CN104142292B - A method for high temperature corrosion tests and characterization of power plant boiler superheater tubes - Google Patents

A method for high temperature corrosion tests and characterization of power plant boiler superheater tubes Download PDF

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CN104142292B
CN104142292B CN201410381675.5A CN201410381675A CN104142292B CN 104142292 B CN104142292 B CN 104142292B CN 201410381675 A CN201410381675 A CN 201410381675A CN 104142292 B CN104142292 B CN 104142292B
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corrosion
high temperature
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depth
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侯世香
顾威
刘东雨
周荣灿
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华北电力大学
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一种用于电站锅炉过热器管高温腐蚀实验及表征的方法,属于高温应力腐蚀技术领域。 A method for high temperature corrosion test and characterization of power boiler superheater tubes for high temperature belonging to the technical field stress corrosion. 选择用于锅炉过热器管的同种金属材料,根据材料所受应力大小确定试样尺寸及精度,通过精加工制备具有一定公差范围的圆筒和圆棒,将圆筒和圆棒装配在一起时产生一定的过盈配合,能保证产生所需要的应力。 For the same kind of metal material selected boiler superheater tubes, the material according to the stress size and sample size determination accuracy, with a certain tolerance range by preparing and finishing a cylindrical rod, the cylindrical rod and fitted together when a certain interference fit, to ensure desired stress generated. 对试样进行高温腐蚀后,统计一定腐蚀条件下试样的非均匀腐蚀深度,然后通过矩估计法估算出最大腐蚀深度,以此为依据表征非均匀腐蚀的程度,对高温腐蚀后的试样进行非均匀腐蚀程度的评价。 After the high temperature corrosion on the specimen, a non-uniform etching depth statistical sample under certain etching conditions, and then estimated by Monent the maximum corrosion depth, as a basis of the degree of non-uniform corrosion characterization, a sample after the high temperature corrosion non-uniform corrosion degree evaluation. 根据实验结果对过热器管材料在高温腐蚀环境及应力状态下的适用性进行评价。 To evaluate the applicability of the superheater tube material at a high temperature corrosive environment and stress states based on experimental results. 本发明的制备方法简单,成本低,适用于锅炉过热器管的高温应力腐蚀实验。 The preparation method is simple, low cost, suitable for high-temperature stress corrosion test boiler superheater tubes.

Description

一种用于电站锅炉过热器管高温腐蚀实验及表征的方法 A method for high temperature corrosion tests and characterization of power plant boiler superheater tubes

技术领域 FIELD

[0001] 本发明属于高温应力腐蚀技术领域,具体涉及一种用于电站锅炉过热器管高温腐蚀实验及表征的方法,用于电厂锅炉过热器管在高温腐蚀环境下的应力腐蚀实验方法及非均匀腐蚀程度的评价方法。 [0001] The present invention belongs to the technical field of high-temperature stress corrosion, particularly relates to a power plant boiler superheater tubes in a high temperature corrosive environment and non-stress corrosion test method and characterization of a method for high temperature corrosion test power boiler superheater tubes used for method to evaluate the degree uniform corrosion.

背景技术 Background technique

[0002] 在电厂中,电站锅炉四管(过热器管、再热器管、省煤器管、水冷壁管)的安全运行, 是保证电站正常运行的先决条件。 [0002] In the power plant, power plant boiler four (superheater tubes, reheater tubes, economizer tubes, the waterwall tubes) safe operation is to ensure the normal operation of the plant prerequisite. 这些管道长期处于高温水或水蒸气的压力和煤燃烧环境中,因此需要有较好的高温组织稳定性,同时具有较高的持久强度和耐高温腐蚀性能,尤其是过热器和再热器管道。 These long-term high-temperature water pipes or water vapor and coal combustion pressure environment, thus the need for good high temperature structural stability while having a high rupture strength and high temperature corrosion, especially superheaters and reheater tubes . 过热器管是在一定的应力状态、一定的温度和一定的腐蚀环境中服役的。 Superheater tubes are in constant state of stress, a temperature and a certain corrosive environment serving. 常用的过热器管一般为珠光体耐热钢、马氏体耐热钢和奥氏体耐热钢,如新型9% ~12%0、了91、了92、冊3(:、了?304!^?347!1和5卯61304!1,以及一些镍基高温合金如111(3〇1161 617、Inconel 690、Inconel 671 等。 Common superheater tubes typically pearlitic heat resistant steel, martensitic steel and austenitic heat-resistant steel, such as the new 9% to 12% 0, 91, 92, Volume 3 (:, the? 304 ! ^? 347! 61304 1 and 5 d! 1, as well as some nickel-base superalloy such as 111 (3〇1161 617, Inconel 690, Inconel 671 and the like.

[0003] 过热器管外壁长期暴露在煤燃烧环境中,受到煤灰和烟气腐蚀。 [0003] superheater tube wall prolonged exposure to the environment in coal combustion, coal ash and flue gas by corrosion. 管道材料在使用前通常要进行一定腐蚀条件下的模拟实验,从而对材料的适用性进行评价。 Piping material before use is usually carried out simulation under certain etching conditions, so that the applicability of the material were evaluated. 实验室中,通常是对煤粉锅炉中的成灰条件进行还原,但高温腐蚀与金属管所受的应力及壁温的关系密切,应力越大、壁温升高,腐蚀加重,这些在实验室模拟时都不能得到充分的还原,使评价结果与实际工况不符。 Laboratory, typically pulverized coal boiler ash reduction conditions, but the high temperature corrosion of the metal tube wall temperature and the stress applied is closely related to the greater stress, the wall temperature rise, increased corrosion, these experiments can not be sufficiently reduced when the simulation chamber, so that the evaluation does not match the actual conditions.

[0004] 过热器管的高温腐蚀,是管内蒸汽压力和管外向火侧的煤灰/烟气腐蚀的共同作用。 [0004] The high temperature corrosion of superheater tubes, the combined effect of the steam pressure in the pipe and ash / flue gas corrosion outgoing fire side. 现有的高温腐蚀实验,是在没有应力下的纯高温腐蚀,或通过应力环对金属材料进行加载的腐蚀;这些无法保证载荷的精确度及高温时应力的恒定。 Conventional high temperature corrosion test, pure elevated temperature in the absence of stress corrosion or corrosion of metallic material by loading stress ring; which can not guarantee the accuracy and high temperature when a constant stress load. 所用的煤灰也是模拟的合成煤灰,与实际煤灰有一定的差距。 The ash is also used synthetic analog of coal ash, the actual coal ash has a certain gap.

[0005] 另外,高温腐蚀动力学研究中,通常采用氧化增重或增厚作为评定腐蚀程度的指标,忽视了高温腐蚀存在点蚀或沿晶界腐蚀的现实。 [0005] In addition, high temperature corrosion kinetics, the weight gain by oxidation or commonly used as a measure of the degree of thickening of corrosion index, ignoring the presence of the real high temperature corrosion pitting or corrosion along the grain boundaries. 因此高温腐蚀程度的表征需要把不均匀腐蚀的局部性和严重性表示出来。 Thus the degree of high temperature corrosion of the non-uniform corrosion characterization requires locality and severity represented.

[0006] 目前,常规的应力腐蚀实验方法存在以下不足: [0006] At present, there is insufficient conventional stress corrosion test methods:

[0007] 1、利用应力环加载,无法保证载荷的精确度及高温时应力的恒定; [0007] 1, using the hoop stress load, can not ensure a constant stress when accuracy and high-temperature load;

[0008] 2、不同材料间常温下产生的应力,高温时会发生变化,常温下的应力腐蚀实验结果,与高温下的应力腐蚀环境相差很多,不能有效地评价材料的适用性,导致实验结果产生误差; [0008] 2, stress generated between the different materials at room temperature, it varies when the temperature, the stress corrosion test results at room temperature, and the stress corrosion at a high temperature environment a lot of difference, can not effectively evaluate the suitability of the material, leading to results generating an error;

[0009] 3、过热器管材的高温腐蚀,是在管内蒸汽压力作用下的高温应力腐蚀,现有的高温腐蚀评价是在没有应力下的纯高温腐蚀或利用应力环加载; [0009] 3, the high temperature corrosion of superheater tubes, stress corrosion at high temperatures under the vapor pressure tube, a conventional high temperature corrosion is evaluated in the absence of a pure high temperature corrosion or stress using stress loading ring;

[0010] 4、锅炉管的高温腐蚀实验中,所用的煤灰是模拟的合成煤灰,与实际煤灰有一定的差距; [0010] 4, the high temperature corrosion test tube boiler, coal ash is used in the synthesis of an analog of ash, fly ash has some actual gap;

[0011] 5、目前对锅炉管候选材料高温腐蚀的评价,采用均匀腐蚀的方法进行评价,与实际严重的非均匀腐蚀不符。 [0011] 5, the current evaluation of high temperature corrosion of boiler tubes candidate materials, uniform corrosion method was evaluated, not consistent with the severe non-uniform etching.

发明内容 SUMMARY

[0012] 本发明的目的在于提供一种用于电站锅炉过热器管高温腐蚀实验及表征的方法, 解决了常规高温腐蚀实验与实际工况不符、实验缺少应力的问题。 [0012] The object of the present invention is to provide a method and characterization of high temperature corrosion test power boiler superheater tubes for solving the conventional high temperature corrosion test does not match with the actual operating conditions, the lack of experimental stress problems. 在实际煤灰和模拟烟气环境中,对超超临界锅炉过热器管材料进行高温应力腐蚀环境的模拟,并对金属的非均匀腐蚀程度进行表征。 Simulated flue gas and ash in the actual environment, for ultra supercritical boiler superheater tubing material to simulate a high temperature environment, stress corrosion, and characterization of non-uniformity of the corrosion of metals.

[0013] 本发明是对所选择的过热器管材料施加应力,选择取自电厂过热器管的煤灰以及合成烟气进行高温腐蚀实验。 [0013] The present invention is a stress is applied to the superheater tubes to the selected material, and synthetic coal ash selected power plant flue gas superheater tubes from a high temperature corrosion test. 在对试样进行高温腐蚀后,统计腐蚀深度,然后借助概率论和数理统计的相关知识,获得通过矩估计法估算出最大腐蚀深度的定量表征非均匀腐蚀程度的方法。 After the sample for high temperature corrosion, the corrosion depth statistics, and then by means of the relevant probability theory and statistics, the maximum corrosion depth to obtain a quantitative characterization of the degree of non-uniform corrosion estimated by Monent.

[0014]金属材料的热膨胀系数随着温度的变化而发生变化,所以不同材料的零件或工件在室温下配合时所产生的应力,随着温度的升高会发生变化,导致实验数据的不准确。 [0014] The thermal expansion coefficient of the metallic material changes with temperature varies, the stress parts or workpieces of different materials at room temperature produced during mating, with increasing temperature will change, resulting in inaccurate experimental data . 同种材料从室温到高温的热膨胀系数变化一致,能使产生的应力尽量保持恒定。 The same material is consistent variation coefficient of thermal expansion from room temperature to a high temperature, stress generated can be kept constant. 本发明充分考虑了超超临界锅炉过热器管的实际应用状态,用相同材料的试样施加一定的应力,利用实际使用的煤灰和合成烟气环境模拟应力腐蚀行为,使实验更接近于实际工况。 The present invention fully contemplates the practical application state ultra supercritical boiler superheater tubes, a certain stress is applied to the same sample of material, using the synthetic coal ash and flue gas actually used environment simulation of stress corrosion behavior, so closer to the actual experimental conditions. 具体工艺步骤如下: The specific process steps are as follows:

[0015] (1)选择用于锅炉过热器管的同种金属材料,设计成圆棒和圆筒耦合试样,圆棒的尺寸范围为Φ 5~Φ 60mm,与之配合的圆筒厚度范围为3~IOmm;开$状如图1和图2所示;计算500~800°C范围内产生应力所需的过盈量,精加工后装配,如图3所示。 [0015] (1) the same kind of metal material selected for boiler superheater tubes, designed to be coupled to the cylindrical rod and the sample, rod size range of Φ 5 ~ Φ 60mm, a thickness range of the cylinder cooperating therewith It is a 3 ~ IOmm; $ shaped like opening shown in FIG. 1 and FIG. 2; the range of 500 ~ 800 ° C calculated to produce the desired amount of interference stress, after finishing the assembly, as shown in FIG. 使500~800°C圆棒和圆筒间产生径向应力P的范围为22MPa〈P〈材料的屈服强度(水的临界压力是22.115MPa)。 That the rods 500 ~ 800 ° C is generated between the cylindrical and radial stress P is in the range of 22MPa <P <yield strength of the material (the critical pressure of water is 22.115MPa). 采用热胀法装配试样。 Sample assembly method using thermal expansion.

[0016] 采用热胀法装配时,理论过盈量δ*(μπι)计算公式: [0016] When using thermal expansion assembly, theoretical interference δ * (μπι) calculated:

[0017] [0017]

Figure CN104142292BD00051

(1) (1)

[0018] 式中,P为径向压力,MPa5C1X2分别为被包容件和包容件的刚性系数; μL、μ2分别为被包容件和包容件材料的泊松比W1 = In [0018] In the formula, P is the radial pressure, MPa5C1X2 coefficients are rigid member is contained, and the accommodating member; μL, μ2 is contained members are Poisson ratio of the material and the containment member W1 = In

Figure CN104142292BD00052

为配合处的公称直径,d2为包容件的外径,mm; E1、E2分别为被包容件和包容件的弹性模量,MPa。 As with the public at the nominal diameter, d2 is the outer diameter of the accommodating member, mm; E1, E2 respectively, and accommodating the accommodating member is an elastic member modulus, MPa.

[0019] 根据求得的理论过盈量5t,确定过盈量δ范围,一般取δ = 5t± (1~10)μηι,加工一批试样,选择其中尺寸接近d+δ*的试样进行实验研究,此时实际径向应力为: [0019] The interference theory 5t obtained, determining the amount of interference [delta] range, and generally δ = 5t ± (1 ~ 10) μηι, a number of sample processing, wherein the selected size closest sample d + δ * experimental study, the actual radial stress at this time is:

[0020] [0020]

Figure CN104142292BD00053

[0021 ] (22〈ρ獅〈实验温度时材料的屈服强度) [0021] (22 <ρ lion <yield strength of the material temperature of the experiment)

[0022] 装配后确保一个底面为平面,将该底面依次使用100#、200#、400#、600#砂纸打磨后,测量试样重量。 [0022] After assembly to ensure a flat bottom surface, the bottom surface sequentially using # 100, # 200, # 400, # 600 after sanding, the measurement sample weight.

[0023] (2)腐蚀性介质为模拟锅炉管工作环境的烟气和实际煤灰。 [0023] (2) the actual smoke and corrosive medium ash simulated environment of a boiler tube. 煤灰取自燃煤电厂的高温过热器管的上部积灰和底部结渣。 Upper ash from coal-superheater tube fouling and slagging bottom. 将灰/渣研成细粉末,用丙酮溶液调成均匀的糊状, 涂覆在试样表面。 Ash / slag crushed to a fine powder with acetone into a uniform paste, the coated surface of the sample. 在干净、干燥的环境中放置10~12h,待表面附着灰渣凝固后,将试样安放到试样架上,各个试样间的距离为5~20mm,试样架放入管式电阻炉。 After standing for 10 ~ 12h in a clean, dry environment, the surface to be adhered to ash solidification, the sample is placed into the sample holder, the distance between each sample of 5 ~ 20mm, the sample rack placed in a tube resistance furnace .

[0024] 气体〇2、0)2、302和吣通过混气装置后,组成配比为(3~10)%0 2+(13~18)%邙2+ (0.2~2)%S02+N2(体积分数)的合成气体,进入电阻炉的合成气体流量在10~60ml/min之间,气体流出电阻炉后进入尾气收集装置(5%的NaOH水溶液)。 [0024] Gas 〇2,0) 2,302 and Qin by the gas mixing means, the composition ratio of (3-10)% 0 2 + (13-18)% Mang 2+ (0.2 ~ 2)% S02 + N2 (volume fraction) of the synthesis gas into synthesis gas flow resistance furnace between 10 ~ 60ml / min, the exhaust gas flows into the collecting device resistance furnace (5% aqueous solution of NaOH). 电阻炉升高到一定温度(500 ~SO(TC),保温一定时间(100~5000h)。实现锅炉过热器管材料在应力状态下,处于高温、 煤灰、烟气介质综合作用下的腐蚀实验。同时放入一组不加应力的试样,将实验结果进行比较。 Resistance furnace rises to a certain temperature (500 ~ SO (TC), holding a certain time (100 ~ 5000h). Boiler superheater tube material in a stressed state, is the combined effect of the corrosion test under the high temperature, ash, flue gas medium At the same time a set of samples placed without stress, the results of experimental studies.

[0025] (3)对试样高温腐蚀后,取出试样,放入丙酮液体中,清净样品表面附着的灰渣,然后烘干,称重。 [0025] (3) high temperature corrosion of the sample after the sample was taken out, placed in acetone solvent, the ash adhered to the surface of the clean sample, then dried and weighed. 打磨试样底面,用扫描电子显微镜统计不同腐蚀条件下试样的腐蚀深度,通过矩估计法估算出最大腐蚀深度,以此为依据表征了非均匀腐蚀的程度,比较施加应力前后腐蚀程度的区别。 Grinding the bottom surface of the sample, the sample statistics etching depth under different etching conditions with a scanning electron microscope, the maximum corrosion depth estimated by Monent as a basis to characterize the non-uniform corrosion, degree of corrosion comparing the difference before and after stress application . 实验中必须有足够大(>50个)的样本容量,才能保证样本的分布状况与总体的分布趋于一致。 The experiment must be large enough (> 50) of the sample size, in order to ensure distribution of the sample with the overall distribution converge.

[0026] 矩估计法对非均匀腐蚀程度的表征: [0026] The characterization of non-uniform degree of corrosion Moment Estimation:

[0027] 假设一个试样各部分的腐蚀深度状况符合均匀分布,即如果假设用随机变量h表示腐蚀的深度,则由h服从均匀分布,也可表示成h~U[a,b],其中a代表腐蚀的最小深度,b 表示腐蚀的最大深度。 [0027] Suppose a situation that the corrosion depth in line with each part of the uniform distribution, i.e., if it is assumed random variable h indicates the depth of etching, by h uniform distribution can also be expressed as h ~ U [a, b], wherein representative of a minimum depth of corrosion, b represents the maximum depth of corrosion.

[0028] 在样本容量足够大时,样本的分布状况和总体的分布状况应当是相同的,可以用样本矩估计总体矩。 [0028] When a sufficiently large sample size, and distribution of the overall distribution of the sample should be the same, can estimate the population sample moments moments.

[0029] 通过实验得到的腐蚀深度表示为lu,其中h表示腐蚀的深度,i是测量的序号,即如果样本容量为N,则i = l、2、3……N。 [0029] represented by the depth of etching is obtained experimentally LU, where h represents the depth of corrosion, i is the measured number, i.e., if the sample size is N, i = l, 2,3 ...... N.

[0030] 根据实验得到的数值,可以计算样本均值和样本的二阶中心距。 [0030] According to the experimental values ​​obtained, the sample mean and the sample can be calculated from the center of the second order.

[0031] 样本均值为 [0031] Sample mean

Figure CN104142292BD00061

(3) (3)

[0032] 根据均匀分布的相关知识,其数学期望为 [0032] According to a uniform distribution of knowledge, which is the mathematical expectation

Figure CN104142292BD00062

(4) (4)

[0033] 令样本均值等于总体的数学期望,得 [0033] so that the sample mean equals the population of mathematical expectation, too

Figure CN104142292BD00063

0) 0)

[0034] 样本的二阶中心距为 [0034] samples of second-center distance

Figure CN104142292BD00064

[0035] 均匀分布的方差为:D(X) = (ba)2/12 (6) [0035] The uniform distribution of the variance: D (X) = (ba) 2/12 (6)

[0036] 令样本二阶中心距等于总体的方差,彳 [0036] so that the center distance equal to the second order overall sample variance, left foot

Figure CN104142292BD00065

(7) (7)

[0037] 由以上公式(5)和(7 ),结合统计得到的N个h值,可得到总体分布中的a和b的值,最大可能腐蚀深度即为 [0037] by the above equation (5) and (7), binding of the N values ​​h statistics obtained, the value obtained in the overall distribution of a and b, that is, the maximum corrosion depth may

Figure CN104142292BD00066

(8) (8)

[0038] 这样就可以推测出最大可能腐蚀深度,对非均匀腐蚀的程度进行表征。 [0038] This may be presumed that the maximum depth of corrosion, degree of corrosion is characterized by non-uniform.

[0039] 本发明与现有技术相比,具有以下优点: [0039] Compared with the prior art the present invention has the following advantages:

[0040] (1)采用存在应力的高温腐蚀试样,是高温腐蚀实验方法上的创新; [0040] (1) the presence of high-temperature stress corrosion coupons, the innovation is high temperature corrosion test method;

[0041] (2)对非均匀腐蚀部分的腐蚀程度进行表征;将高温腐蚀程度与材料的力学性能劣化联系起来是对高温腐蚀研究的理论创新; [0041] (2) The extent of corrosion on the non-uniform corrosion characterizing portion; the extent of corrosion of high temperature mechanical performance deterioration material linked to high temperature corrosion theoretical innovation research;

[0042] (3)本发明的制备方法简单,成本低。 [0042] (3) The preparation method is simple, low cost.

附图说明 BRIEF DESCRIPTION

[0043] 图1圆筒主视图。 [0043] FIG cylindrical front view.

[0044] 图2圆棒主视图。 [0044] The rod 2 a front view of FIG.

[0045] 图3装配图。 [0045] FIG. 3 is fitted FIG.

具体实施方式 Detailed ways

[0046] 下面结合具体实施例对本发明做进一步说明。 [0046] The following specific embodiments of the present invention further in conjunction with FIG.

[0047] 实施例1 [0047] Example 1

[0048] (1)选择电厂用于过热器管的T91钢作为实验材料,实验温度为600°C,腐蚀时间为300h。 [0048] (1) Select a plant of T91 superheater tubes as the experimental material, the exposure temperature of 600 ° C, corrosion time of 300h. 600°C时,材料的弹性模量为E= 1.68 X 105MPa、泊松比μ = 0.29、屈服强度为326MPa。 When 600 ° C, the elastic modulus is E = 1.68 X 105MPa, Poisson's ratio μ = 0.29, the yield strength of 326MPa. 取圆棒直径d = 5mm,圆筒外径cb= 15_。 Take rod diameter d = 5mm, the outer diameter of the cylindrical cb = 15_.

Figure CN104142292BD00071

[0049] [0049]

[0050] [0050]

[0051] [0051]

[0052] m〇 [0052] m〇

[0053] [0053]

[0054] [0054]

[0055] 22MPa〈p獅<60(TC 时的屈服强度326MPa。 [0055] 22MPa <p lion <60 (yield strength of TC 326MPa.

[0056] 选择δ = 2~3μπι的试样进行装配,装配后确保一个底面为平面,将该底面依次使用100#、200#、400#、600#砂纸打磨后,测量试样重量。 [0056] Sample selection δ = 2 ~ 3μπι be assembled after assembly to ensure a flat bottom surface, the bottom surface sequentially using # 100, # 200, # 400, # 600 after sanding, the measurement sample weight.

[0057] (2)煤灰取自600°C过热器管上部的积灰,将积灰研成细粉末后用丙酮溶液调成均匀的糊状,涂覆在试样表面。 [0057] (2) fly ash from fouling the upper 600 ° C superheater tubes, the fouling and research into a fine powder with acetone into a uniform paste, the coated surface of the sample. 在干净、干燥的环境中放置12h,待表面附着灰渣凝固后,将试样安放到试样架上,各个试样间的距离为l〇mm,试样架放入管式电阻炉。 In a clean, dry environment 12h, the ash adhered to the surface to be solidified, the sample is placed into the sample holder, the distance between each sample is l〇mm sample rack placed in a tube resistance furnace. 合成气体的组成(体积分数)为:15 % C02+3 · 5 % 02+0 · 25 % S02+81 · 25 %N2,进入电阻炉的流量为20ml/min,用铂丝网作为催化剂以使反应2S02+0 2 = 2S03保持平衡。 Composition of the synthesis gas (volume fraction): 15% C02 + 3 · 5% 02 + 0 · 25% S02 + 81 · 25% N2, the flow resistance into the furnace was 20ml / min, with a platinum mesh as a catalyst to make The reaction 2S02 + 0 2 = 2S03 balance. 气体流出炉后进入尾气收集装置(5% 的NaOH水溶液)。 After gas stream enters the furnace off-gas collecting means (5% aqueous solution of NaOH). 同时选择一组没有施加应力的试样进行对比实验。 Selecting a set of samples while no stress is applied to comparative tests.

[0058] 电阻炉升高到600°C,保温时间为IOOh、200h、300h。 [0058] The resistance furnace was raised to 600 ° C, holding time IOOh, 200h, 300h. 实现锅炉过热器管材料在应力状态下,处于高温、煤灰、烟气介质综合作用下的腐蚀实验。 Boiler superheater tube material in the state of stress, is the combined effect of the corrosion test under the high temperature, ash, flue gas medium.

[0059] (3)对试样腐蚀后取出试样,用丙酮液清净样品表面附着的灰渣,烘干称重后打磨试样底面,用扫描电子显微镜统计试样的腐蚀深度60个,通过式/7 = £(Χ') + λ/^(Υ)计算得到下述结果: [0059] (3) Remove the sample after etching of the sample, with the attached ash sample surface clean of acetone, dried and weighed polished bottom surface of the sample, the statistical sample with a scanning electron microscope corrosion depth 60, by formula / 7 = £ (Χ ') + λ / ^ (Υ) is calculated with the following results:

[0060] 腐蚀IOOh的试样,其最大腐蚀深度为0.112mm, [0060] Corrosion IOOh sample, the maximum corrosion depth of 0.112mm,

[00611 腐蚀200h的试样,其最大腐蚀深度为0.136mm, [00611 corrosion coupons 200h, the maximum corrosion depth of 0.136mm,

[0062] 腐蚀300h的试样,其最大腐蚀深度为0.157mm。 [0062] The corrosion coupons 300h, the maximum corrosion depth of 0.157mm.

[0063] 无应力的试样: [0063] unstressed sample:

[0064] 腐蚀IOOh的试样,其最大腐蚀深度为0.083mm, [0064] Corrosion IOOh sample, the maximum corrosion depth of 0.083 mm,

[0065] 腐蚀200h的试样,其最大腐蚀深度为0.116mm, [0065] The corrosion coupons 200h, the maximum corrosion depth of 0.116 mm,

[0066] 腐蚀300h的试样,其最大腐蚀深度为0.125mm。 [0066] The corrosion coupons 300h, the maximum corrosion depth of 0.125mm.

[0067] 实施例2 [0067] Example 2

[0068] (1)选择电厂锅炉管常用的HR3C钢作为实验材料,实验温度为700°C,腐蚀时间为300h。 [0068] (1) Select the boiler tube for power generation purposes HR3C steel as experimental material, the exposure temperature of 700 ° C, corrosion time of 300h. 700°C时,材料的弹性模量为E = 1.47 X IO5MPa、泊松比μ = 0.29、屈服强度为147MPa。 When 700 ° C, the elastic modulus is E = 1.47 X IO5MPa, Poisson's ratio μ = 0.29, the yield strength of 147MPa. 取圆棒直径d = 30mm,圆筒外径d2 = 4Ctam〇 Take rod diameter d = 30mm, d2 = the outer diameter of the cylindrical 4Ctam〇

[0069] 700。 [0069] 700. (:,当? = 5010^时, (: When ^ = 5010 when?

Figure CN104142292BD00081

[0072] 选择基孔制,具体尺寸为孔Φ3〇Γ)4,轴(丨)3()盟1,最小过盈量为42μπι,最大过盈量为50μηι。 [0072] Select hole basis, the specific size of the hole Φ3〇Γ) 4, a shaft (Shu) 3 () AU 1, the minimum amount of interference 42μπι, the maximum amount of interference 50μηι.

[0070] [0070]

[0071] [0071]

Figure CN104142292BD00082

[0073] δ = 42μπι 时 [0073] δ = time 42μπι

[0074] δ = 50μηι 时 [0074] δ = 50μηι when

[0075] 22MPa〈p獅<700°C时的屈服强度147MPa,符合要求。 [0075] 22MPa <p lion <147MPa yield strength at 700 ° C, to meet the requirements.

[0076]选择δ = 45~48μπι的试样进行装配,装配后确保一个底面为平面,将该底面依次使用100#、200#、400#、600#砂纸打磨后,测量试样重量。 [0076] Sample selection δ = 45 ~ 48μπι be assembled after assembly to ensure a flat bottom surface, the bottom surface sequentially using # 100, # 200, # 400, # 600 after sanding, the measurement sample weight.

[0077] (2)煤灰为取自600°C过热器管底部的结渣,将结渣研磨成粉末,用丙酮溶液调成均匀的糊状,涂覆在试样表面。 [0077] (2) 600 ° C from coal ash as a superheater tube bottom slag, the slag ground to a powder with acetone into a uniform paste, the coated surface of the sample. 在干净、干燥的环境中放置12h,待表面附着灰渣凝固后,将试样安放到试样架上,各个试样间的距离为15mm,试样架放入管式电阻炉。 After 12h is placed in a clean, dry environment, the surface to be adhered to ash solidification, the sample is placed into the sample holder, a distance of 15mm between each sample, the sample rack placed in a tube resistance furnace. 合成气体的组成(体积分数)为:15 % C02+3 · 5 % 02+0 · 5 % S02+81 % N2,进入电阻炉的流量为30ml/min,用铂丝网作为催化剂以使反应2S02+0 2 = 2S03保持平衡。 Composition of the synthesis gas (volume fraction): 15% C02 + 3 · 5% 02 + 0 · 5% S02 + 81% N2, the flow resistance into the furnace was 30ml / min, with a platinum mesh as a catalyst for the reaction 2S02 +0 2 = 2S03 balance. 气体流出炉后进入尾气收集装置(5 %的NaOH水溶液)。 After gas stream enters the furnace off-gas collecting means (5% aqueous solution of NaOH). 同时选择一组没有施加应力的试样进行对比实验。 Selecting a set of samples while no stress is applied to comparative tests. 同时选择一组没有施加应力的试样进行对比实验。 Selecting a set of samples while no stress is applied to comparative tests.

[0078] 电阻炉升高到700°C,保温时间为10011、20011、30011。 [0078] The resistance furnace was raised to 700 ° C, holding time 10011,20011,30011. 实现锅炉过热器管材料在应力状态下,处于高温、煤灰、烟气介质综合作用下的腐蚀实验。 Boiler superheater tube material in the state of stress, is the combined effect of the corrosion test under the high temperature, ash, flue gas medium.

[0079] (3)对试样腐蚀后取出试样,用丙酮液清净样品表面附着的灰渣,烘干称重后打磨试样底面,用扫描电子显微镜统计试样的腐蚀深度60个,通过式6 = + 计算得到下述结果: [0079] (3) Remove the sample after etching of the sample, with the attached ash sample surface clean of acetone, dried and weighed polished bottom surface of the sample, the statistical sample with a scanning electron microscope corrosion depth 60, by 6 = + calculation formula with the following results:

[0080] 腐蚀IOOh的试样,其最大腐蚀深度为0.091mm, [0080] Corrosion IOOh sample, the maximum corrosion depth of 0.091mm,

[0081 ] 腐蚀200h的试样,其最大腐蚀深度为0.1 llmm, [0081] The corrosion coupons 200h, the maximum corrosion depth of 0.1 llmm,

[0082] 腐蚀300h的试样,其最大腐蚀深度为0.129mm。 [0082] The corrosion coupons 300h, the maximum corrosion depth of 0.129mm.

[0083]无应力的试样: [0083] unstressed sample:

[0084] 腐蚀IOOh的试样,其最大腐蚀深度为0.075mm, [0084] Corrosion IOOh sample, the maximum corrosion depth of 0.075mm,

[0085] 腐蚀200h的试样,其最大腐蚀深度为0.102mm, [0085] The corrosion coupons 200h, the maximum corrosion depth of 0.102 mm,

[0086] 腐蚀300h的试样,其最大腐蚀深度为0.112mm。 [0086] corrosion coupons 300h, the maximum corrosion depth of 0.112mm.

[0087] 实施例3 [0087] Example 3

[0088] (1)选择电厂锅炉管常用的HR3C钢作为实验材料,实验温度为700°C,腐蚀时间为300h。 [0088] (1) Select the boiler tube for power generation purposes HR3C steel as experimental material, the exposure temperature of 700 ° C, corrosion time of 300h. 700°C时,材料的弹性模量为E = 1.47 X IO5MPa、泊松比μ = 0.29、屈服强度为147MPa。 When 700 ° C, the elastic modulus is E = 1.47 X IO5MPa, Poisson's ratio μ = 0.29, the yield strength of 147MPa. 取圆棒直径d = 50mm,圆筒外径d2 = 6Ctam〇 Take rod diameter d 50mm, = d2 = the outer diameter of the cylindrical 6Ctam〇

[0089] 700。 [0089] 700. (:,当? = 5010^时, (: When ^ = 5010 when?

Figure CN104142292BD00091

[0090] [0090]

[0091] [0091]

[0092] 选择基孔制,具体尺寸为孔Φ50|.™4,:轴(丨)5〇盟最小过盈量为102μπι,最大过盈量为118μηι〇 [0092] Select hole basis, the specific size of the hole Φ50 |. ™ 4 ,: shaft (Shu) 5〇 AU is the minimum amount of interference 102μπι, the maximum amount of interference 118μηι〇

Figure CN104142292BD00092

[0093] δ = 1〇2μηι0\ [0093] δ = 1〇2μηι0 \

[0094] δ = 118μηι0\ [0094] δ = 118μηι0 \

[0095] 22MPa〈p獅<700°C时的屈服强度147MPa,符合要求。 [0095] 22MPa <p lion <147MPa yield strength at 700 ° C, to meet the requirements.

[0096] 选择δ = 108~114μπι的试样进行装配,装配后确保一个底面为平面,将该底面依次使用100#、200#、400#、600#砂纸打磨后,测量试样重量。 [0096] Sample selection δ = 108 ~ 114μπι be assembled after assembly to ensure a flat bottom surface, the bottom surface sequentially using # 100, # 200, # 400, # 600 after sanding, the measurement sample weight.

[0097] (2)煤灰为取自600°C过热器管底部的结渣,将结渣研磨成粉末,用丙酮溶液调成均匀的糊状,涂覆在试样表面。 [0097] (2) 600 ° C from coal ash as a superheater tube bottom slag, the slag ground to a powder with acetone into a uniform paste, the coated surface of the sample. 在干净、干燥的环境中放置12h,待表面附着灰渣凝固后,将试样安放到试样架上,各个试样间的距离为15mm,试样架放入管式电阻炉。 After 12h is placed in a clean, dry environment, the surface to be adhered to ash solidification, the sample is placed into the sample holder, a distance of 15mm between each sample, the sample rack placed in a tube resistance furnace. 合成气体的组成(体积分数)为:15 % C02+3 · 5 % O2+1 % S02+80 · 5 % N2,进入电阻炉的流量为30ml/min,用铂丝网作为催化剂以使反应2S02+0 2 = 2S03保持平衡。 Composition of the synthesis gas (volume fraction): 15% C02 + 3 · 5% O2 + 1% S02 + 80 · 5% N2, the flow resistance into the furnace was 30ml / min, with a platinum mesh as a catalyst for the reaction 2S02 +0 2 = 2S03 balance. 气体流出炉后进入尾气收集装置(5 %的NaOH水溶液)。 After gas stream enters the furnace off-gas collecting means (5% aqueous solution of NaOH). 同时选择一组没有施加应力的试样进行对比实验。 Selecting a set of samples while no stress is applied to comparative tests. 同时选择一组没有施加应力的试样进行对比实验。 Selecting a set of samples while no stress is applied to comparative tests.

[0098] 电阻炉升高到700°C,保温时间为10011、20011、30011。 [0098] resistance furnace was raised to 700 ° C, holding time 10011,20011,30011. 实现锅炉过热器管材料在应力状态下,处于高温、煤灰、烟气介质综合作用下的腐蚀实验。 Boiler superheater tube material in the state of stress, is the combined effect of the corrosion test under the high temperature, ash, flue gas medium.

[0099] (3)对试样腐蚀后取出试样,用丙酮液清净样品表面附着的灰渣,烘干称重后打磨试样底面,用扫描电子显微镜统计试样的腐蚀深度60个,通过式= + 计算得到下述结果: [0099] (3) Remove the sample after etching of the sample, with the attached ash sample surface clean of acetone, dried and weighed polished bottom surface of the sample, the statistical sample with a scanning electron microscope corrosion depth 60, by = + calculated by the following formula results:

[0100] 腐蚀IOOh的试样,其最大腐蚀深度为0.113mm, [0100] Corrosion IOOh sample, the maximum corrosion depth of 0.113 mm,

[0101] 腐蚀200h的试样,其最大腐蚀深度为0.132mm, [0101] corrosion coupons 200h, the maximum corrosion depth of 0.132 mm,

[0102] 腐蚀300h的试样,其最大腐蚀深度为0.149mm。 [0102] corrosion coupons 300h, the maximum corrosion depth of 0.149mm.

[0103] 无应力的试样: [0103] unstressed sample:

[0104] 腐蚀IOOh的试样,其最大腐蚀深度为0.095mm, [0104] Corrosion IOOh sample, the maximum corrosion depth of 0.095mm,

[0105] 腐蚀200h的试样,其最大腐蚀深度为0.146mm, [0105] corrosion coupons 200h, the maximum corrosion depth of 0.146mm,

[0106] 腐蚀300h的试样,其最大腐蚀深度为0.138mm。 [0106] corrosion coupons 300h, the maximum corrosion depth of 0.138mm.

[0107] 通过三个实施例的实验可知,与没有施加应力状态比较,施加应力的试样,腐蚀程度较大,腐蚀较严重。 [0107] Experimental Example understood by three, compared to the stress state is not applied, the stress applied to the sample, the degree of corrosion is large, more serious corrosion. 随着腐蚀气氛中SO2含量的增加,腐蚀程度也增加。 With the increase of SO2 content in a corrosive environment, the degree of corrosion also increases.

[0108] 随着腐蚀时间的增加,试样的理论最大腐蚀深度是逐渐增大的,并且试样的理论最大腐蚀深度大于所有的样本值。 [0108] As the etching time increases, the maximum corrosion depth is gradually increased sample theory, the theoretical and the sample is greater than the maximum corrosion depth of all the sample values. 因此,使用此方法可以起到较好的估计和推测的效果,用这种方法来表征非均匀腐蚀的程度在理论上是可行的。 Thus, this method can play a better estimation of the estimation and, in this way to characterize the extent of non-uniform corrosion is theoretically possible.

[0109] 通过上述非均匀腐蚀表征方法的实例,可知使用这种方法来表征非均匀腐蚀是可行的。 [0109] By way of example of the non-uniform corrosion characterization methods, it was found to characterize the non-uniform corrosion is feasible using this method. 由于所有的数据都来源于实际统计的结果,因此对统计的精度以及统计样本的数量提出了较高的要求。 Since all data are derived from the results of the actual statistics, so statistics on the number and accuracy of sample statistics put forward higher requirements.

Claims (2)

1. 一种用于电站锅炉过热器管高温腐蚀实验及表征的方法,其特征在于,实验工艺步骤如下: (1) 选择用于锅炉过热器管的同种金属材料,设计成圆棒和圆筒耦合试样,圆棒的尺寸范围为Φ 5~Φ 60mm,与之配合的圆筒厚度范围为3~IOmm;计算500~800°C范围内产生应力所需的过盈量,精加工后装配;使500~800°C圆棒和圆筒间产生径向应力P的范围为22MPa〈P〈材料的屈服强度,采用热胀法装配试样; 采用热胀法装配时,过盈量心计算公式: 1. A method for high temperature corrosion test and characterization of power boiler superheater tubes, characterized in that, the experimental process steps as follows: (1) the same kind of metal material selected for boiler superheater tubes, designed as a round rod and after calculating the amount of interference in the stress required to produce 500 ~ 800 ° C range, finishing; coupled sample tube, rod size range of Φ 5 ~ Φ 60mm, with a thickness in the range of a cylindrical fitting 3 ~ IOmm assembly; so the range 500 ~ 800 ° C P between the radial stresses generated as the cylinder rod and 22MPa <P <material yield strength, thermal expansion method using a sample assembly; thermal expansion during use of the assembly process, the amount of interference heart The formula is:
Figure CN104142292BC00021
(1) 式中,P为径向压力,MPa W1X2分别为被包容件和包容件的刚性系数;μι、μ2分别为被包容件和包容件材料的泊松比W1 = I-P1 (1) In the formula, P is the radial pressure, MPa W1X2 coefficients are rigid member is contained, and the accommodating member; μι, μ2 are inclusive piece of material containment member and the Poisson ratio of I-P1 as W1 =
Figure CN104142292BC00022
为配合处的公称直径,d2为包容件的外径,mm 分别为被包容件和包容件的弹性模量,MPa; 根据求得的过盈量3t,确定过盈量δ范围,取5 = 5t± (1~1〇)μηι,加工一批试样,选择其中尺寸接近d+δ*的试样进行实验研究,此时实际径向应力为: As with the public at the nominal diameter, d2 is the outer diameter of the containment member, mm respectively is contained a modulus of elasticity member and accommodating member, MPa; determined according to the amount of interference 3t, δ determined interference range, taking 5 = 5t ± (1 ~ 1〇) μηι, a number of sample processing, wherein the selected size closest d + δ * sample, the experimental studies, the actual radial stress at this time is:
Figure CN104142292BC00023
(2) 装配后确保一Iι±υ y:y I ι±υ,w ι±υ πλ次使用100#、200#、400#、600#砂纸打磨后,测量试样重量; (2) 腐蚀性介质为模拟锅炉管工作环境的烟气和实际煤灰,煤灰取自燃煤电厂的高温过热器管的上部积灰和底部结渣;将灰/渣研成细粉末,用丙酮溶液调成均匀的糊状,涂覆在试样表面;放置10~12h,待表面附着灰渣凝固后,将试样安放到试样架上,各个试样间的距离为5~20mm,试样架放入管式电阻炉; 气体O2、CO2、SO2和N2通过混气装置后,组成按体积分数为(3~10)% O2+(13~18)% CO2+ (0.2~2)%S02+N2的合成气体,进入电阻炉的合成气体流量在10~60ml/min之间,气体流出电阻炉后进入尾气收集装置;电阻炉升高到500~800°C温度,保温100~5000h;实现锅炉过热器管材料在应力状态下,处于高温、煤灰、烟气介质综合作用下的腐蚀实验;同时放入一组不加应力的试样,将实验结果进 (2) after assembly to ensure a Iι ± υ y: y I ι ± υ, w ι ± υ πλ times using # 100, # 200, # 400, # 600 after sanding, the measurement sample weight; (2) Corrosion medium to simulate the working environment of the boiler flue gas duct and the actual ash, ash from an upper portion of the superheater tube fouling fired power plant and a bottom slag; RESEARCH the ash / slag into a fine powder, transferred into a solution of acetone smooth paste, the coated surface of the sample; placed 10 ~ 12h, the ash adhered to the surface to be solidified, the sample is placed into the sample holder, the distance between each sample of 5 20mm ~, put the sample holder the tube resistance furnace; gas O2, CO2, SO2 and N2 through the gas mixing device, consisting of a volume fraction of (3 ~ 10)% O2 + (13 ~ 18)% CO2 + (0.2 ~ 2)% S02 + N2 synthesis of gas into synthesis gas flow resistance furnace between 10 ~ 60ml / min, the exhaust gas flows into the collection device resistance furnace; increased resistance furnace to a temperature of 500 ~ 800 ° C, holding 100 ~ 5000h; boiler superheater materials under stress conditions, is corrosion test under the combined effect of high temperature, ash, flue gas medium; the same time into a set of samples without stress, the results into 比较; (3) 对试样高温腐蚀后,取出试样,放入丙酮液体中,清净试样表面附着的灰渣,然后烘干,称重;打磨试样底面,用扫描电子显微镜统计不同腐蚀条件下试样的腐蚀深度,通过矩估计法估算出最大腐蚀深度,以此为依据表征了非均匀腐蚀的程度,比较施加应力前后腐蚀程度的区别;实验中样本容量>50个,保证样本的分布状况与总体的分布趋于一致。 Comparative; (3) high temperature corrosion of the sample after the sample was taken out, placed in acetone solvent, the ash adhered to the surface of the clean sample, and then dried, weighed; a sample polished bottom surface, different statistical etching using a scanning electron microscope corrosion depth of the sample under conditions estimated by Monent the maximum corrosion depth as a basis for characterizing the degree of non-uniform corrosion, degree of corrosion of the difference between before and after applying stress comparison; experiment sample size> 50, to ensure that the sample distribution and population distribution converge.
2. 根据权利要求1所述的用于电站锅炉过热器管高温腐蚀实验及表征的方法,其特征在于,所述的表征方法,是用矩估计法对非均匀腐蚀程度的进行表征; 假设用随机变量h表示腐蚀的深度,则由h服从均匀分布,表示成h~U[a,b],其中a代表腐蚀的最小深度,b表示腐蚀的最大深度; 在样本容量足够大时,样本的分布状况和总体的分布状况应当是相同的,用样本矩估计总体矩; 通过实验得到的腐蚀深度表示为lu,其中h表示腐蚀的深度,i是测量的序号,即样本容量为N,贝lji = l、2、3……N; 根据实验得到的数值,计算样本均值和样本的二阶中心距; 蚀; 2. The method of experiment and characterization of high temperature corrosion of superheater tubes Utility Boiler according to claim 1, characterized in that the characterization methods are characterized by moment estimation method for non-uniform degree of corrosion; Suppose that random variable h indicates the depth of etching, by h uniform distribution, expressed as h ~ U [a, b], wherein a represents a minimum depth of corrosion, b represents the maximum corrosion depth; when a sufficiently large sample size, sample distribution and distribution of general should be the same, with sample moments estimated overall moment; etching depth obtained by experiments expressed as LU, where h represents the depth of corrosion, i is the serial number measured, i.e. the sample size is N, shellfish lji = l, 2,3 ...... N; in accordance with the experimental values ​​obtained, the sample mean and the sample is calculated from the center of the second order; erosion;
Figure CN104142292BC00031
这样推测出最大腐蚀深度,对非均匀腐蚀的程度进行表征。 Such presumed maximum corrosion depth, a non-uniform degree of corrosion were characterized.
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