CN104142292B - A kind of for Utility Boiler Superheater pipe high temperature corrosion experiment and the method for sign - Google Patents
A kind of for Utility Boiler Superheater pipe high temperature corrosion experiment and the method for sign Download PDFInfo
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Abstract
A kind of for Utility Boiler Superheater pipe high temperature corrosion experiment and the method for sign, belong to high temperature stress corrosion technology field.Select the same metal material for boiler superheater tube, specimen size and precision is determined according to stress intensity suffered by material, be there is cylinder and the pole of certain margin of tolerance by polish preparation, produce certain interference fit when cylinder and pole being assembled together, can guarantee that the stress required for generation.After sample is carried out high temperature corrosion, add up the unsymmetrical corrosion degree of depth of sample under certain etching condition, then estimate maximum corrosion depth by moments estimation method, characterize the degree of unsymmetrical corrosion on this basis, the sample after high temperature corrosion is carried out the evaluation of unsymmetrical corrosion degree.According to experimental result, the suitability under high-temperature corrosion environment and stress state of the superheater tube material is evaluated.The preparation method of the present invention is simple, low cost, it is adaptable to the high temperature stress corrosion experiment of boiler superheater tube.
Description
Technical field
The invention belongs to high temperature stress corrosion technology field, it is specifically related to a kind of for Utility Boiler Superheater pipe high temperature corrosion experiment and the method that characterizes, for boiler of power plant superheater tube stress etching experiment method under high-temperature corrosion environment and the evaluation methodology of unsymmetrical corrosion degree.
Background technology
In power plant, the safe operation of power station boiler four-tube (superheater tube, reheater tube, economizer tube, water screen tube), it is to ensure that the prerequisite that power station is properly functioning.These pipelines are chronically in high-temperature water or the pressure of steam and coal combustion environments, it is therefore desirable to have preferable high temperature microstructure stability, have higher creep rupture strength and high-temperature corrosion resistance performance, especially superheater and reheater piping simultaneously.Superheater tube is to be on active service in certain stress state, certain temperature and certain corrosive environment.Conventional superheater tube is generally pearlite heatproof steel, martensite heat-resistant steel and austenitic heat-resistance steel, such as novel 9%～12%Cr, T91, T92, HR3C, TP304H, TP347H and Super304H, and some nickel base superalloys such as Inconel 617, Inconel 690, Inconel 671 etc..
Superheater tube outer wall is chronically exposed in coal combustion environments, by coal ash and flue gas corrosion.Pipeline material the most generally to carry out the simulation experiment under certain etching condition, thus the suitability to material is evaluated.In laboratory, it is typically the one-tenth ash condition in pulverized-coal fired boiler is reduced, but high temperature corrosion and the stress suffered by metal tube and wall temperature is in close relations, stress is the biggest, wall temperature raises, corrosion increases the weight of, these all can not sufficiently be reduced when laboratory simulation, makes evaluation result not be inconsistent with actual condition.
The high temperature corrosion of superheater tube, is the common effect of the coal ash/flue gas corrosion of the interior steam pressure of pipe and pipe extroversion fire side.Existing high temperature corrosion is tested, and is the pure high temperature corrosion under not having stress, or the corrosion loaded metal material by NOL ring；When these degree of accuracy that cannot ensure load and high temperature, stress is constant.Coal ash used is also the synthesis coal ash of simulation, has a certain distance with actual coal ash.
It addition, in high temperature corrosion dynamics research, generally use oxidation weight gain or thicken the index as evaluation extent of corrosion, ignoring high temperature corrosion and there is spot corrosion or the reality along grain boundary corrosion.Therefore characterizing of high temperature corrosion degree needs locality and the seriousness of non-uniform corrosion to show.
At present, conventional stress etching experiment method has the disadvantage that
1, NOL ring is utilized to load, it is impossible to when the degree of accuracy of guarantee load and high temperature, stress is constant；
2, the stress produced under room temperature between different materials, can change during high temperature, and the stress etching experiment result under room temperature is mutually far short of what is expected with the stress corrosion environment under high temperature, it is impossible to effectively to evaluate the suitability of material, causes experimental result to produce error；
3, the high temperature corrosion of superheater tubes, is the corrosion of the high temperature stress under steam pressure effect in pipe, and existing high temperature corrosion evaluation is the pure high temperature corrosion under not having stress or utilizes NOL ring to load；
4, in the high temperature corrosion experiment of boiler tube, coal ash used is the synthesis coal ash of simulation, has a certain distance with actual coal ash；
5, the current evaluation to boiler tube candidate material high temperature corrosion, uses the method for homogeneous corrosion to be evaluated, and the unsymmetrical corrosion serious with reality is not inconsistent.
Summary of the invention
It is an object of the invention to provide a kind of for Utility Boiler Superheater pipe high temperature corrosion experiment and the method for sign, solve conventional high temperature corrosion experiment and be not inconsistent with actual condition, test the problem lacking stress.In actual coal ash and simulated flue gas environment, ultra-supercritical boiler superheater tube material is carried out the simulation of high temperature stress corrosive environment, and the unsymmetrical corrosion degree of metal is characterized.
The present invention is that selected superheater tube material is applied stress, selects to take from the coal ash of power plant's superheater tube and synthesis flue gas carries out high temperature corrosion experiment.After sample is carried out high temperature corrosion, add up corrosion depth, then by theory of probability and the relevant knowledge of mathematical statistics, it is thus achieved that the method being estimated the quantitatively characterizing unsymmetrical corrosion degree of maximum corrosion depth by moments estimation method.
The thermal coefficient of expansion of metal material changes along with the change of temperature, so produced stress when the part of different materials or workpiece at room temperature coordinate, along with the rising of temperature can change, causes the inaccurate of experimental data.Same material thermal coefficient of expansion change from room temperature to high temperature is consistent, and the stress of generation can be made to keep constant as far as possible.The present invention has taken into full account the realistic application conditions of ultra-supercritical boiler superheater pipe, applies certain stress with the sample of identical material, utilizes actually used coal ash and synthesis flue gas environmental simulation stress corrosion behavior, makes experiment closer to actual condition.Concrete technology step is as follows:
(1) selecting the same metal material for boiler superheater tube, be designed to pole and cylinder coupling sample, the size range of pole is Φ 5～Φ 60mm, and matched cylinder thickness range is 3～10mm；Shape is as depicted in figs. 1 and 2；Produce the magnitude of interference needed for stress in the range of calculating 500～800 DEG C, assemble after polish, as shown in Figure 3.500～800 DEG C are made between pole and cylinder, to produce the radial stress P yield strength (critical pressure of water is 22.115MPa) in the range of 22MPa < P < material.Use flatulence of heat type method assembling sample.
When using the assembling of flatulence of heat type method, theoretical magnitude of interference δt(μm) computing formula:
In formula, P is radial pressure, MPa；C1、C2It is respectively internal member and the stiffness coefficient of external member；μ1、μ2It is respectively internal member and the Poisson's ratio of external member material；C1=1-μ1,D is the nominal diameter at cooperation, d2For the external diameter of external member, mm；E1、E2It is respectively internal member and the elastic modelling quantity of external member, MPa.
According to the theoretical magnitude of interference δ tried to achievet, determine magnitude of interference δ scope, typically take δ=δt± (1～10) μm, processes batch to be tested, selects wherein to be closely sized to d+ δtSample carry out experimentation, actual radial stress is:
(22<pActual< yield strength of material during experimental temperature)
Guarantee after assembling that a bottom surface is plane, after this bottom surface is used 100#, 200#, 400#, 600# sand papering successively, measure sample weight.
(2) Korrosionsmedium is the flue gas of simulation boiler tube working environment and actual coal ash.Top dust stratification and the bottom slagging scorification of the Superheater tube of coal-burning power plant taken from by coal ash.Ash/slag is ground into fine powder, with the uniform pasty state of acetone soln furnishing, is coated in specimen surface.Placing 10～12h in environment clean, that be dried, after surface attachment lime-ash solidifies, be placed on specimen mounting by sample, the distance between each sample is 5～20mm, and specimen mounting puts into tube type resistance furnace.
Gas O2、CO2、SO2And N2After gas mixing device, composition and ratio is (3～10) %O2+ (13～18) %CO2+ (0.2～2) %SO2+N2The forming gas of (volume fraction), the forming gas flow of entrance resistance furnace is between 10～60ml/min, and gas enters tail gas collecting device (the NaOH aqueous solution of 5%) after flowing out resistance furnace.Resistance furnace is increased to uniform temperature (500～800 DEG C), held for some time (100～5000h).Realize boiler superheater tube material under stress state, be in the corrosion experiment under high temperature, coal ash, flue gas medium comprehensive function.Put into one group of sample being not added with stress simultaneously, experimental result is compared.
(3), after to sample high temperature corrosion, take out sample, put in acetone liquid, the lime-ash of peace and quiet sample surfaces attachment, then dry, weigh.Polishing sample bottom surface, by the corrosion depth of sample under the scanning electron microscope different etching condition of statistics, estimates maximum corrosion depth by moments estimation method, characterizes the degree of unsymmetrical corrosion on this basis, compares and applies the difference of extent of corrosion before and after stress.Experiment must have sufficiently large (> 50) sample size, the distribution situation of guarantee sample reaches unanimity with overall distribution.
The moments estimation method sign to unsymmetrical corrosion degree:
Assume that the corrosion depth situation of a sample each several part meets to be uniformly distributed, i.e. if it is assumed that represent the degree of depth of corrosion with stochastic variable h, then obeyed by h and be uniformly distributed, may also indicate that into h～U [a, b], wherein a represents the minimum-depth of corrosion, and b represents the depth capacity of corrosion.
When sample size is sufficiently large, the distribution situation of sample and overall distribution situation should be identical, can estimate population moment by sample moment.
The corrosion depth obtained by experiment is expressed as hi, wherein h represents the degree of depth of corrosion, and i is the sequence number measured, if i.e. sample size is N, then i=1,2,3 ... N.
According to the numerical value that obtains of experiment, can calculate the second-order central of sample average and sample away from.
Sample average is:
According to equally distributed relevant knowledge, its mathematic expectaion is:
Sample average is made to be equal to overall mathematic expectaion:
The second-order central of sample away from for:
Equally distributed variance is: D (X)=(b-a)2/12 (6)
Make sample second-order central away from equal to overall variance, obtain:
By above formula (5) and (7), the N number of h value obtained in conjunction with statistics, the value of a and b in available population distribution, maximum possible corrosion depth is:
Thus can deduce maximum possible corrosion depth, the degree of unsymmetrical corrosion is characterized.
The present invention compared with prior art, has the advantage that
(1) there is the high temperature corrosion sample of stress in employing, is the innovation on high temperature corrosion experimental technique；
(2) extent of corrosion of unsymmetrical corrosion part is characterized；The mechanical property deterioration of high temperature corrosion degree with material being connected is the theory innovation to high temperature corrosion research；
(3) preparation method of the present invention is simple, low cost.
Accompanying drawing explanation
Fig. 1 cylinder front view.
Fig. 2 pole front view.
Fig. 3 installation diagram.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
(1) selecting power plant for the T91 steel of superheater tube as experiment material, experimental temperature is 600 DEG C, during corrosion
Between be 300h.When 600 DEG C, the elastic modelling quantity of material is E=1.68 × 105MPa, Poisson's ratio μ=0.29, yield strength are 326MPa.Take diameter of the rod d=5mm, outside diameter of cylinder d2=15mm.
600 DEG C, as p=30MPa,
Calculate: C1=1-μ1=1-0.29=0.71,
Select basic hole system, the most a size of holeAxleMinimum interference amount is 2 μm, and maximum interference amount is 6 μm.
During the μm of δ=2,
During the μm of δ=6,
22MPa<pActual< yield strength 326MPa when 600 DEG C.
The sample selecting δ=2～3 μm assembles, and guarantees that a bottom surface is plane after assembling, after this bottom surface is used 100#, 200#, 400#, 600# sand papering successively, measures sample weight.
(2) dust stratification on 600 DEG C of superheater tube tops taken from by coal ash, uses the uniform pasty state of acetone soln furnishing, be coated in specimen surface after dust stratification is ground into fine powder.Placing 12h in environment clean, that be dried, after surface attachment lime-ash solidifies, be placed on specimen mounting by sample, the distance between each sample is 10mm, and specimen mounting puts into tube type resistance furnace.The composition (volume fraction) of forming gas is: 15%CO2+ 3.5%O2+ 0.25%SO2+ 81.25%N2, the flow entering resistance furnace is 20ml/min, with platinum gauze as catalyst so that reacting 2SO2+O2=2SO3Keep balance.Gas flows out furnace rear and enters tail gas collecting device (the NaOH aqueous solution of 5%).Select one group of sample not applying stress to carry out contrast experiment simultaneously.
Resistance furnace is increased to 600 DEG C, and temperature retention time is 100h, 200h, 300h.Realize boiler superheater tube material under stress state, be in the corrosion experiment under high temperature, coal ash, flue gas medium comprehensive function.
(3) take out sample after sample being corroded, with the lime-ash of acetone solution peace and quiet sample surfaces attachment, dry sample bottom surface of polishing after weighing, by the corrosion depth 60 of scanning electron microscope statistical test sample, pass through formulaIt is calculated following result:
The sample of corrosion 100h, its maximum corrosion depth is 0.112mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.136mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.157mm.
Stressless sample:
The sample of corrosion 100h, its maximum corrosion depth is 0.083mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.116mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.125mm.
Embodiment 2
(1) selecting the HR3C steel that power plant boiler tube is commonly used as experiment material, experimental temperature is 700 DEG C, and etching time is 300h.When 700 DEG C, the elastic modelling quantity of material is E=1.47 × 105MPa, Poisson's ratio μ=0.29, yield strength are 147MPa.Take diameter of the rod d=30mm, outside diameter of cylinder d2=40mm.
700 DEG C, as p=50MPa,
Calculate: C1=1-μ1=1-0.29=0.71,
Select basic hole system, the most a size of holeAxleMinimum interference amount is 42 μm, and maximum interference amount is 50 μm.
During the μm of δ=42,
During the μm of δ=50,
22MPa<pActual< yield strength 147MPa when 700 DEG C, meets the requirements.
The sample selecting δ=45～48 μm assembles, and guarantees that a bottom surface is plane after assembling, after this bottom surface is used 100#, 200#, 400#, 600# sand papering successively, measures sample weight.
(2) coal ash is to take from the slagging scorification bottom 600 DEG C of superheater tubes, by slagging scorification grind into powder, with the uniform pasty state of acetone soln furnishing, is coated in specimen surface.Placing 12h in environment clean, that be dried, after surface attachment lime-ash solidifies, be placed on specimen mounting by sample, the distance between each sample is 15mm, and specimen mounting puts into tube type resistance furnace.The composition (volume fraction) of forming gas is: 15%CO2+ 3.5%O2+ 0.5%SO2+ 81%N2, the flow entering resistance furnace is 30ml/min, with platinum gauze as catalyst so that reacting 2SO2+O2=2SO3Keep balance.Gas flows out furnace rear and enters tail gas collecting device (the NaOH aqueous solution of 5%).Select one group of sample not applying stress to carry out contrast experiment simultaneously.Select one group of sample not applying stress to carry out contrast experiment simultaneously.
Resistance furnace is increased to 700 DEG C, and temperature retention time is 100h, 200h, 300h.Realize boiler superheater tube material under stress state, be in the corrosion experiment under high temperature, coal ash, flue gas medium comprehensive function.
(3) take out sample after sample being corroded, with the lime-ash of acetone solution peace and quiet sample surfaces attachment, dry sample bottom surface of polishing after weighing, by the corrosion depth 60 of scanning electron microscope statistical test sample, pass through formulaIt is calculated following result:
The sample of corrosion 100h, its maximum corrosion depth is 0.091mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.111mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.129mm.
Stressless sample:
The sample of corrosion 100h, its maximum corrosion depth is 0.075mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.102mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.112mm.
Embodiment 3
(1) selecting the HR3C steel that power plant boiler tube is commonly used as experiment material, experimental temperature is 700 DEG C, and etching time is 300h.When 700 DEG C, the elastic modelling quantity of material is E=1.47 × 105MPa, Poisson's ratio μ=0.29, yield strength are 147MPa.Take diameter of the rod d=50mm, outside diameter of cylinder d2=60mm.
700 DEG C, as p=50MPa,
Calculate: C1=1-μ 1=1-0.29=0.71,
Select basic hole system, the most a size of holeAxleMinimum interference amount is 102 μm, and maximum interference amount is 118 μm.
During the μm of δ=102,
During the μm of δ=118,
22MPa<pActual< yield strength 147MPa when 700 DEG C, meets the requirements.
The sample selecting δ=108～114 μm assembles, and guarantees that a bottom surface is plane after assembling, after this bottom surface is used 100#, 200#, 400#, 600# sand papering successively, measures sample weight.
(2) coal ash is to take from the slagging scorification bottom 600 DEG C of superheater tubes, by slagging scorification grind into powder, with the uniform pasty state of acetone soln furnishing, is coated in specimen surface.Placing 12h in environment clean, that be dried, after surface attachment lime-ash solidifies, be placed on specimen mounting by sample, the distance between each sample is 15mm, and specimen mounting puts into tube type resistance furnace.The composition (volume fraction) of forming gas is: 15%CO2+ 3.5%O2+ 1%SO2+ 80.5%N2, the flow entering resistance furnace is 30ml/min, with platinum gauze as catalyst so that reacting 2SO2+O2=2SO3Keep balance.Gas flows out furnace rear and enters tail gas collecting device (the NaOH aqueous solution of 5%).Select one group of sample not applying stress to carry out contrast experiment simultaneously.Select one group of sample not applying stress to carry out contrast experiment simultaneously.
Resistance furnace is increased to 700 DEG C, and temperature retention time is 100h, 200h, 300h.Realize boiler superheater tube material under stress state, be in the corrosion experiment under high temperature, coal ash, flue gas medium comprehensive function.
(3) take out sample after sample being corroded, with the lime-ash of acetone solution peace and quiet sample surfaces attachment, dry sample bottom surface of polishing after weighing, by the corrosion depth 60 of scanning electron microscope statistical test sample, pass through formulaIt is calculated following result:
The sample of corrosion 100h, its maximum corrosion depth is 0.113mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.132mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.149mm.
Stressless sample:
The sample of corrosion 100h, its maximum corrosion depth is 0.095mm,
The sample of corrosion 200h, its maximum corrosion depth is 0.146mm,
The sample of corrosion 300h, its maximum corrosion depth is 0.138mm.
By the experiment of three embodiments, comparing with not applying stress state, apply the sample of stress, extent of corrosion is relatively big, corrodes more serious.Along with SO in corrosive environment2The increase of content, extent of corrosion also increases.
Along with the increase of etching time, the theoretical maximum corrosion depth of sample is gradually increased, and the theoretical maximum corrosion depth of sample is more than all of sample value.Therefore, using the method can play preferably and estimate and the effect of supposition, the degree characterizing unsymmetrical corrosion in this way is feasible in theory.
Example by above-mentioned unsymmetrical corrosion characterizing method, it is known that it is feasible for making to characterize unsymmetrical corrosion in this way.Owing to all of data all derive from the result of actual count, therefore the precision of statistics and the quantity of statistical sample are proposed higher requirement.
Claims (2)
1. test and the method for sign for Utility Boiler Superheater pipe high temperature corrosion for one kind, it is characterised in that experimental technique step is as follows:
(1) selecting the same metal material for boiler superheater tube, be designed to pole and cylinder coupling sample, the size range of pole is Φ 5～Φ 60mm, and matched cylinder thickness range is 3～10mm；Produce the magnitude of interference needed for stress in the range of calculating 500～800 DEG C, assemble after polish；Make 500～800 DEG C between pole and cylinder, to produce the radial stress P yield strength in the range of 22MPa < P < material, use flatulence of heat type method assembling sample；
When using the assembling of flatulence of heat type method, magnitude of interference δtComputing formula:
In formula, P is radial pressure, MPa；C1、C2It is respectively internal member and the stiffness coefficient of external member；μ1、μ2It is respectively internal member and the Poisson's ratio of external member material；C1=1-μ1,D is the nominal diameter at cooperation, d2For the external diameter of external member, mm；E1、E2It is respectively internal member and the elastic modelling quantity of external member, MPa；
According to the magnitude of interference δ tried to achievet, determine magnitude of interference δ scope, take δ=δt± (1～10) μm, processes batch to be tested, selects wherein to be closely sized to d+ δtSample carry out experimentation, actual radial stress is:
Guarantee after assembling that a bottom surface is plane, after this bottom surface is used 100#, 200#, 400#, 600# sand papering successively, measure sample weight；
(2) Korrosionsmedium is the flue gas of simulation boiler tube working environment and actual coal ash, and top dust stratification and the bottom slagging scorification of the Superheater tube of coal-burning power plant taken from by coal ash；Ash/slag is ground into fine powder, with the uniform pasty state of acetone soln furnishing, is coated in specimen surface；Placing 10～12h, after surface attachment lime-ash solidifies, be placed on specimen mounting by sample, the distance between each sample is 5～20mm, and specimen mounting puts into tube type resistance furnace；
Gas O2、CO2、SO2And N2After gas mixing device, forming by volume mark is (3～10) %O2+ (13～18) %CO2+ (0.2～2) %SO2+N2Forming gas, enter the forming gas flow of resistance furnace between 10～60ml/min, gas flows out and enters tail gas collecting device after resistance furnace；Resistance furnace is increased to 500～800 DEG C of temperature, is incubated 100～5000h；Realize boiler superheater tube material under stress state, be in the corrosion experiment under high temperature, coal ash, flue gas medium comprehensive function；Put into one group of sample being not added with stress simultaneously, experimental result is compared；
(3), after to sample high temperature corrosion, take out sample, put in acetone liquid, the lime-ash of peace and quiet specimen surface attachment, then dry, weigh；Polishing sample bottom surface, by the corrosion depth of sample under the scanning electron microscope different etching condition of statistics, estimates maximum corrosion depth by moments estimation method, characterizes the degree of unsymmetrical corrosion on this basis, compares and applies the difference of extent of corrosion before and after stress；Sample size in experiment > 50, it is ensured that the distribution situation of sample reaches unanimity with overall distribution.
The most according to claim 1 for Utility Boiler Superheater pipe high temperature corrosion experiment and the method for sign, it is characterised in that described characterizing method, is to characterize unsymmetrical corrosion degree by moments estimation method；
Assuming to represent with stochastic variable h the degree of depth of corrosion, then obeyed by h and be uniformly distributed, be expressed as h～U [a, b], wherein a represents the minimum-depth of corrosion, and b represents the depth capacity of corrosion；
When sample size is sufficiently large, the distribution situation of sample and overall distribution situation should be identical, estimate population moment by sample moment；
The corrosion depth obtained by experiment is expressed as hi, wherein h represents the degree of depth of corrosion, and i is the sequence number measured, i.e. sample size is N, then i=1,2,3 ... N；
According to the numerical value that obtains of experiment, calculate the second-order central of sample average and sample away from；
Sample average is:
According to equally distributed relevant knowledge, its mathematic expectaion is
Sample average is made to be equal to overall mathematic expectaion:
The second-order central of sample away from for:
Equally distributed variance is: D (X)=(b-a)2/12 (6)
Make sample second-order central away from equal to overall variance, obtain:
By above formula (5) and (7), the N number of h value obtained in conjunction with statistics, the value of a and b in available population distribution, maximum corrosion depth is:
So deduce maximum corrosion depth, the degree of unsymmetrical corrosion is characterized.
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