrosion, 23.7% by corrosion cracking, 14.6% by intercrystalline corrosion and corrosion of welds, 14.3% by pitting corrosion, and 13% by other types of corrosion. In addition in \[i\] it is noted that the relative level of material damage by corrosion of the equipment metal is 2~ times higher than the average level in the entire sphere of metal use. It should be noted that in many cases the determination of the type and causes of failure of the base metal and welds of the chemical industry equipment is very difficult and requires a complex approach for solving this problem. In a complex examination of the metal of a damaged apparatus, it is possible to determine the main cause of failure and factors contributing to it. The direction of the investigation and selection of the appropriate methods are determined by the features of the material failure and the operating conditions of the equipment. The investigation should be started by a visual examination of the damaged equipment in order to determine the location of failures, corrosion damage, existence of cracks, etc. It is useful to set up a scheme of the equipment failure~ It is also useful to familiarize oneself with the technical documentation, and work scheme in order to detect possible devia- tions in the operation conditions of the equipment. In many cases it is necessary to deter- mine the chemical composition of steel and its agreement with GOST; here attention should be paid to the content in steel of harmful additions and gases. It is necessary to check the mechanical properties of the metal in order to establish an agreement between the properties and the technical norms. In the material being investigated, it is necessary to determine the level of residual stresses, which are dangerous in the case of corrosion cracking, corrosion fatigue, and also in the case of a complex stressed state. In addition, it is possible to carry out color radiography of damaged subassemblies and parts which makes possible to detect cracks in the metal and the character of their location and also to obtain important information on the type of metal damage. Defectoscopy of the metal is necessary when the fracture of the part changes as a result of corrosion damage in interaction with the aggressive medium. A metallographic investigation of the metal structure yields valuable information, since in service important changes can take place in the metal structure caused by re- crystallization processes when the apparatus works at elevated temperatures. An analysis 1989. Translated from Khimicheskoe i Neftyanoe Mashinostroenie, No. 12, pp. 33-34, December, 0009-2355/89/1112- 0719512.50 9 1990 Plenum Publishing Corporation 719 of the microstructure makes it possible to detect the metallurgical defects (the presence of non-metallic inclusions, sigma phase, ferrite, etc.) as well as the defects of welds. Metallographic investigations are also important in determining the failure caused by inter- crystalline corrosion or by corrosion cracking, since this makes possible a unique determina- tion of the fracture character. However, in many cases for determining the causes of failure of chemical industry apparatus, components, and subassemblies it is necessary to use modern physical investigation methods. One of the most effective methods for the investigation of failure is fractographic analysis which is realized by the raster or transmission electron microscopy method~ The fractographic method can be used for detecting brittle failure and its connection with crystallographic planes or interphase boundaries of structural components~ In the case of ductile fracture the pitting relief or the zone of stretching on the fracture is determined by the fractographic method. In the case of fatigue fracture an analysis is carried out of the fatigue grooves or track traces. A detailed fractographic analysis provides valuable information on the fracture type. By means of the fractographic analysis it is possible to determine the fracture source and the crack propagation trajectory. By the fractographic method is determined also the degree of action of the aggressive medium or hydrogenation on the fracture process. In addition, the features of the fracture structure give additional information on the charac- ter of failure. Thus, a typical feature of the fracture under the action of a constant load is the existence on the fracture surface of a large number of cracks. In ductile fracture the shape of pits is largely determined by the character of the loads applied. A wide scatter of pits with regard to dimensions shows the nonuniformity of the structure of the material being examined. The intercrystalline character of frac- ture, when the corrosion products are absent on the fracture, suggests the segregation of harmful contaminants on the grain boundaries or the existence of film separations on them. A mixed surface relief containing intergranular failure and another type of relief suggests a nonuniformity of harmful contaminants on the grain boundaries. The presence of corrosion products on the surface of the intergranular fracture indi- cates cracking of the metal as a result of corrosion under stress. There are several other signs which permit, from the details of the fracture relief, determination of the features of external factors (stress, medium, etc.) leading to material failure. An analysis of the data on the type of fracture obtained by the fractographic method makes it possible in most cases to determine the special features of metal fracture and the causes of failure of parts and subassemblies of the chemical equipment. However, there are also cases when the fractographic method gives incomplete information on the cause of metal failure and only a general picture of the failure topography~ Besides, the character of failure is often affected by structural changes accumulating in service, i.e., recrys- tailization, separation of dispersed excess phases, changes in the density and the character of the distribution of dislocations, etc. In this case information on the type and possible causes of failure can be obtained by means of transmission electron microscopy~ For the diagnosis of the causes of failure of the chemical industry apparatus, sub- assemblies, and parts local methods of microanalysis, such as x-ray spectral analysis and Auger-spectroscopy are being used successfully. These methods permit a microanalysis of very small volumes of metal. Thus, with the x-ray spectral analysis method it is possible to determine the composition of the matrix and inclusions, the degree of nonuniformity of the distribution of elements in the specimen being examined, and to carry out a topographi- cal analysis of the character of element distribution, the composition of corrosion products by the interaction of metal and the aggressive medium. In addition, this method can be used to determine the composition of surface films on corrosion-resistant steels and alloys. Auger-spectroscopy also permits solving these problems and in addition determining the presence of segregation of harmful contaminants on grain boundaries, establish the areas of local composition changes, impoverishment by chromium near the carbides or the grain boundaries, as well as determining the composition of fine inclusions (less than i ~m) in steels and alloys. 720 In addition to the microanalysis methods described above, for the investigation of the damaged apparatuses other methods can be used (x-ray photoelectron spectroscopy, secondary ion mass spectrometry, laser mass spectrometry, etc.). However, in most cases they are less effective than the x-ray spectral analysis or Auger-spectroscopy. Thus, on the basis of these considerations the following sequence can be recommended for determining the causes of failure of parts and subassemblies of the chemical industry taking into account the fractographic analysis described in \[2\]. i. Construction of the failure scheme with detection of the fracture source, struc- tural stress concentrators, and presence of signs of surface damage. 2. Determination of the agreement between the part dimensions and specifications of the drawing, and between the chemical composition and mechanical properties of the metal and the technological conditions. This permits checking not only the correctness of heat treatment, but also the maintenance of equipment operation in work at elevated temperatures. 3. Determination of fracture orientation in relation to the direction of the action of the principal stresses. 4. Determination of the type and degree of the macroplastic strain and its localiza- tion as a whole and in the vicinity of the fracture. 5. Determination of the type of failure in the fracture, i.e., plastic, brittle, fatigue, intercrystalline, transcrystalline; existence of signs of intercrystalline cor- rosion, corrosion cracking, and pitting. 6. Determination on the fracture surface of sharply distinguished macroscopic areas, differinginstructure and color, indicating the duration of failure in time, as well as other macroscopic signs, i.e., cuts, steps, fatigue grooves, etc. 7. Exposure on the fracture of corrosion products, oxides and others, and their con- nection with the source of failure. 8. Exposure of cracks close to and away from the fracture, evaluation of their loca- tion, number, and direction. 9. Investigation of the macro- and microstructure of the metal, their agreement with the given semifinished product, detection of structure faults, often a stonelike fracture, presence of ferritic phase in austenitic steels and of the sigma-phase in austenitic and austenitic-ferritic steels. I0. Use of microanalysis methods for the identification of nonmetallic inclusions present in the source of the fracture of inclusions on which micropores are formed in duc- tile fractures, and also segregations along the grain boundaries and film segregations. ii. Study of the fine structure (distribution of dislocations, packing defects) for exposure of changes appearing in the material of the equipment in service. In a number of cases, for example, for the equipment from austenitic or austenitic-ferritic steel it is useful to determine whether in the material appears a tendency to intercrystalline cor- rosion as a result of long service at elevated temperatures. Examples of a complex investigation of failure of components and subassemblies of chemical equipment in particular using fractographic analysis are given in \[3-5\]. It should be noted that each work concerned with thedetermination of the causes of failure of equipment in service conditions is a separate investigation. Accumulation and systematization of experience in the field of diagnostics of the character and causes of failure of parts and subassemblies of equipment, and statistical processing of results, are important tasks of materials scientists, corrosion specialists, technologists, and designers in the field concerned. This work must be carried out in the institutes of the relevant field, familiar with the special operational features of the equipment. It is necessary to increase work on the diagnostics of equipment failure. An important role shold here be attached to the equipment of scientific research institutes and laboratories, and to exchange of experience between the institutes of the relevant fields. I. LITERATURE CITED Ya. M. Kolotrykin, Metal and Corrosion \[in Russian\], Metallurgiya, Moscow (1985). 721 . 3. 4. 5~ To A. Gordeeva and I. P. Zhegina, Analysis of Fracture in Assessing the Reliability of Materials \[in Russian\], Mashinostroenie, Moscow (1978). Mo B. Chizhmakov and M. B. Shapiro, Use of Contemporary Physical Methods for the Investigation of Corrosion-resistant Steels and Alloys \[in Russian\], TsINTIKhImnefte- mash, Moscow (1986). M. B. Shapiro, Yuo P. Surkov, M. B. Chizmakov, and A. L. Belinskii, "Investigation of the failure of water heating pipes in ammonia manufacture," Khim. Neft. Mashinostro, 30-32 (1978). Fractography and Atlas of Fractograms. Reference Book \[in Russian\], Metallurgiya, Moscow (1982)o 722
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化工設(shè)備組件，子組件失效的原因診斷
M. B. Chizhmakov and M. B. Shapiro
UDC 66.023:620.193:660.077
在高溫和壓力下以及腐蝕性介質(zhì)的作用，化工設(shè)備發(fā)生故障的性質(zhì)和原因的診斷需要采取金屬的物理化學(xué)調(diào)查的當(dāng)代方法。正確確定化工設(shè)備零部件失效的原因使設(shè)計師能夠根據(jù)所選擇的材料結(jié)構(gòu)和設(shè)備計算方法是否滿足使用條件。
對于技師來說，如果失效是因為使用的技術(shù)或不完善的技術(shù)偏差引起的，那么技師利用這些結(jié)果，可以改變設(shè)備制造工藝。對于用戶來說，失效的原因的調(diào)查結(jié)果，使人們有可能得到有關(guān)的操作方法和工藝參數(shù)的結(jié)論。此外，機器和設(shè)備故障的性質(zhì)和原因的分析，可以預(yù)測其使用壽命。
正如對化工行業(yè)一家外國公司所進行的設(shè)備故障的原因調(diào)查，由于局部腐蝕引起的材料失效占大部分，設(shè)備故障的分析表明，全面腐蝕的占27.5％，腐蝕開裂的占23.7％，晶間腐蝕，焊縫腐蝕的占14.6％，點蝕的占14.3％，其他類型的腐蝕占13％，此外，據(jù)悉，金屬設(shè)備腐蝕的物質(zhì)損失水平比整個領(lǐng)域金屬損失的平均水平高出2.8倍以上。
應(yīng)當(dāng)指出的是，在許多情況下確定基本金屬及化工設(shè)備的焊接失效類型和原因是非常困難的，需要復(fù)雜的方法解決這個問題。損壞設(shè)備的金屬的檢查很復(fù)雜，但確定失效的主要原因是可能的。調(diào)查的方向和選擇適當(dāng)?shù)姆椒ㄊ怯刹牧鲜Ш驮O(shè)備的經(jīng)營狀況的特點決定的。
為了確定故障、腐蝕損壞，裂縫的存在的位置等，調(diào)查應(yīng)當(dāng)由目視檢查損壞的設(shè)備開始。為了檢測設(shè)備的運行狀況可能出現(xiàn)的偏差，作一個設(shè)備故障的記錄表并且熟悉自己的技術(shù)資料和工作計劃是有用的。確定鋼的化學(xué)成分和其與GOST認(rèn)證協(xié)議在許多情況下是必要的；這里應(yīng)注意鋼的失效和鋼中氣體的含量。檢查金屬的機械性能，以便建立一個之間的性能和技術(shù)規(guī)范的協(xié)議，這是必要的。
在被調(diào)查的材料中，有必要確定殘余應(yīng)力的大小，它在腐蝕開裂，腐蝕疲勞的情況下很危險，復(fù)雜應(yīng)力狀態(tài)也如此。此外，可以對損壞的零部件進行彩色照相，這就有可能檢測金屬裂縫和它的位置，還獲得金屬損害類型的重要信息。零件部分?jǐn)嗔褜?dǎo)致腐蝕破壞與介質(zhì)的侵蝕相互作用，因此金屬探傷是必要的。
金屬結(jié)構(gòu)的金相調(diào)查產(chǎn)生有價值的信息，當(dāng)設(shè)備在高溫下工作時，由于重結(jié)晶過程，會引起工作過程中金屬結(jié)構(gòu)發(fā)生重要的變化。
分析微觀結(jié)構(gòu)能夠檢測冶金缺陷（非金屬夾雜物的存在，σ相，鐵素體等）以及焊縫的缺陷。在確定由晶間腐蝕還是由腐蝕開裂導(dǎo)致失效時金相調(diào)查也很重要，因為這可能出現(xiàn)可以唯一確定斷裂的特征。
然而，在許多情況下，確定化工儀器、部件和組件失效的原因時使用現(xiàn)代物理的調(diào)查方法是必要的。
調(diào)查失敗的最有效的方法之一是斷口分析，這是通過柵格或透射電子顯微鏡法實現(xiàn)的。斷口的方法可用于檢測脆性破壞以及其與晶面或結(jié)構(gòu)部件的相間邊界的連接。
在韌性斷裂腐蝕或斷裂拉伸區(qū)的情況下，由分析斷口的方法確定。在疲勞斷裂的情況下分析疲勞槽或軌道痕跡。詳細的斷口分析為判斷斷裂類型提供有價值的信息。
通過斷口分析，能夠確定斷裂源和裂紋擴展軌跡。由斷口的方法確定侵蝕介質(zhì)或斷裂過程氫化的程度。此外，斷裂結(jié)構(gòu)的特點，提供了更多失效的信息。因此，在恒定負載下的作用下，斷裂的一個典型特征是斷口表面存在大量的裂縫。
韌性斷裂坑的形狀在很大程度上取決于所施加的載荷性質(zhì)。廣泛分散的坑的尺寸顯示了正在檢查的材料結(jié)構(gòu)的不均勻性。當(dāng)斷裂時沒有腐蝕產(chǎn)物，晶間斷裂的特點表明晶界偏析的有害污染物由于膜的存在被分離?；旌媳砻婧芯Ч收虾土硪环N類型表明在晶界上的有害污染物的不均勻性。
晶斷裂表面存在腐蝕產(chǎn)物表明金屬的開裂是由于應(yīng)力腐蝕。從斷裂過程的細節(jié)來看有幾個其他的跡象能夠確定導(dǎo)致材料失效的外部因素（壓力，介質(zhì)等）
的特點。
通過對由斷口的方法獲得的關(guān)于斷裂類型的數(shù)據(jù)分析使得它在大多數(shù)情況下，能夠確定金屬斷口的特點和化工設(shè)備零部件失效的原因。然而，有時斷口的方法不能完全確定金屬失效的原因而只有失效情況的大致圖片。另外，失效的特點常受使用過程中積累的結(jié)構(gòu)變化的影響，即重結(jié)晶，分散過剩的階段的分離，密度變化，位錯分布特征等。在這種情況下，失效的類型和可能的原因可以通過透射電子顯微鏡獲得。
對于化工設(shè)備失效原因診斷的零部件微量法正在成功使用，如X-射線譜和俄歇光譜分析。這些方法需要微量體積很小的金屬的。因此，使用X射線譜分析方法能夠確定基質(zhì)和夾雜物的組成，待檢測試樣中的元素分布不均勻程度以及進行的元素分布特征的分析和由金屬和侵蝕介質(zhì)的相互作用組成的腐蝕產(chǎn)物。此外，這種方法可以用來確定耐腐蝕鋼和合金表面薄膜的組成。
俄歇光譜也可以解決這些問題，除了確定存在晶界上的有害污染物分離，建立局部成分變化的面積，碳化物或晶界附近鉻的缺乏以及確定鋼和合金的細夾雜物（少于1微米）的組成。
損壞儀器的調(diào)查除了以上所述的微量方法，可以使用其他方法（X射線光電子能譜，二次離子質(zhì)譜質(zhì)譜，激光等）。然而，在大多數(shù)情況下，它們不如X-射線譜分析或Auger光譜有效。
因此，按下列順序在這些因素的基礎(chǔ)上結(jié)合[2]中描述的斷口分析可以確定化工設(shè)備零部件故障的原因。
1. 通過檢測斷裂源，結(jié)構(gòu)的應(yīng)力集中，表面存在的損傷跡象建立失效的圖表
2. 確定零件的尺寸和繪圖規(guī)格，金屬的化學(xué)成分與力學(xué)性能和工藝條件之間的要求，這樣不僅檢查了熱處理的正確性，也保證了高溫條件下工作設(shè)備的維修。
3. 確定斷裂時主應(yīng)力的作用方向。
4. 確定宏觀彈性應(yīng)變以及其局部作為一個整體在斷裂附近的的類型與程度。
5. 確定斷裂故障類型，即，彈性變形，脆性變形，疲勞，沿晶，穿晶；存在晶間腐蝕，腐蝕開裂，點蝕的跡象。
6. 確定斷裂面在結(jié)構(gòu)和顏色以及其他宏觀的跡象上的不同，即斷口，疲勞槽等，說明了故障的持續(xù)時間。
7. 找出斷裂的腐蝕產(chǎn)物，氧化物和其他物質(zhì)，以及它們與失效原因的關(guān)系。
8. 找出接近和遠離斷口的裂縫，確定它們的位置，數(shù)量和方向。
9. 檢查金屬的宏觀和微觀結(jié)構(gòu)，對給出的半成品的意見，檢測結(jié)構(gòu)故障，往往是一個石頭狀斷口，存在奧氏體鋼鐵素體相、西格瑪相奧氏體鐵素體相和奧氏體 - 鐵素體鋼。
10. 使用微量分析法鑒定非金屬夾雜物，呈現(xiàn)斷裂中夾雜物的來源，韌性斷裂中形成微孔，也存在沿晶界和膜偏析物，
11. 研究精細結(jié)構(gòu)（位錯分布，包裝缺陷），從而找出工作中設(shè)備材料中出現(xiàn)的變化。例如，在許多情況下，對于奧氏體或奧氏體 - 鐵素體鋼設(shè)備，確定長期在高溫下工作材料是否有晶間腐蝕的傾向很有用。
復(fù)雜化工設(shè)備的零部件的故障調(diào)查，通常利用斷口分析[3-5]。
應(yīng)當(dāng)指出的是，在使用條件下，確定設(shè)備故障原因相關(guān)的每項工作都是一個獨立的調(diào)查，診斷領(lǐng)域的設(shè)備零部件故障的原因經(jīng)驗的積累和系統(tǒng)化和結(jié)果的統(tǒng)計處理，是材料科學(xué)家，腐蝕專家，技術(shù)人員在，以及在相關(guān)領(lǐng)域的設(shè)計師的重要任務(wù)。這項工作必須在相關(guān)領(lǐng)域機構(gòu)開展，從而熟悉設(shè)備的特殊操作特點。增加設(shè)備的故障診斷工作很有必要。這里需要附加一個重要的角色，即重視科研院所和實驗室設(shè)備以及相關(guān)領(lǐng)域的研究機構(gòu)之間的經(jīng)驗交流。