CN101201309A - Method for measuring hot rolling iron scale and oxide phase surface density thereof as well as usage - Google Patents
Method for measuring hot rolling iron scale and oxide phase surface density thereof as well as usage Download PDFInfo
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- CN101201309A CN101201309A CNA200610147265XA CN200610147265A CN101201309A CN 101201309 A CN101201309 A CN 101201309A CN A200610147265X A CNA200610147265X A CN A200610147265XA CN 200610147265 A CN200610147265 A CN 200610147265A CN 101201309 A CN101201309 A CN 101201309A
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Abstract
The invention relates to a method to measure the area density of the hot rolled iron scale surface and a use thereof. The invention is primarily to solve the technical problem that large errors occur when a light microscope or a scanning electron microscope is used to measure the thickness of the iron scale. The method to measure the area density of the hot rolled iron scale and the oxide phase involved comprises the following steps: sampling; pickling; weighing and calculating. In the step of sampling, after a hot rolled plate is rapidly cooled, a small sample is taken by means of line cutting. In the step of pickling, the pickle liquor is HCL with the concentration ranging from 160 g/L to 200g/L, and the pickling temperature ranges from 30 DEG C to 40 DEG C; the iron scale is quickly dissolved in an exfoliation way, and when the iron scale is exfoliated and completely cleaned away, pickling is terminated. In the step of weighing and calculating, the masses of the sample before and after the pickling are measured by using the weight method, and the mass difference is the mass of the iron scale dissolved. The area density of the iron scale is calculated according to the area of the hot rolled iron scale to be measured on the surface to calculate the area density of the iron scale. The average thickness of the hot rolled iron scale can be got according to the area density of the iron scale.
Description
Technical field:
The present invention relates to a kind of method and purposes of measuring the hot rolling iron scale surface density, specifically, it is the mass number that is used to measure the surperficial contained iron scale of hot-rolled steel iron product unit areas such as band steel, wire rod, be surface density, and can also calculate than iron scale average thickness in the large tracts of land scope according to surface density numerical value and known volume density.
Background technology:
The hot-rolled steel iron product is as the band steel, and its surface can generate the iron scale of as-rolled condition in process of production, and the growth mechanism of this iron scale is different from the iron scale of state of nature growth.Generally, the iron scale porosity of state of nature growth is very high, and the oxygen atom diffusion is fully grown soon, and cortex is thick; The iron scale of hot-rolled state, during owing to high temperature, its toughness plasticity is good, and after rolling, cortex is thin and fine and close, and extraneous oxygen atom diffusion is difficult.
By patent and other literature searches, also do not relate to the relevant content of measuring the hot rolling iron scale surface density, some documents are described the thickness of hot-strip scale on surface, its method of measuring iron scale thickness generally is to use optical microscope or scanning electron microscope, this just relates to iron scale sample preparation problem, because the measuring error that sample preparation causes is very big sometimes, how to carry out the comparison of data, this is still disputable.In addition, the measurement of thickness only is the point at limited quantity, its scope is very little, because iron scale and steel matrix interface under the hot-rolled condition are more coarse, and general Ra 1.3～2.5, and it is inhomogeneous, therefore, the thickness measurements representativeness of hot rolling iron scale is relatively poor, can only be that sxemiquantitative is measured, and measure the hot rolling iron scale surface density, be only the method that in than the large tracts of land scope, characterizes steel products scale on surface content more accurately.
" iron and steel " the 38th the 9th phase of volume is introduced: VAI Lin Ci steel mill adopts the picnometer method to determine the pickling time, length consuming time, and the pickling time be difficult to accurately determine that this method also can't provide the information of any relevant electrochemical reaction during less than 20s.Based on the pickling terminal point determining method of oxidation material potential measurement, the result is accurate, and favorable reproducibility helps to understand the electrochemical reaction that takes place in the acid cleaning process.But this method needs corresponding potentiometer, and, if the iron scale pickling is inhomogeneous, still there is the difficult problem of judging of pickling terminal point.
Measure the experimental technique widespread use of the per surface quality (surface density) of steel products overlay coating metal, as GB/T 1839-2003 steel products zinc coating quality test method, this standard code the principle of zinc coating quality test method, testing liquid, sample, step, calculating as a result etc. on the steel products unit area, this has certain reference value to the present invention.But what this method was measured is the quality of steel products surface disparate metals zinc coat, and its dissolving terminal point ratio is easier to control.And iron scale is the complex oxide of steel products surface with metalloid, and the pickling terminal point is difficult to be judged.In addition, measure the hot rolling iron scale surface density and mainly also have following problem:
1, the list of references of relevant hot rolling iron scale quantitative test seldom, organize patent database and dimension Pu Qikanshuojuku to deliver literature search to China, the U.S., Japan, Britain, Germany, France, Switzerland's seven state's patent databases and Europe, the world two, also do not have to find the relevant document introduction of measuring hot rolling iron scale surface density method.
2, acid wash is effective ways of removing iron scale, all contains ferro element in steel matrix and the scale on surface, how to judge accurately that the pickling terminal point is crucial.Pickling terminal point determining method based on the oxidation material potential measurement needs corresponding potentiometer, and, if the iron scale pickling is inhomogeneous, still there is the difficult problem of judging of pickling terminal point.
3, hot rolling iron scale is under the quick gentle slow cool down condition of cooling, and its micromechanism, thing phase composition, performance difference are very big, particularly the slow iron scale under the cooling condition, its adhesiveness is good, under the certain condition, pickling is inhomogeneous, accurately judges pickling terminal point difficulty.Pickling temperature is too high, too low, iron scale pickling reaction velocity too soon, too slow, also can't accurately judge the pickling terminal point, this needs preferred appropriate pickling temperature.
Summary of the invention:
The objective of the invention is: for the scientific research of hot rolling, acid cleaning process, produce the method that the complete mensuration iron scale surface density of a cover is provided, and can also calculate than iron scale average thickness in the large tracts of land scope according to surface density numerical value and known volume density.
The present invention is achieved through the following technical solutions: measure hot rolling iron scale and reach the wherein method of oxide phase surface density, may further comprise the steps:
Sampling: hot rolled plate is got little sample with the line cutting mode after cooling off fast;
Pickling: pickle is the HCL of 160～200g/L concentration, and pickling temperature is 30～40 ℃, peels off mode when iron scale with sheet and dissolves fast, is the pickling terminal point when exfoliated, clean, stops pickling;
Weighing and calculating: use weight method, measure the quality of sample pickling front and back, the quality numerical value that is the iron scale that is dissolved of poor quality according to surface hot rolling iron scale area to be determined, calculates the surface density numerical value of iron scale.
After the iron scale pickling reaches the pickling terminal point, will contain Fe immediately
2+, Fe
3+Acid solution pour in the container that size is fit to and seal, avoid Fe
2+Further oxidation.With measuring iron ions in acidic liquid analysis on Content method, contained Fe in the acid solution after the quantitative measurement test
2+, Fe
3+Molal quantity, calculate FeO, the Fe of " chemical sense " in the iron scale dissolved
2O
3Molal quantity, thereby not only can calculate the iron scale quality numerical value of dissolving, and can provide FeO, the Fe of " chemical sense "
2O
3Component ratio, can the quantitative Analysis hot rolling after fast under the state of cooling, the content and the surface density numerical value thereof of each the oxide phase on the real physical crystallography meaning of hot rolling iron scale.
According to the surface density numerical value ρ that is measured
AWith known volume density ρ
v, can calculate the average thickness d of the iron scale of sampling in the areal extent.
The invention has the beneficial effects as follows: the FeO, the Fe that have defined " chemical sense "
2O
3This notion is to be different from FeO, the Fe on the real physical crystallography meaning
3O
4, Fe
2O
3Thing phase notion is the Fe of 1mol
3O
4Regard the FeO of 1mol and the Fe of 1mol as
2O
3Mixing on chemical sense.Solved problem how to judge iron scale pickling terminal point.
The present invention is by measuring iron scale surface density numerical value, after can the quantitative Analysis hot rolling fast under the state of cooling, the surface density numerical value of each oxide thing phase in the hot rolling iron scale, and can be according to surface density numerical value and known volume density calculation than iron scale average thickness values in the large tracts of land scope.
Hot rolling iron scale surface density numerical representation method the quality control level of hot-rolled steel iron product scale on surface, not only provide important feedback information to hot rolling production, and to iron scale removal technology, the control of particularly widely used pickling production technology has important value.
Description of drawings:
Figure 1 shows that under the condition of fast cooling that iron scale forms the cross section pattern of 2 layers of structure.
Figure 2 shows that under the normal slowly cooling condition, iron scale forms has the pilotaxitic texture cross section pattern of separating out feature mutually.
Figure 3 shows that the HCL acid liquor temperature rolls the comparison of the trend that influences of iron scale pickling time to certain SPHC belt steel surface.
Embodiment:
1, the selection foundation of sampling mode and preferred
In theory, normal hot rolling iron scale is mainly by FeO, Fe
3O
4, Fe
2O
3Three kinds of oxide phase compositions, Fe
3O
4Content is higher, Fe
2O
3Content takes second place, and FeO is less.
Experimental studies show in a large number, under quick cooling and normal slow process for cooling condition, and the pilotaxitic texture (normal slow the cooling) that 2 kinds of cross section patterns of iron scale formation as shown in Figure 1 and Figure 2, are respectively 2 layers of structures (cooling fast), separate out mutually.EBSD analyzes and further shows from the crystallography angle, and the iron scale of 2 layers of structure (cooling fast) is mainly by outer Fe
3O
4, internal layer FeO forms the Fe of minute quantity
2O
3Be distributed in Fe
3O
4Interior and the outmost surface of layer, and Fe
2O
3Content and Fe
3O
4Compare and to ignore.
Because the hot rolling iron scale of fast cold-peace slow cooling has visibly different structure, its pickling mechanism is also different.The former is that the sheet stripping type dissolves fast, the poor adhesion of iron scale and matrix, and under low sour temperature, Fe
3O
4Indissoluble, and FeO is easily molten; The latter is the disperse dissolving, and the adhesiveness of iron scale and matrix is good, and under low sour temperature, the pickling dissolving of iron scale is inhomogeneous, accurately judges pickling terminal point difficulty.
A large amount of tests also show, be cooled to the room temperature process from about 700 ℃ of high temperature, no matter cold soon, still be under low oxygen partial pressure environment, slowly cool off, thickening of hot rolling iron scale is very little, and the band steel oxidation iron sheet of rolled state particularly is because the densification of outer oxide iron sheet, extraneous oxygen atom is difficult more to internal divergence, and thickening almost of iron scale stops.Therefore, on the engineering science meaning, hot rolling iron scale is under slow cooling and fast cool condition, and its quality numerical value can be thought of equal value.
According to above-mentioned analysis, select the sampling mode of cooling fast, hot rolling iron scale is carried out acid washing test, pickling is dissolved fast with the sheet stripping type, can realize accurately judging the pickling terminal point, and judge that the pickling terminal point does not need the potentiometer aid identification, thereby make operation, the control ratio of test be easier to grasp.In time take out sample and carry out rinsing, oven dry, can ignore the dissolving of acid solution matrix.With the hot-strip is example; curling back 30～60 minutes in; the coil of strip afterbody is taken a sample; in the time of can both obtaining to have 2 layers of structure, pickling with the rapidly-soluble hot rolling iron scale of sheet stripping type; compare with the normal slowly type of cooling of actual coil of strip; hot rolling iron scale quality numerical value is equivalent under 2 kinds of cooling conditions, but the test that difference produced of sampling mode control effect is then completely different.
Need explanation especially, the fast cold and hot iron scale that rolls can not be used the line cutting mode and get little sample with the sampling of shear method, because, the iron scale fragility of this state is big, and limit portion iron scale causes fragmentation easily or peels off, and influences the homogeneity of follow-up pickling and the accuracy of mensuration.
2, pickling temperature is preferred
Pickling temperature is one of the key factor that influences the pickling course of dissolution of hot rolling iron scale.Fig. 3 has compared the HCL acid liquor temperature rolls the iron scale pickling time to certain SPHC belt steel surface the trend that influences.As can be seen from the figure, improve acid liquor temperature, rolling the iron scale pickling time sharply reduces, and concerning acid washing test, the pickling terminal point is difficult to control; When acid liquor temperature was low, acid accumulator penetration was slow, and it is long to roll the iron scale pickling time, and concerning acid washing test, the pickling terminal point also is difficult to assurance.
Test shows, the HCL acid solution of 160～200g/L concentration, preferred acid liquid temp are in the time of 30～40 ℃, and the hot rolling iron scale that quick cooling is taken a sample carries out acid washing test, realize the accurate control of pickling terminal point easily, this is with regard to the further problem how to judge iron scale pickling terminal point that solved.
3, solve the upper and lower scale on surface pickling of the band steel problem in asynchronism(-nization) step
Concerning hot-strip, also there is the problem in upper and lower scale on surface pickling asynchronism(-nization) step sometimes, by the method for covering,, will not need the surface and the cross section of pickling to cover processing as using acid-resistant paint, oil paint etc.
4, weight method is measured the quality numerical value and the surface density of iron scale
Produce the known sample of surface area, use weight method, measure the quality of sample pickling front and back, the quality numerical value that is the iron scale that is dissolved of poor quality before and after the sample pickling according to the area of pickled surface, calculates the surface density ρ of iron scale
A
5, calculate the surface density of each oxide phase in the iron scale
As previously mentioned, be different from FeO, Fe on the physics crystallography meaning
3O
4, Fe
2O
3Thing phase notion is the Fe of 1mol
3O
4Regard the FeO of 1mol and the Fe of 1mol as
2O
3Mixing on chemical sense.
After the iron scale pickling reaches the pickling terminal point, will contain Fe immediately
2+, Fe
3+Acid solution pour in the container that size is fit to and seal, avoid Fe
2+Further oxidation.With measuring iron ions in acidic liquid analysis on Content method, the Fe in the acid solution after the quantitative measurement test
2+, Fe
3+Molal quantity, calculate FeO, the Fe of " on the chemical sense " in the iron scale dissolved
2O
3Molal quantity, thereby not only can calculate the iron scale quality numerical value of dissolving, and can calculate FeO, Fe on the chemical sense
2O
3Component ratio, can the quantitative Analysis hot rolling after fast under the state of cooling, FeO, Fe in the hot rolling iron scale
3O
4, Fe
2O
3The actual content of thing phase, wherein Fe
2O
3The thing phase content is few, can ignore or can be regarded as Fe
3O
4The component of thing phase further can be calculated FeO, Fe in the hot rolling iron scale under this state
3O
4Surface density ρ
AFeO, ρ
AFe3O4Numerical value.
6, calculate the average thickness of the iron scale in the sampling areal extent
According to the surface density numerical value ρ that is measured
AWith known volume density ρ
v, can calculate the average thickness d of the iron scale of sampling in the areal extent.
Further specify the present invention below in conjunction with example:
Sample is the hot-strip that cools off fast, and non-acid wash topical oil coating covers processing, is of a size of to be generally 30mm * 20mm * δ (thickness), and surface hot rolling iron scale area (single face) to be determined is A; After sample cleaning, the drying, measure the preceding mass M of sample pickling
1(g).
The HCL acid solution of 180g/L concentration, the preferred acid liquid temp is 35 ± 1 ℃, pickling T.T. 50 ~ 60s, iron scale is peeled off mode with sheet and is dissolved fast, exfoliated, clean only about 10s of time, and the pickling terminal point is controlled easily, during the pickling terminal point, stop pickling fast, after sample rinsing, cleaning, drying, the mass M after the pickling of mensuration sample
2(g).
Calculate quality numerical value M, the surface density ρ of the iron scale that is dissolved
AFor:
ρ
A＝M/A＝(M
1-M
2)/A
Fe in the acid solution of assay test back
2+, Fe
3+Molal quantity be: N
Fe2+, N
Fe3+Iron scale pickling soluble chemistry reaction equation is as follows:
Fe
3O
4(Fe
2O
3+FeO)+8HCL＝2FeCL
3+FeCL
2+4H
2O (1)
FeO+2HCL＝FeCL
2+H
2O (2)
Fe
3O
4, Fe
2O
3, FeO molal weight be respectively 232g/mol, 160g/mol, 72g/mol, according to above-mentioned chemical equation (1), (2), can calculate:
In the iron scale that is dissolved, the FeO on the chemical sense, Fe
2O
3The component mol ratio is:
N
Fe2+∶0.5×N
Fe3+
Can measure iron scale mass M (FeO on the chemical sense, the Fe that is dissolved with above-mentioned weight method
2O
3), also can be according to Fe
2+, Fe
3+Molal quantity N
Fe2+, N
Fe3+Be calculated as follows:
M＝72g/mol×N
Fe2++160g/mol×0.5×N
Fe3+＝72N
Fe2++80N
Fe3+
In the iron scale that is dissolved, actual contained Fe
3O
4, FeO quality be respectively:
MF
e3O4＝232g/mol×0.5×N
Fe3+＝116N
Fe3+
M
FeO＝72g/mol×(N
Fe2+-0.5×N
Fe3+)＝72N
Fe2+-36N
Fe3+
FeO in iron scale and the iron scale, Fe
3O
4Surface density numerical value be respectively:
ρ
A=M/A=(M
1-M
2)/A (weightless weight method)
ρ
A=M/A=(M
1-M
2)/A=72N
Fe2++ 80N
Fe3+(ferric ion determination method)
ρ
AFeO＝M
FeO/A；ρ
AFe3O4＝M
Fe3O4/A
The volume density ρ of hot rolling iron scale
vUnder the known conditions, calculate the average thickness of iron scale:
d＝ρ
A/ρ
v
Claims (4)
1. method of measuring the hot rolling iron scale surface density is characterized in that may further comprise the steps:
Sampling: hot rolled plate is got little sample with the line cutting mode after cooling off fast;
Pickling: pickle is the HCL of 160～200g/L concentration, and pickling temperature is 30～40 ℃, peels off mode when iron scale with sheet and dissolves fast, is the pickling terminal point when exfoliated, clean, stops pickling;
Weighing and calculating: use weight method, measure the quality of sample pickling front and back, the quality numerical value that is the iron scale that is dissolved of poor quality according to surface hot rolling iron scale area to be determined, is calculated as follows the surface density numerical value of iron scale, ρ
A=(M
1-M
2)/A, wherein ρ
ABe the surface density numerical value of iron scale, M
1Be the quality before the sample pickling, M
2Be the quality after the sample pickling, A is a surface hot rolling iron scale area to be determined.
2. the method for mensuration hot rolling iron scale surface density according to claim 1, it is characterized in that the iron scale pickling reaches the pickling terminal point after, will contain Fe immediately
2+, Fe
3+Acid solution pour in the container that size is fit to and seal, with measuring iron ions in acidic liquid analysis on Content method, contained Fe in the acid solution after the quantitative measurement test
2+, Fe
3+Molal quantity, and then obtain Fe
3O
4, FeO quality, be calculated as follows Fe
3O
4, FeO surface density numerical value, ρ
AFe3O4=M
Fe3O4/ A, ρ
AFeO=M
FeO/ A is ρ wherein
AFe3O4Be Fe
3O
4Surface density numerical value, M
Fe3O4Be Fe
3O
4Quality, ρ
AfeOBe the surface density numerical value of FeO, M
FeOBe the quality of FeO, A is a surface hot rolling iron scale area to be determined.
3. the method for mensuration hot rolling iron scale surface density according to claim 1 is characterized in that by the method for covering, and uses acid-resistant paint or oil paint, will not need the surface and the cross section of pickling to cover processing.
4. the method for the described mensuration hot rolling iron scale of claim 1 surface density is used to measure the purposes of the average thickness of iron scale.
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|---|---|---|---|
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| CN101879530A (en) * | 2010-06-25 | 2010-11-10 | 东北大学 | Soft measurement method of thickness of scale on surface of hot continuous rolling strip steel |
| CN101509894B (en) * | 2009-03-23 | 2012-06-27 | 首钢总公司 | Method for measuring scale element distribution in thickness direction |
| CN103447311A (en) * | 2013-09-12 | 2013-12-18 | 江绍成 | Method for controlling the size of hot ring rolling product based on online weighing |
| CN105628607A (en) * | 2015-12-29 | 2016-06-01 | 首钢总公司 | Oxide scale binding force representation method |
| CN109115668A (en) * | 2018-09-26 | 2019-01-01 | 首钢集团有限公司 | A method of test hot rolled steel plate surface oxidation iron sheet porosity |
| CN109163788A (en) * | 2018-08-29 | 2019-01-08 | 日照钢铁控股集团有限公司 | Exempt from phosphating roll bending dry film weight detection method |
| CN109283132A (en) * | 2018-11-06 | 2019-01-29 | 首钢集团有限公司 | A kind of experimental method measuring iron scale binding force |
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| CN112085727A (en) * | 2020-09-17 | 2020-12-15 | 东北大学 | Intelligent identification method for scale structure on surface of hot rolled steel |
| CN112394001A (en) * | 2020-10-27 | 2021-02-23 | 中国石油天然气集团有限公司 | Method and system for detecting and evaluating oxide skin of petroleum steel pipe |
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|---|---|---|---|---|
| CN101509894B (en) * | 2009-03-23 | 2012-06-27 | 首钢总公司 | Method for measuring scale element distribution in thickness direction |
| CN101879530A (en) * | 2010-06-25 | 2010-11-10 | 东北大学 | Soft measurement method of thickness of scale on surface of hot continuous rolling strip steel |
| CN101879530B (en) * | 2010-06-25 | 2013-03-13 | 东北大学 | Soft measurement method of thickness of scale on surface of hot continuous rolling strip steel |
| CN103447311A (en) * | 2013-09-12 | 2013-12-18 | 江绍成 | Method for controlling the size of hot ring rolling product based on online weighing |
| CN105628607A (en) * | 2015-12-29 | 2016-06-01 | 首钢总公司 | Oxide scale binding force representation method |
| CN109163788A (en) * | 2018-08-29 | 2019-01-08 | 日照钢铁控股集团有限公司 | Exempt from phosphating roll bending dry film weight detection method |
| CN109115668A (en) * | 2018-09-26 | 2019-01-01 | 首钢集团有限公司 | A method of test hot rolled steel plate surface oxidation iron sheet porosity |
| CN109283132B (en) * | 2018-11-06 | 2021-06-15 | 首钢集团有限公司 | Experimental method for measuring binding force of iron scale |
| CN109283132A (en) * | 2018-11-06 | 2019-01-29 | 首钢集团有限公司 | A kind of experimental method measuring iron scale binding force |
| CN110082492A (en) * | 2019-04-25 | 2019-08-02 | 宣化钢铁集团有限责任公司 | Wire rod iron scale mechanical stripping performance test methods |
| CN112085727A (en) * | 2020-09-17 | 2020-12-15 | 东北大学 | Intelligent identification method for scale structure on surface of hot rolled steel |
| CN112085727B (en) * | 2020-09-17 | 2023-07-11 | 东北大学 | Intelligent identification method for oxide scale structure on surface of hot rolled steel |
| CN112394001A (en) * | 2020-10-27 | 2021-02-23 | 中国石油天然气集团有限公司 | Method and system for detecting and evaluating oxide skin of petroleum steel pipe |
| CN112630130A (en) * | 2020-11-04 | 2021-04-09 | 江苏省沙钢钢铁研究院有限公司 | Method for detecting iron oxide on surface of hot-rolled wire rod |
| CN116377448A (en) * | 2023-03-10 | 2023-07-04 | 华中科技大学 | Automatic pickling device and method for surface oxide layer of precision investment casting |
| CN116377448B (en) * | 2023-03-10 | 2023-12-19 | 华中科技大学 | Automatic pickling device and method for surface oxide layer of precision investment casting |
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