CN101566555B - High-precision immersed-salt hot corrosion test method - Google Patents
High-precision immersed-salt hot corrosion test method Download PDFInfo
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- CN101566555B CN101566555B CN2009100113494A CN200910011349A CN101566555B CN 101566555 B CN101566555 B CN 101566555B CN 2009100113494 A CN2009100113494 A CN 2009100113494A CN 200910011349 A CN200910011349 A CN 200910011349A CN 101566555 B CN101566555 B CN 101566555B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 62
- 230000007797 corrosion Effects 0.000 title claims abstract description 56
- 238000010998 test method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 52
- 239000000956 alloy Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012153 distilled water Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000011010 flushing procedure Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000005258 corrosion kinetic Methods 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000012360 testing method Methods 0.000 claims description 45
- 230000014759 maintenance of location Effects 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000003643 water by type Substances 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 230000006641 stabilisation Effects 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 4
- 238000006467 substitution reaction Methods 0.000 claims description 2
- 238000010586 diagram Methods 0.000 abstract 2
- 238000004321 preservation Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- 210000000080 chela (arthropods) Anatomy 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910000601 superalloy Inorganic materials 0.000 description 4
- 239000007769 metal material Substances 0.000 description 3
- 229910000905 alloy phase Inorganic materials 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a high-precision immersed-salt hot corrosion test method. The method comprises the following steps: selecting a sample of which surface smoothness is 2.5 microns, cleaning andblow-drying the sample, then putting the sample into an alumina crucible and filling the alumina crucible by salt; putting the crucible into a box muffle furnace at a set temperature, and beginning r ecording time; adding the salt into the crucible at certain period, taking out and cooling the crucible after reaching a set heat preservation time, adding distilled water into the crucible and putting the crucible into a glass dish, pouring the sample and the liquid into a large beaker after the crucible is cooled, repeatedly cleaning the crucible, and filling the liquid into the large beaker; putting the large beaker into a thermostatic water area for 30 to 50 minutes; taking out the large sample and placing the sample at the upper part of a large beaker rim, flushing the sample by the distilled water twice to thrice and then putting the sample into a small beaker; and filtering the solution in the large beaker and flushing a product to the small beaker, drying and weighing the small beaker and recording data, substituting the data into a formula to calculate the mass increment in a unit area, using the mass increment as a longitudinal coordinate and using the heat preservation time as a transverse coordinate to draw a hot corrosion kinetics curve diagram of the sample, and using origin 8.0 software to linearly simulate data points in the diagram to obtain a sample weight increment curvilinear equation, wherein the slope coefficient of the equation is the alloy hot corrosion rate.
Description
Technical field
The present invention relates to a kind of hot corrosion test method, particularly a kind of high-precision immersed-salt hot corrosion test method.
Background technology
When metal material is worked in high temperature (600～1200 ℃) environment,,, when burning, form as SO as sulphur, potassium, sodium, vanadium etc. often owing to the impurity that contains in the fuel
2, SO
3, H
2S, V
2O
5, CO, CO
2Deng reactions such as gas and airborne oxygen, NaCl and the corrosion of accelerated material.Particularly, along with the widespread use of gas turbine in industry such as generating, naval vessel, the acting in conjunction of low-grade fuel and marine atmosphere tends to cause the accelerated corrosion of metal material, sometimes even cause catastrophic accident.Above-mentioned corrosion phenomenon can be summarized as: metal or alloy surface deposition fuse salt (NaCl, Na
2SO
4) and cause corrosion, nowadays this corrosion extensively is called hot corrosion.
Therefore the hot corrosion resistance of metal material is evaluated, and then the level of the hot corrosion resistance of definite material is highly significant.
Summary of the invention
The invention provides a kind of high-precision immersed-salt hot corrosion test method, this method is the mass incremental in the weighing hot corrosion process accurately, makes the confidence level of test figure higher.
A kind of high-precision immersed-salt hot corrosion test method provided by the invention is characterized in that concrete steps are as follows:
(1) test preliminary work:
Select the hot corrosion sample of constant weight alumina crucible and fixed measure for use, the volume that requires sample is less than selecting 1/4th of alumina crucible for use, and it is 2.5 microns that sample surfaces smooth finish will reach Ra;
The serviceability temperature of material is selected suitable test temperature per sample, the empty muffle furnace 40h at least that burns under test temperature, and the empty material that comes off that burns in the clearing furnace of back is in the crucible that prevents to drop in the hot corrosion process of the test;
Alumina crucible is chosen inwall and entire crucible is stand-by after 1100 ℃ of skies burn at least 40h;
Select two kinds of beakers of size for use, the large beaker volume is greater than 1000 times that corrode sample volume, and the small beaker volume is greater than 20 times of corrosion sample volume, and is with alcohol wash beaker inside and outside wall, stand-by after drying up the back weigh and writing down the data of weighing;
Choose temperature retention time;
(2) process of the test:
At first sample is used acetone ultrasonic cleaning 5～10 minutes, the back is taken out and is dried up back measurement size, weigh with alcohol ultrasonic cleaning 1～3 minute.
Then sample is put into the constant weight alumina crucible, sample is placed height should be lower than 1/2nd of the crucible degree of depth, add full crucible with salt, after being warmed up to design temperature etc. box muffle furnace, put into the crucible that sample and salt are housed, treat temperature stabilization opening entry time behind the design temperature, again with salt, be generally 5～10 hours with the salt cycle every some cycles; Take out crucible with crucible tongs after arriving the temperature retention time of testing setting, only allow crucible tongs contact crucible outer wall in the taking-up process, prevent to pick and place and sneak into other material in the crucible process, take out crucible and be placed on air cooling in the glassware, fall into to prevent dust; The cooling back adds distilled water in crucible, guarantee that no liquid overflows, place the sealed glass ware to leave standstill in crucible after adding distilled water, behind the cool to room temperature sample and liquid are poured in the large beaker of constant weight together, by above operation cleaning crucible at least 10 times repeatedly, during the liquid of flushing is all packed large beaker at every turn, will wash the crucible inwall with the wash bottle that distilled water is housed at last, the liquid of flushing is inserted in the large beaker; Add distilled water and make liquid reach 60%～90% of large beaker capacity in large beaker, 30～50min is left standstill in the constant temperature waters of then large beaker being put into temperature and be 70～90 ℃.
From large beaker, take out bulk sample with tweezers afterwards, place the top of beaker mouth, wash sample 2～3 times, sample is put into the constant weight small beaker, be placed in the seal glass ware stand-by with the wash bottle that distilled water is housed; Solution in the large beaker is filtered with quantitative filter paper, and with corroding residue in the distilled water flushing large beaker to filter paper, use the residual corrosion product 5～10 times on the distilled water flushing filter paper then, corrosion product is flushed in the small beaker, at last small beaker is put into drying baker oven dry back and taken out, weigh and record data;
The processing of each sample is carried out according to above identical test procedure fully in the test, the corresponding different temperature retention time of each sample;
(3) calculate:
With the following formula of gained test figure substitution:
Surface area formula: S
Table=2 * (length * wide+wide * height+length * height) ÷ 100
S wherein
Table-surface area of sample, the cm of unit
2Length-sample the length of side, the mm of unit;
Mass incremental: Δ m=m
After-m
Before
Δ m-mass incremental wherein, m
BeforeQuality before the-corrosion, m
After-corrosion back quality, unit is mg;
The mass incremental of unit area: Δ m '=Δ m/S
Table
The mass incremental of Δ m '-unit area wherein, the mg/cm of unit
2
With the temperature retention time is horizontal ordinate, the mass area ratio increment is an ordinate, draw the hot corrosion kinetic curve figure of sample alloy, utilize the data point in this curve map of origin8.0 software linear analogue again, draw the weightening finish curvilinear equation of sample alloy, the slope of gained equation is the hot corrosion speed of this alloy.
Description of drawings
Fig. 1 is that DZ125 and IN738 alloy are at 900 ℃ of following hot corrosion kinetic curve figure;
Fig. 2 is that DZ125L and DZ68 alloy are at 850 ℃ of following hot corrosion kinetic curve figure.
Embodiment
Calculate required formula:
Surface area formula: S
Table=2 * (length * wide+wide * height+length * height) ÷ 100 1)
S wherein
Table-surface area of sample, the cm of unit
2Length-sample the length of side, the mm of unit;
Mass incremental: Δ m=m
After-m
Before2)
Δ m-mass incremental wherein, m
BeforeQuality before the-corrosion, m
After-corrosion back quality, unit is mg;
The mass incremental of unit area: Δ m '=Δ m/S
Table3)
The mass incremental of Δ m '-unit area wherein, the mg/cm of unit
2
Embodiment 1:
Compare the hot corrosion resistance of DZ125 and IN738 alloy, the main chemical compositions of two kinds of nickel base superalloys sees Table 1, and test temperature is chosen as 900 ℃, and the test used salt is: NaCl: Na
2SO
4=1: 3 solid particle requires mechanical means to mix, and needs to prepare the Na of at least 3 bottles of 500g
2SO
4NaCl with 1 bottle of 500g.18 time points that test is chosen see Table 2, each 18 in the sample of two kinds of alloys of selection, and sample size is 10 * 10 * 15mm, and surface smoothness is the Ra=2.5 micron; Select 60 alumina crucibles, size is: height 30mm, inside diameter ranges
Prepare 2 large beakers that volume is 1500ml, 2 volumes are the small beaker of 100ml.
The chemical constitution of table 1DZ125 and IN738 alloy (weight percentage, %)
Test required instrument and equipment:
Alumina crucible, stainless steel crucible pincers, beaker, precision 100,000/ electronic balance, drying baker, constant temperature waters heating instrument, muffle furnace, wash bottle, ultrasonic cleaning instrument, vernier caliper, antimagnetic type tweezer, electric blower, funnel.
Test required reagent:
Distilled water, quantitative filter paper at a slow speed, acetone, alcohol, Na
2SO
4And NaCl.
(1) test preliminary work:
1) with the DZ125 that processes and the sample of IN738 nickel base superalloy, with acetone ultrasonic cleaning 8 minutes, used the alcohol ultrasonic cleaning then 2 minutes, take out and dry up the back and uses the vernier caliper measurement size, use the electronic balance weigh, record data are in table 2, table 3.
2) the empty muffle furnace 40h that burns under 900 ℃ of temperature cleans out burner hearth after empty the burning.
3) with 60 alumina crucibles 1100 ℃ empty burn 40h after, therefrom choose inwall and entire 36 crucibles are stand-by.
4) with the large beaker of the 1500ml that selects for use and the small beaker of 100ml, use the alcohol wash inside and outside wall, dry up back weighing small beaker weight, and stand-by behind the record data, and the small beaker quality is 76.8574g.
(2) test operation step:
1) sample shove charge
Get DZ125 and IN738 alloy phase with each one in the sample of temperature retention time, put into alumina crucible respectively, and in crucible, fill it up with salt, after muffle furnace reaches 900 ℃, two crucibles are put in the stove, and the opening entry time behind temperature stabilization to 900 ℃, the cycle of adding salt is 6h.
2) sample comes out of the stove
With temperature retention time 1h is example: after temperature retention time arrives 1h, with the stainless steel crucible pincers two crucibles are taken out respectively, only allow crucible tongs contact crucible outer wall in the crucible taking-up process, prevent to pick and place and sneak into other material in the crucible process, the crucible of taking-up is placed on glassware hollow and is chilled to room temperature.
It is the same that sample At All Other Times goes out furnace operating.
3) cleaning of sample
In the crucible of cool to room temperature, add distilled water, will guarantee in the adding distil water process that no liquid overflows; Place in the sealed glass ware behind the crucible adding distilled water and leave standstill 1.5h, then sample and liquid one are played in the large beaker of constant weight; By above operation cleaning crucible 12 times repeatedly, the liquid that at every turn washes crucible is all packed in the large beaker of constant weight, at last will be with the wash bottle flushing crucible inwall that distilled water is housed 3 times, and the liquid of flushing is inserted in the large beaker.In large beaker, add distilled water and make amount of liquid reach 1000ml, then beaker is put into temperature and be 90 ℃ constant temperature waters and place 40min.
4) weighing of corrosion back sample
Behind the constant temperature waters heating 40min, from large beaker, take out bulk sample with antimagnetic type tweezer, be placed on the top of beaker mouth, wash the folded sample of tweezers 3 times with the wash bottle that distilled water is housed, then sample is put into the 100ml small beaker of constant weight, placed the sealed glass ware stand-by.Solution in the large beaker is filtered, filter paper is selected quantitative filter paper at a slow speed for use, and with corroding residue in the distilled water flushing large beaker to filter paper, use the residual corrosion product 8 times on the distilled water flushing filter paper then, at last corrosion product is flushed in the small beaker, the constant weight small beaker is put into drying baker oven dry after, with the weight of electronic balance weighing beaker and sample and, sample actual weight after the quality that deducts small beaker then obtains corroding, and record data are in table 2, table 3.
The processing of each sample in the test is carried out according to above identical test procedure fully, requires the corresponding fixing temperature retention time of a sample.
(3) test findings and analysis:
The hot corrosion test figure of two kinds of alloys sees Table 2 and table 3 respectively, table 2 be the DZ125 alloy at 900 ℃, the test figure after the different time hot corrosion, table 3 be the IN738 alloy at 900 ℃, the test figure after the different time hot corrosion.Wherein surface area calculates according to formula 1) calculate, increase quality Δ m according to formula 2) calculate, the mass incremental of unit area is according to formula 3) calculate, with outcome record in table 2, table 3.
900 ℃ of different time salt-coated tests of table 2 DZ125 alloy data
The salt-coated test data of 900 ℃ of different times of table 3 IN738 alloy
According to table 2,3 data, with the temperature retention time is horizontal ordinate, the mass area ratio increment is an ordinate, utilizes the Origin8.0 mapping software to draw the hot corrosion kinetic curve of DZ125 and IN738 alloy, and Fig. 1 is 900 ℃ of hot corrosion kinetic curve figure of DZ125 and IN738 alloy.
Utilize the data point among origin8.0 software linear analogue Fig. 1.Draw the weightening finish curvilinear equation of DZ125 and IN738 alloy, the weightening finish curvilinear equation of DZ125 alloy is y=59.6x-54, and the weightening finish curvilinear equation of IN738 alloy is y=2.13x+2.73.
The slope of analog linearity equation is the hot corrosion speed of alloy, and under test condition, the hot corrosion speed of DZ125 alloy is 59.6mg/ (cm
2* h), the hot corrosion speed of IN738 alloy is 2.13mg/ (cm
2* h), the hot corrosion speed of visible DZ125 alloy shows that significantly greater than the IN738 alloy corrosion and heat resistant ability of DZ125 alloy significantly is lower than the IN738 alloy.
Embodiment 2:
Compare the hot corrosion resistance of DZ125L and DZ68 alloy, the main chemical compositions of two kinds of nickel base superalloys sees Table 4, and test temperature is chosen as 850 ℃, and the test used salt is: NaCl: Na
2SO
4=1: 2 solid particle requires mechanical means to mix, and needs to prepare the Na of at least 2 bottles of 500g
2SO
4NaCl with 1 bottle of 500g.8 time points that test is chosen see Table 5, each 8 in the sample of two kinds of alloys of needs, and sample size is 10 * 10 * 10mm, surface smoothness is the Ra=2.5 micron; Select 40 alumina crucibles, crucible all is of a size of: highly be 30mm, inside diameter ranges is φ 18～φ 30mm; Prepare 2 large beakers that volume is 1000ml, 2 volumes are the small beaker of 50ml.
The chemical constitution of table 4 DZ125L and DZ68 alloy (weight percentage, %)
Test required instrument and equipment:
Alumina crucible, stainless steel crucible pincers, beaker, precision 100,000/ electronic balance, drying baker, constant temperature waters heating instrument, muffle furnace, wash bottle, ultrasonic cleaning instrument, vernier caliper, antimagnetic type tweezer, electric blower, funnel.
Test required reagent:
Distilled water, quantitative filter paper at a slow speed, acetone, alcohol, Na
2SO
4And NaCl.
The preliminary work of test:
1) with the DZ125L that processes and the sample of DZ68 nickel base superalloy, with acetone ultrasonic cleaning 7 minutes, used the alcohol ultrasonic cleaning then 3 minutes, take out and dry up the back and uses the vernier caliper measurement size, use the electronic balance weigh, record data are in table 5, table 6.
2) the empty muffle furnace 50h that burns under 850 ℃ of temperature cleans out burner hearth after empty the burning.
3) with 40 alumina crucibles 1100 ℃ empty burn 50h after, therefrom choose inwall and entire 16 crucibles are stand-by.
4) with the large beaker of the 1000ml that selects for use and the small beaker of 50ml, use the alcohol wash inside and outside wall, dry up back weighing small beaker weight, and stand-by behind the record data, and 50ml beaker quality is 33.8581g.
Hot corrosion test operation step:
1) sample shove charge
Get DZ125L and DZ68 alloy phase with each one in the sample of temperature retention time, put into alumina crucible respectively and add fullly with salt, after muffle furnace reaches 850 ℃, two crucibles are put in the stove, the opening entry time behind temperature stabilization to 850 ℃, the cycle of adding salt is 10h.
2) sample comes out of the stove
With temperature retention time 3h is example: after temperature retention time arrives 3h, with the stainless steel crucible pincers two crucibles are taken out respectively, only allow crucible tongs contact crucible outer wall in the crucible taking-up process, prevent to pick and place and sneak into other material in the crucible process, the crucible of taking-up is placed on glassware hollow and is chilled to room temperature.
It is the same that sample At All Other Times goes out furnace operating.
3) cleaning of sample
In the crucible of cool to room temperature, add distilled water, will guarantee in the adding distil water process that no liquid overflows; Place in the sealed glass ware behind the adding distilled water in the crucible and leave standstill 1h, then sample and liquid one are played in the large beaker of constant weight; By above operation cleaning crucible 10 times repeatedly, the liquid that at every turn washes crucible is all packed in the large beaker of constant weight, at last will be with the wash bottle flushing crucible inwall that distilled water is housed 3 times, and the liquid of flushing is inserted in the large beaker.Add distilled water to large beaker then and make amount of liquid reach 800ml, then beaker is put into temperature and be 80 ℃ constant temperature waters and place 50min.
4) weighing of corrosion back sample
Behind the constant temperature waters heating 50min, from large beaker, take out bulk sample with antimagnetic type tweezer, be placed on the top of beaker mouth, wash the folded sample of tweezers 2 times with the wash bottle that distilled water is housed, sample is put into the 50ml small beaker of constant weight, place the sealed glass ware stand-by.Solution in the large beaker is filtered, filter paper is selected quantitative filter paper at a slow speed for use, and with corroding residue in the distilled water flushing large beaker to filter paper, use the residual corrosion product 9 times on the distilled water flushing filter paper then, at last corrosion product is flushed in the small beaker, the constant weight small beaker is put into drying baker oven dry after, with the weight of electronic balance weighing beaker and sample and, sample actual weight after the quality that deducts small beaker obtains corroding then, and record data are in table 5, table 6.
The processing of each sample in the test is carried out according to above identical test procedure fully, requires the corresponding fixing temperature retention time of a sample.
Test findings and analysis:
The hot corrosion test figure of two kinds of alloys sees Table 5 and table 6 respectively.Table 5 is the test figure of DZ125L alloy after 850 ℃ of different time hot corrosions, table 6 is DZ125L, the test figure of DZ68 alloy after 850 ℃ of different time hot corrosions, wherein surface area calculates according to formula 1) calculate, increase quality Δ m according to formula 2) calculate, the mass incremental of unit area is according to formula 3) calculate, with outcome record in table 5, table 6.
According to table 5,6 data, with the temperature retention time is horizontal ordinate, the mass area ratio increment is an ordinate, utilizes the Origin8.0 mapping software to draw the hot corrosion kinetic curve of DZ125L and DZ68 alloy, and Fig. 2 is 850 ℃ of hot corrosion kinetic curve figure of DZ125L and DZ68 alloy.
Distribute from the visible non-linear rule of data point distribution, therefore utilize the data point in the heterogeneous formula simulation drawing 2 of secondary of origin8.0 software, draw the weightening finish curvilinear equation of DZ125L and DZ68 alloy, the weightening finish curvilinear equation of DZ125L alloy is y=2.35+0.32x-0.008x
2, the weightening finish curvilinear equation of DZ68 alloy is y=0.79-0.08x+0.003x
2
850 ℃ of different time salt-coated tests of table 5DZ125L alloy data
850 ℃ of table 6DZ68 alloys, different time salt-coated test data
Ask first order derivative to obtain the corrosion rate equation of change of two kinds of alloys to the weightening finish curve's equation of DZ125L and DZ68 alloy, DZ125L is: dy/dx=0.32-0.016x, DZ68 is: dy/dx=-0.08+0.006x.
From the corrosion rate equation of change as seen, having for a long time hot corrosion incubation period of DZ68 alloy, and the hot corrosion of DZ125L alloy is very short incubation period, be no more than 50h in temperature retention time, the corrosion rate of DZ68 alloy is greater than the DZ125L alloy, that is to say that the hot corrosion resistance of DZ68 alloy is significantly better than the DZ125L alloy when 850 ℃ of temperature retention times are no more than 50h.Along with temperature retention time surpasses 50h, serious hot corrosion has all taken place in two kinds of alloys.
Claims (1)
1. high-precision immersed-salt hot corrosion test method is characterized in that:
(1) test preliminary work:
Select the hot corrosion sample of constant weight alumina crucible and fixed measure for use, the volume that requires sample is less than selecting 1/4th of alumina crucible for use, and it is 2.5 microns that sample surfaces smooth finish will reach Ra;
The serviceability temperature of material is selected suitable test temperature per sample, the empty muffle furnace 40h at least that burns under test temperature, the empty material that comes off that burns in the clearing furnace of back;
Alumina crucible is chosen inwall and entire crucible is stand-by after 1100 ℃ of skies burn at least 40h;
Select two kinds of beakers of size for use, the large beaker volume is greater than 1000 times that corrode sample volume, and the small beaker volume is greater than 20 times of corrosion sample volume, and is with alcohol wash beaker inside and outside wall, stand-by after drying up the back weigh and writing down the data of weighing;
Choose temperature retention time;
(2) process of the test:
At first sample is used acetone ultrasonic cleaning 5～10 minutes, the back is taken out and is dried up back measurement size, weigh with alcohol ultrasonic cleaning 1～3 minute; Then sample is put into the constant weight alumina crucible, sample is placed height should be lower than 1/2nd of the crucible degree of depth, add full crucible with salt, after being warmed up to design temperature etc. box muffle furnace, put into the crucible that sample and salt are housed, treat temperature stabilization opening entry time behind the design temperature, every some cycles again with salt, with the salt cycle be 5～10 hours; Take out crucible with crucible tongs after arriving the temperature retention time of testing setting, only allow crucible tongs contact crucible outer wall in the taking-up process, take out crucible and be placed on air cooling in the glassware; The cooling back adds distilled water in crucible, guarantee that no liquid overflows, place the sealed glass ware to leave standstill in crucible after adding distilled water, behind the cool to room temperature sample and liquid are poured in the large beaker of constant weight together, by above operation cleaning crucible at least 10 times repeatedly, during the liquid of flushing is all packed large beaker at every turn, will wash the crucible inwall with the wash bottle that distilled water is housed at last, the liquid of flushing is inserted in the large beaker; Add distilled water and make liquid reach 60%～90% of large beaker capacity in large beaker, 30～50min is left standstill in the constant temperature waters of then large beaker being put into temperature and be 70～90 ℃; From large beaker, take out bulk sample with tweezers, place the top of beaker mouth, wash sample 2～3 times, sample is put into the constant weight small beaker, be placed in the seal glass ware stand-by with the wash bottle that distilled water is housed; Solution in the large beaker is filtered with quantitative filter paper, and with corroding residue in the distilled water flushing large beaker to filter paper, use the residual corrosion product 5～10 times on the distilled water flushing filter paper then, corrosion product is flushed in the small beaker, at last small beaker is put into drying baker oven dry back and taken out, weigh and record data;
The processing of each sample is carried out according to above identical test procedure fully in the test, the corresponding different temperature retention time of each sample;
(3) with the following formula of gained test figure substitution:
Surface area formula: S
Table=2 * (length * wide+wide * height+length * height) ÷ 100
S wherein
Table-surface area of sample, the cm of unit
2Length-sample the length of side, the mm of unit;
Mass incremental: Δ m=m
After-m
Before
Δ m-mass incremental wherein, m
BeforeQuality before the-corrosion, m
After-corrosion back quality, unit is mg;
The mass incremental of unit area: Δ m '=Δ m/S
Table
The mass incremental of Δ m '-unit area wherein, the mg/cm of unit
2
With the temperature retention time is horizontal ordinate, the mass area ratio increment is an ordinate, draw the hot corrosion kinetic curve figure of sample alloy, utilize the data point in this curve map of origin8.0 software linear analogue again, draw the weightening finish curvilinear equation of sample alloy, the slope of gained equation is the hot corrosion speed of this alloy.
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| CN105445172B (en) * | 2015-11-10 | 2018-06-05 | 中国航空工业集团公司北京航空材料研究院 | Aluminum alloy surface corrosion tests under one kind of multiple solid particle absorption |
| CN106442300A (en) * | 2016-11-21 | 2017-02-22 | 中国科学院金属研究所 | High-accuracy spray deposition salt hot corrosion experiment method |
| CN106908373B (en) * | 2017-03-09 | 2019-05-10 | 青海大学 | The experimental method of low-density fibre material corrosion behavior in medium of fused salt |
| CN109856038B (en) * | 2019-01-23 | 2022-01-18 | 国核宝钛锆业股份公司 | Test method for accelerating uniform corrosion of zirconium alloy |
| CN110132826A (en) * | 2019-04-12 | 2019-08-16 | 西北工业大学 | The test method of nickel-base high-temperature single crystal alloy hot corrosion resistance |
| CN112326541A (en) * | 2020-10-12 | 2021-02-05 | 安工腐蚀检测实验室科技（无锡）有限公司 | Automatic corrosion simulation tester device |
| CN112924256A (en) * | 2021-01-29 | 2021-06-08 | 西安热工研究院有限公司 | Preparation method of corrosion test piece surface salt film |
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| EP0186383A1 (en) * | 1984-12-11 | 1986-07-02 | Westinghouse Electric Corporation | Method of determining corrosion resistance |
| US4902625A (en) * | 1984-12-11 | 1990-02-20 | Westinghouse Electric Corp. | Rapid corrosion test for zirconium and zirconium alloy weldments |
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| EP0186383A1 (en) * | 1984-12-11 | 1986-07-02 | Westinghouse Electric Corporation | Method of determining corrosion resistance |
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| US4902625A (en) * | 1984-12-11 | 1990-02-20 | Westinghouse Electric Corp. | Rapid corrosion test for zirconium and zirconium alloy weldments |
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