CN104713759A - Method for detecting surface oxidized scale sample of hot rolled steel plate - Google Patents
Method for detecting surface oxidized scale sample of hot rolled steel plate Download PDFInfo
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- CN104713759A CN104713759A CN201510075957.7A CN201510075957A CN104713759A CN 104713759 A CN104713759 A CN 104713759A CN 201510075957 A CN201510075957 A CN 201510075957A CN 104713759 A CN104713759 A CN 104713759A
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Abstract
The invention provides a method for detecting a surface oxidized scale sample of a hot rolled steel plate, aims to overcome the defects of a conventional test sample preparation method and checking method of hot rolled metal oxidized scale, and belongs to the field of back scattering image analysis of a surface layer structure of a high-temperature oxidized metal. The method specifically comprises the following steps: putting a metal sample which is oxidized at high temperature into a non-metal tube, performing cold embedding by using liquid epoxy resin and a curing agent of the liquid epoxy resin, and implementing processes such as grinding, polishing, corrosion by using a nitric acid ethanol mixed solution and surface carbon plating, so as to finally obtain a metal cross section oxidized scale sample which is applicable to observation by using a field emission electronic probe. Due to the adoption of the method, the oxidized scale sample of which metal is subjected to high-temperature oxidization is relatively easily and conveniently prepared, the loose phase of Fe2O3, Fe3O4 and FeO on an outer layer can be effectively protected by the epoxy resin in a cold state, and the surface oxidized scale can be prevented from dropping off in hot embedding. Through corrosion by using a mixed solution of nitric acid and ethanol, the structure of the surface oxidized scale and the metallographic phase of a metal substrate can be clearly revealed after corrosion, and the imaging effect can be relatively clear.
Description
Technical field
The invention belongs to the back scattered image analysis field of the surface structure of metallic high temperature oxidation, particularly a kind of detection method of hot rolled steel plate surface oxidation iron sheet sample.
Background technology
At present, along with increasing hot-rolled product just progressively replaces the cold-rolled products of same specification, thus the surface quality requirements of user to hot-strip is more and more higher.Although the iron and steel enterprise of China has progressively paid attention to the surface quality of hot-rolled product in recent years, surface imperfection has also frequently occurred, causes the surface and the internal soundness that reduce steel, makes deep processing rejection rate severe overweight subsequently, strip plate surface smoothness extreme difference.Therefore, in order to strengthen the competitive power of China's hot rolling slab, the quality control on the surface of hot-strip is exactly the direction that we concentrate research now.The subject matter of Surfaces of Hot Rolled Strip quality is exactly that scale structure control is improper, the iron sheet press-in that the peeling off of iron scale causes and make belt steel surface occur part or large-area red rust and the surface imperfection such as pit, pitted skin is the problem of puzzlement hot rolling slab surface quality always.Therefore study iron scale structure at different conditions and thickness, grasp the formation mechenism of different scale structure, and then the formation controlling it is necessary.
The heat that the preparation method of sample of current hot-rolling metal iron scale mainly adopts is inlayed, as shown in patent CN-101856669-A, the shortcoming that heat is inlayed is, owing to needing the shaping loading force carrying out 50-130 DEG C of heating and 80-300bar in heating process, iron scale sample is at hot mosaic process generating portion stress, iron scale is broken and inclination easily, and this has just manufactured very large difficulty for the detection of iron scale.Secondly current corrosive liquid is the mixed solution of acidic alcohol, and its shortcoming is scale structure to be corroded out and cannot erode away metallic matrix structure, is unfavorable for the detection of iron scale matrix.The metaloscope that the equipment of current detection iron scale mainly uses, its shortcoming is that the imaging effect of light microscopic is unintelligible, cannot reach the testing requirement to accurate scale structure and thickness.
Summary of the invention
The object of the invention is the defect existed for preparation method of sample and the inspection method of current hot-rolling metal iron scale, provide a kind of detection method of hot rolled steel plate surface oxidation iron sheet sample.The method is simple to operation, can also play a protective role to high temperature rear oxidation iron sheet sample, and can obtain the structure of iron scale and metallic matrix more clearly and organize picture.
A detection method for hot rolled steel plate surface oxidation iron sheet sample, comprises the following steps:
(1) sample
Heat-obtaining rolled steel plate sample, good specification is thickness 2-4.5mm;
(2) Pipe Cutting
Be the section of iron scale sample long side surface due to what need to observe, so choose the non-metal pipe that diameter is greater than sample length, the length and the Sample Width that intercept tubing are close, and good length is Sample Width ± 5mm;
Described non-metal pipe is not containing metal ingredient, do not react with epoxy resin, fusing point higher than the tubing of 50 DEG C, such as, pvc pipe, PPR pipe, PE pipe etc.;
(3) inlay
By the epoxy resin of liquid state and hardening agent mixing and stirring, slant setting is until bubble collapse in medium;
Seal up tubing side, sample is put into tubing cavity, make a long side surface contact of sample on sealing surface, in tubing, multiple sample can be placed; Then joined by epoxy resin medium in tubing cavity, medium wraps sample, until cover sample completely uniformly by the liquid fluidity of self; 3 ~ 6 hours are solidified, the obtained sample fixed in the baking oven again tubing being placed in 40 ~ 50 DEG C;
(4) polish
Polish with the section of sand paper to the sample fixed having low granularity to high granularity successively, be preferably the SiC sand paper of 800#, 1000#, 1200# and 1500# to the sand paper of high granularity by low granularity, the cut of polishing to sample is the granularity of last specification sand paper; Polishing adopts manual water mill, and with free-pouring pure water for medium, polishing is carried out with flushing simultaneously;
(5) polishing
Employing specification is that the sample section of having polished is carried out polishing by the abrasive pastes of W2.5-3.5 on buffing machine, removes the cut of sand papering; Specification is adopted to be the abrasive pastes polishing 5 ~ 15min of W0.5-1.5 again; Finally with clear water or alcohol polishing 5 ~ 15min, obtain the sample of polished hot rolled steel plate surface oxidation iron sheet; The rotating speed of buffing machine is 800 ~ 1000r/min preferably;
(6) chemical corrosion
Be make corrosive liquid after the nitric acid of 50-70% and ethanol mixing by mass concentration, in corrosive liquid, the percent by volume of nitric acid is 3-7%; Corrosive liquid is dripped to polished sample section, after corrosion 3 ~ 10s, sample is immersed in 5 ~ 10min in alcohol or acetone soln, then air-dry or dry up;
(7) microscopic examination
Adopt field emission electron probe (EPMA) to observe the section of iron scale sample, complete detection;
In order to increase the electric conductivity of sample, before detection the sample corroded can be put into high vacuum vapor deposition instrument and plating carbon.
Technical characterstic of the present invention:
(1) the present invention adopts cold method for embedding; solidify in the baking box of 40 ~ 50 DEG C; liquid-state epoxy resin has good mobility; avoid the crimp of sample oxidation iron sheet in high temperature mosaic process or come off; and prevent the inclination of sample; as long as the degree of tilt of sample can be adjusted before epoxy resin cure, and can the loose Fe of available protecting skin by the epoxy resin under cold state
2o
3, Fe
3o
4, FeO phase.Epoxy resin after solidification has the heat resistance of excellent mechanical property, chemical resistance, excellent electrical property and brilliance.
(2) what the corrosive liquid in the present invention adopted is make mixed solution after nitric acid and ethanol mix, and in mixed solution, the percent by volume of nitric acid is 3-7%, and the weight concentration of nitric acid is 50-70%; With glue head dropper, corrosive liquid is dripped to polished sample surfaces, after corrosion 3 ~ 10s, sample is soaked fully in alcohol or acetone soln, and then with the rapid draing of hair-dryer hot blast.Scale structure and metallic matrix metallographic structure can be corroded out convenient detection.
(3) the present invention adopts the backscattered electron in field emission electron probe (EPMA) to carry out sample detection.Backward scattering utilizes electronics elastic scattering dorsad, increases imaging from the quantity of the backscattered electron of sample surfaces effusion with the increase of average atomic mass solid and sample Local Phase for the increase at the inclination angle of incoming beam.Thus the structure of iron scale and metal collective more clearly can be obtained and organize picture.
Accompanying drawing explanation
Fig. 1 is the hot rolled steel plate surface oxidation iron sheet sample section schematic diagram that the present invention obtains;
Wherein, 1, tubing, 2, epoxy resin, 3, metallic matrix, 4, iron scale;
Fig. 2 is the hot rolled steel plate surface oxidation iron sheet sample object figure that the embodiment of the present invention 1 obtains;
Fig. 3 is the EPMA backward scattering detection figure of the hot rolled steel plate surface oxidation iron sheet sample section structure that the embodiment of the present invention 1 obtains;
Wherein, a, Fe
2o
3layer, b, Fe
3o
4layer, c, FeO layer, d, FeO eutectoid product, e, metallic matrix;
Fig. 4 is the EPMA backward scattering detection figure of the metallic matrix tissue of the hot rolled steel plate surface oxidation iron sheet sample section detection that the embodiment of the present invention 1 obtains;
Fig. 5 is the EPMA backward scattering detection figure of the hot rolled steel plate surface oxidation iron sheet sample section structure that the embodiment of the present invention 2 obtains;
Wherein, f, Fe
3o
4layer, g, FeO layer, h, metallic matrix;
Fig. 6 is the EPMA backward scattering detection figure of the metallic matrix tissue of the hot rolled steel plate surface oxidation iron sheet sample section that the embodiment of the present invention 2 obtains;
Fig. 7 is the EPMA backward scattering detection figure of the hot rolled steel plate surface oxidation iron sheet sample section structure that the embodiment of the present invention 3 obtains;
Wherein, i, Fe
2o
3layer, j, Fe
3o
4layer, k, FeO layer, l, FeO eutectoid product, m, metallic matrix;
Fig. 8 is the EPMA backward scattering detection figure of the hot rolled steel plate surface oxidation iron sheet sample section structure that the embodiment of the present invention 4 obtains;
Wherein, n, Fe
2o
3layer, o, Fe
3o
4layer, p, FeO layer, q, FeO eutectoid product, x, metallic matrix.
Embodiment
The liquid-state epoxy resin adopted in the embodiment of the present invention and hardening agent are chemical products, and ethanol is industrial products, and nitric acid is industrial products, and PVC, PE and PPR pipe are common building pipe, and sand paper is SiC sand paper, and abrasive pastes are artificial diamond paste.
Field emission electron probe (EPMA) model is JXA-8530F.
The 208C High that Cressington company of high vacuum Du Tanyishi Britain produces.
Embodiment 1
1, sample F e-Cr alloy is heated to 1100 DEG C, be incubated with stove cool to room temperature after 2 hours, then adopt wire cutting method to cut out section on hot-strip, long 8mm, wide 10mm, thickness is 2.2mm, is that cleaning fluid removes surface and oil contaminant with acetone;
2, cut-off footpath is the pvc pipe of 15mm, adopts one section that cutter intercepting 12mm is long;
3, cut the oilpaper of one piece of 30 × 30mm, with solid gum, oilpaper is sealed pvc pipe side; Again the epoxy resin of liquid state and hardening agent are weighed in proportion, pour in beaker, stir with glass bar, slant setting 25min, until the bubble collapse in medium;
Sample is vertically put into tubing, and make a long side surface contact of sample on sealing surface, outwardly, as depicted in figs. 1 and 2, the sample section seen is long side surface outwardly to another long side surface; Dip epoxy resin medium with glass bar, be added dropwise in pvc pipe along tube wall, epoxy resin medium wraps sample, until cover sample uniformly by the liquid fluidity of self; Static placement is after 10 minutes, places 4 hours, then turn off heating power supply by sample cool to room temperature in drying baker, the obtained sample fixed in the drying baker sample inlayed being placed on 50 DEG C;
4,800# is adopted successively, 1000#, the section of SiC sand paper to sample long side surface of 1200# and 1500# is polished, what polishing adopted is manual water mill, with free-pouring water for medium, polishing is carried out with rinsing simultaneously, before entering next stage sand paper, needs to grind sample until remove the wearing depth that upper level sand paper causes completely;
5, the sample section of having polished is carried out polishing, adopt granularity to be the abrasive pastes of W2.5, on the metallic phase polisher milling of rotary speed 900r/min, the cut of SiC sand paper is removed in polishing; Granularity is adopted to be the abrasive pastes of W1.0 again, polishing 15min on the metallic phase polisher milling of same rotating speed; Finally use clear water polishing 15min on the metallic phase polisher milling of same rotational speed;
6, make mixed solution by after the nitric acid of mass concentration 50% and ethanol mixing, in mixed solution, the percent by volume of nitric acid is 3.5%; With glue head dropper, corrosive liquid is dripped to polished sample section, after corrosion 8s, sample is soaked 7min in ethanol, and then with the rapid draing of hair-dryer hot blast;
7, the sample corroded is put into high vacuum vapor deposition instrument and plate carbon;
8, adopt field emission electron probe (EPMA) to observe the section of iron scale sample in the sample after plating carbon, complete the detection of the scale structure of high-temperature oxydation.
Can be seen the Fe-Cr alloy sample inlayed by Fig. 2, iron scale is complete, without broken and inclination; Can be seen by field emission electron probe (EPMA) the backward scattering detection figure of Fig. 3 and Fig. 4, under EPMA, observe iron scale overall picture, iron scale one-piece construction is intact, does not occur crackle, and skin is completely wrapped in epoxy resin.Observe iron scale backward scattering picture and can pick out Fe one by one
2o
3layer, Fe
3o
4pro-eutectoid Fe in layer, FeO layer and FeO layer
3o
4structure.The metallographic pattern of the matrix of metal can also be observed simultaneously.
Embodiment 2
1, sample F e-Cr alloy is heated to 800 DEG C, is incubated after 2 hours with stove cool to room temperature; Adopt wire cutting method on hot-strip, to cut out section, long 11mm, wide 8mm, thickness is 2.3mm, is that cleaning fluid removes surface and oil contaminant with acetone;
2, cut-off footpath is the PE pipe of 20mm, adopts one section that cutter intercepting 13mm is long;
3, cut one piece of oilpaper, with solid gum, oilpaper is sealed PE pipe side; The epoxy resin of liquid state and hardening agent are weighed in proportion, is poured in beaker, stirs with glass bar, slant setting 10 ~ 30min, until the bubble collapse in medium;
Sample is vertically put into tubing, and make a long side surface contact of sample on sealing surface, another long side surface outwardly; Dip epoxy resin medium with glass bar, along in tube wall instillation PE pipe, epoxy resin medium wraps sample, until cover sample uniformly by the liquid fluidity of self; Place 6 hours in the drying baker sample inlayed being placed on 40 DEG C, then turn off heating power supply by sample cool to room temperature in drying baker, the obtained sample fixed;
4, adopt 800# successively, the SiC sand paper of 1000#, 1200# and 1500# is polished to section, what polishing adopted is manual water mill, with free-pouring water for medium, polishing is carried out with rinsing simultaneously, and the cut of polishing to sample is the granularity of last specification sand paper;
5, the sample section of having polished is carried out polishing, adopt granularity to be the abrasive pastes of W3.5, on the metallic phase polisher milling of rotary speed 1000r/min, the cut of SiC sand paper is removed in polishing; Granularity is adopted to be the abrasive pastes of W1.5 again, polishing 5min on the metallic phase polisher milling of same rotating speed; Finally use alcohol polishing 10min on the metallic phase polisher milling of same rotational speed;
6, make mixed solution by after mass concentration 50% nitric acid and ethanol mixing, in mixed solution, the percent by volume of nitric acid is 5%; By with glue head dropper, corrosive liquid is dripped to polished sample section, after corrosion 5s, sample is soaked 5min in acetone soln, and then with the rapid draing of hair-dryer hot blast;
7, sample is put into high vacuum vapor deposition instrument, allow the sample section corroded plate one deck carbon;
8, adopt field emission electron probe (EPMA) to observe the section of iron scale sample, complete the detection of the scale structure of high-temperature oxydation.
Can see that field emission electron probe (EPMA) backward scattering of this sample section structure detects figure by Fig. 5 and Fig. 6.
Embodiment 3
1, sample F e-Cr alloy is heated to 900 DEG C, is incubated after 2 hours with stove cool to room temperature; Adopt wire cutting method on hot-strip, to cut out section, long 10mm, wide 12mm, thickness is 2.35mm, is that cleaning fluid removes surface and oil contaminant with acetone;
2, cut-off footpath is the PPR pipe of 15mm, adopts one section that cutter intercepting 12mm is long;
3, cut one piece of oilpaper, with solid gum, oilpaper is sealed PPR pipe side; The epoxy resin of liquid state and hardening agent are weighed in proportion, is poured in beaker, stirs with glass bar, slant setting 10 ~ 30min, until the bubble collapse in medium;
Sample is vertically put into tubing, and make a long side surface contact of sample on sealing surface, another long side surface outwardly; Dip epoxy resin medium with glass bar, from tube wall instillation PPR pipe, epoxy resin medium wraps sample, until cover sample uniformly by the liquid fluidity of self; Place 3.5 hours in the drying baker sample inlayed being placed on 45 DEG C, then turn off heating power supply by sample cool to room temperature in drying baker, the obtained sample fixed;
4, adopt 800# successively, the SiC sand paper of 1000#, 1200# and 1500# is polished to section, what polishing adopted is manual water mill, with free-pouring water for medium, polishing is carried out with rinsing simultaneously, and the cut of polishing to sample is the granularity of last specification sand paper;
5, the sample section of having polished is carried out polishing, adopt granularity to be the abrasive pastes of W2.5, on the metallic phase polisher milling of rotary speed 800r/min, the cut of SiC sand paper is removed in polishing; Granularity is adopted to be the abrasive pastes of W0.5 again, polishing 15min on the metallic phase polisher milling of same rotating speed; Finally use clear water polishing 5min on the metallic phase polisher milling of same rotational speed;
6, make mixed solution by after mass concentration 60% nitric acid and ethanol mixing, in mixed solution, the percent by volume of nitric acid is 5%; By with glue head dropper, corrosive liquid is dripped to polished sample section, after corrosion 10s, sample is soaked 10min in alcoholic solution, and then with the rapid draing of hair-dryer hot blast;
7, the sample corroded is put into high vacuum vapor deposition instrument and plate carbon;
8, adopt field emission electron probe (EPMA) to observe the section of iron scale sample, complete the detection of the scale structure of high-temperature oxydation.
Can see that field emission electron probe (EPMA) backward scattering of this sample section structure detects figure by Fig. 7.
Embodiment 4
1, sample F e-Cr alloy is heated to 1000 DEG C, is incubated after 2 hours with stove cool to room temperature; Adopt wire cutting method on hot-strip, to cut out section, long 8mm, wide 12mm, thickness is 2.2mm, is that cleaning fluid removes surface and oil contaminant with acetone;
2, cut-off footpath is the pvc pipe of 15mm, adopts one section that cutter intercepting 10mm is long;
3, cut one piece of oilpaper, with solid gum, oilpaper is sealed pvc pipe side; The epoxy resin of liquid state and hardening agent are weighed in proportion, is poured in beaker, stirs with glass bar, slant setting 10 ~ 30min, until the bubble collapse in medium;
Sample is vertically put into tubing, and make a long side surface contact of sample on sealing surface, another long side surface outwardly; Dip epoxy resin medium with glass bar, from tube wall instillation pvc pipe, epoxy resin medium wraps sample, until cover sample uniformly by the liquid fluidity of self; Place 3 hours in the drying baker sample inlayed being placed on 50 DEG C, then turn off heating power supply by sample cool to room temperature in drying baker, the obtained sample fixed;
4,800# is adopted successively, 1000#, the SiC sand paper of 1200# and 1500# is polished to section, what polishing adopted is manual water mill, with free-pouring water for medium, polishing is carried out with rinsing simultaneously, before entering next stage sand paper, needs to grind sample until remove the wearing depth that upper level sand paper causes completely;
5, the sample section of having polished is carried out polishing, adopt granularity to be the abrasive pastes of W3.5, on the metallic phase polisher milling of rotary speed 900r/min, the cut of SiC sand paper is removed in polishing; Granularity is adopted to be the abrasive pastes of W1.0 again, polishing 10min on the metallic phase polisher milling of same rotating speed; Finally use clear water polishing 15min on the metallic phase polisher milling of same rotational speed;
6, make mixed solution by after mass concentration 70% nitric acid and ethanol mixing, in mixed solution, the percent by volume of nitric acid is 7%; By with glue head dropper, corrosive liquid is dripped to polished sample surfaces, after corrosion 3s, sample is soaked 5min in acetone soln, and then with the rapid draing of hair-dryer hot blast;
7, the sample corroded is put into high vacuum vapor deposition instrument and plate carbon;
8, adopt field emission electron probe (EPMA) to observe the section of iron scale sample, complete the detection of the scale structure of high-temperature oxydation.
Can see that field emission electron probe (EPMA) backward scattering of this sample section structure detects figure by Fig. 8.
Embodiment 5
1, sample F e-Mn alloy is heated to 1000 DEG C, is incubated after 2 hours with stove cool to room temperature; Adopt wire cutting method on hot-strip, to cut out section, long 8mm, wide 10mm, thickness is 4.5mm, is that cleaning fluid removes surface and oil contaminant with acetone;
2, cut-off footpath is the pvc pipe of 15mm, adopts one section that cutter intercepting 10mm is long;
3, cut one piece of oilpaper, with solid gum, oilpaper is sealed pvc pipe side; The epoxy resin of liquid state and hardening agent are weighed in proportion, is poured in beaker, stirs with glass bar, slant setting 10 ~ 30min, until the bubble collapse in medium;
Sample is vertically put into tubing, and make a long side surface contact of sample on sealing surface, another long side surface outwardly; Dip epoxy resin medium with glass bar, from tube wall instillation pvc pipe, epoxy resin medium wraps sample, until cover sample uniformly by the liquid fluidity of self; Place 4 hours in the drying baker sample inlayed being placed on 50 DEG C, then turn off heating power supply by sample cool to room temperature in drying baker, the obtained sample fixed;
4,800# is adopted successively, 1000#, the SiC sand paper of 1200# and 1500# is polished to section, what polishing adopted is manual water mill, with free-pouring water for medium, polishing is carried out with rinsing simultaneously, before entering next stage sand paper, needs to grind sample until remove the wearing depth that upper level sand paper causes completely;
5, the sample section of having polished is carried out polishing, adopt granularity to be the abrasive pastes of W3.5, on the metallic phase polisher milling of rotary speed 800r/min, the cut of SiC sand paper is removed in polishing; Granularity is adopted to be the abrasive pastes of W1.0 again, polishing 15min on the metallic phase polisher milling of same rotating speed; Finally use clear water polishing 15min on the metallic phase polisher milling of same rotational speed;
6, make mixed solution by after mass concentration 60% nitric acid and ethanol mixing, in mixed solution, the percent by volume of nitric acid is 5%; By with glue head dropper, corrosive liquid is dripped to polished sample surfaces, after corrosion 8s, sample is soaked 5min in acetone soln, and then with the rapid draing of hair-dryer hot blast;
7, adopt field emission electron probe (EPMA) to observe the section of iron scale sample, complete the detection of the scale structure of high-temperature oxydation.
Claims (8)
1. a detection method for hot rolled steel plate surface oxidation iron sheet sample, is characterized in that, comprises the following steps:
(1) sample
One piece of sample is extracted from hot rolled steel plate;
(2) Pipe Cutting
Choose the non-metal pipe that diameter is greater than sample length, intercept one section; Described non-metal pipe is not containing metal ingredient, do not react with epoxy resin, fusing point is higher than the tubing of 50 DEG C;
(3) inlay
By the epoxy resin of liquid state and hardening agent mixing and stirring, slant setting is until bubble collapse in medium;
Seal up tubing side, sample is put into tubing cavity; Then joined by epoxy resin medium in tubing cavity, medium wraps sample, until cover sample completely uniformly by the liquid fluidity of self; Heat in the baking oven again tubing being placed in 40 ~ 50 DEG C, epoxy resin medium is solidified, the obtained sample fixed;
(4) polish
Polish with by the section of sand paper to the sample fixed of low granularity to high granularity successively, the cut of polishing to sample is the granularity of last specification sand paper;
(5) polishing
With abrasive pastes 1, the sample section of having polished is carried out polishing on buffing machine, remove the cut of sand papering; Use abrasive pastes 2 polishing again; Finally with clear water or alcohol polishing, obtain polished hot rolled steel plate surface oxidation iron sheet sample;
(6) chemical corrosion
Corrosive liquid is dripped to polished sample section, after corrosion 3 ~ 10s, sample is immersed in 5 ~ 10min in alcohol or acetone soln, then air-dry or dry up;
(7) microscopic examination
Adopt field emission electron probe to observe the section of iron scale sample, complete detection.
2. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, in described step (3), it is 3 ~ 6 hours that tubing is placed in heating setting time in baking oven.
3. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, the polishing mode described in step (4) is manual water mill, and with free-pouring pure water for medium, polishing is carried out with flushing simultaneously.
4. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, the SiC sand paper being followed successively by 800#, 1000#, 1200# and 1500# by low granularity to the sand paper of high granularity described in step (4).
5. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, the specification of the abrasive pastes 1 described in step (5) is W2.5-3.5; The specification of described abrasive pastes 2 is W0.5-1.5.
6. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, in described step (5), the polishing time of abrasive pastes 2 is 5 ~ 15min; Clear water or alcohol polishing time are 5 ~ 15min.
7. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, it is characterized in that, corrosive liquid described in step (6) is: be make corrosive liquid after the nitric acid of 50-70% and ethanol mixing by mass concentration, in corrosive liquid, the percent by volume of nitric acid is 3-7%.
8. the detection method of a kind of hot rolled steel plate surface oxidation iron sheet sample according to claim 1, is characterized in that, in described step (7), before employing field emission electron probe in detecting, the sample corroded is put into high vacuum vapor deposition instrument and plates carbon.
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| CN113960082A (en) * | 2021-11-08 | 2022-01-21 | 东北大学 | Sample preparation method for hot-rolled strip steel iron scale EBSD analysis |
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