CN109283132B - Experimental method for measuring binding force of iron scale - Google Patents

Experimental method for measuring binding force of iron scale Download PDF

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CN109283132B
CN109283132B CN201811311151.3A CN201811311151A CN109283132B CN 109283132 B CN109283132 B CN 109283132B CN 201811311151 A CN201811311151 A CN 201811311151A CN 109283132 B CN109283132 B CN 109283132B
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CN109283132A (en
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许斐范
杨建炜
刘立伟
曹建平
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Shougang Corp
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating

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Abstract

The application discloses an experimental method for measuring binding force of iron scale, which comprises the following steps: firstly, processing N hot rolling samples, wherein N is a positive integer greater than or equal to 2; respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel; after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing; preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution; and taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples. The technical effects of simple operation, short measurement period, less external interference factors and high accuracy of experimental results are achieved.

Description

Experimental method for measuring binding force of iron scale
Technical Field
The application relates to the technical field of metal surface coating measurement, in particular to an experimental method for measuring the binding force of iron scale.
Background
During rolling, the iron on the surface of the hot-rolled substrate is in contact with oxygen in the air to form an oxide layer of several to several tens of micrometers, called scale. Technological parameters such as temperature, cooling speed and the like in the rolling process can influence the structure of the iron scale, so that the binding force between the iron scale and a substrate is influenced, but the strength of the binding force of the iron scale influences the generation of defects such as red rust, black ash and the like of a hot-rolled product to a great extent, so that the method for measuring the binding force between the iron scale and the substrate is explored, the qualitative analysis of the binding force of the iron scale is realized, the adjustment and the perfection of the rolling process are facilitated, and the occurrence rate of the defects is reduced.
However, in the process of implementing the technical solution in the embodiment of the present application, the inventor of the present application finds that the above prior art has at least the following technical problems:
in the prior art, the binding force of the iron scale is measured by generally adopting a drawing method and a pixel identification method, and the technical problems of complex and fussy operation, easy interference of external factors and poor reliability exist.
Content of application
The embodiment of the application provides an experimental method for measuring the binding force of the iron scale, and solves the technical problems that the operation is complex, the operation is easily interfered by external factors, and the reliability is poor due to the fact that the binding force of the iron scale is measured by a drawing method and a pixel identification method in the prior art. The technical effects of simple operation, short measurement period, less external interference factors and high accuracy of experimental results are achieved.
In order to solve the above problem, an embodiment of the present application provides an experimental method for measuring a binding force of an iron scale, where the method includes: processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2; respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel; after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing; preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution; taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples; and the complete stripping time of each iron scale of the N hot-rolled samples is used for representing the strength of the bonding force of each iron scale of the N hot-rolled samples and the matrix.
Preferably, the predetermined gauge has a length and width of 20mm by 20 mm.
Preferably, after the concentrated hydrochloric acid and the deionized water are prepared according to a certain proportion to obtain a dilute hydrochloric acid solution, the method further comprises: storing the dilute hydrochloric acid solution into a volumetric flask; and sealing the volumetric flask.
Preferably, the concentration range of the concentrated hydrochloric acid is 36-38%.
Preferably, the preparation ratio of the concentrated hydrochloric acid to the deionized water is 1: 1.
Preferably, the taking of N equal amounts of the dilute hydrochloric acid solution, the acid washing of the N hot-rolled samples respectively, and the recording of the complete peeling time of the iron scales of the N hot-rolled samples specifically include: pouring N parts of the diluted hydrochloric acid solution with the same amount into N beakers respectively; respectively putting the N sealed hot-rolled samples into the N beakers; stirring the N hot-rolled samples in the same direction at a preset stirring speed by using a glass rod, and carrying out acid pickling on the N sealed hot-rolled samples; and recording the complete stripping time of the iron scales of the N hot rolling samples until the iron scales of the N hot rolling samples are completely stripped.
Preferably, the preset stirring speed is 30-60 r/min.
Preferably, the silica gel is 704 silica gel.
One or more technical solutions in the embodiments of the present application have at least one or more of the following technical effects:
the embodiment of the application provides an experimental method for measuring the binding force of iron scale, and the method comprises the following steps: processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2; respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel; after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing; preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution; and taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples. Since the time for complete flaking of each of the scales of the N hot-rolled samples depends on the FeO content of the innermost layer of the scales of the N hot-rolled samples, whereas the FeO content of the innermost layer of the scales of the N hot-rolled samples is used to characterize the strength of the bonding force of each of the scales of the N hot-rolled samples to the substrate, the strength of the bonding force to the substrate can be obtained from the time for complete flaking of the scales of the hot-rolled samples. Therefore, the technical problems that the operation is complex and tedious, the interference of external factors is easy to occur and the reliability is poor due to the fact that the binding force of the iron scale is measured by a drawing method and a pixel identification method commonly adopted in the prior art are solved. The technical effects of simple operation, short measurement period, less external interference factors and high accuracy of experimental results are achieved.
The foregoing description is only an overview of the technical solutions of the present application, and the present application can be implemented according to the content of the description in order to make the technical means of the present application more clearly understood, and the following detailed description of the present application is given in order to make the above and other objects, features, and advantages of the present application more clearly understandable.
Drawings
Fig. 1 is a schematic flow chart of an experimental method for measuring binding force of iron scale provided in an embodiment of the present application.
Detailed Description
The embodiment of the application provides an experimental method for measuring the binding force of iron scales, and solves the technical problems that the binding force of the iron scales is measured by a drawing method and a pixel identification method commonly adopted in the prior art, the operation is complex, the interference of external factors is easy to occur, and the reliability is poor.
In order to solve the technical problems, the technical scheme provided by the application has the following general idea: processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2; respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel; after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing; preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution; and taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples. Since the time for complete flaking of each of the scales of the N hot-rolled samples depends on the FeO content of the innermost layer of the scales of the N hot-rolled samples, whereas the FeO content of the innermost layer of the scales of the N hot-rolled samples is used to characterize the strength of the bonding force of each of the scales of the N hot-rolled samples to the substrate, the strength of the bonding force to the substrate can be obtained from the time for complete flaking of the scales of the hot-rolled samples. Therefore, the technical problems that the operation is complex and tedious, the interference of external factors is easy to occur and the reliability is poor due to the fact that the binding force of the iron scale is measured by a drawing method and a pixel identification method commonly adopted in the prior art are solved. The technical effects of simple operation, short measurement period, less external interference factors and high accuracy of experimental results are achieved.
The technical solutions of the present application are described in detail below with reference to the drawings and specific embodiments, and it should be understood that the specific features in the embodiments and examples of the present application are detailed descriptions of the technical solutions of the present application, and are not limitations of the technical solutions of the present application, and the technical features in the embodiments and examples of the present application may be combined with each other without conflict.
Example one
Fig. 1 is a schematic flow chart of an experimental method for measuring binding force of iron scale in an embodiment of the present invention, as shown in fig. 1, the method includes:
step 110: processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2;
step 120: respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel;
step 130: after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing;
further, the length and width of the predetermined specification is 20mm by 20 mm; the silica gel is 704 silica gel.
Specifically, firstly, processing N hot-rolled samples according to the size of 20mm by 20mm in length and width, wherein N is a positive integer greater than or equal to 2 and is respectively marked as 1#, 2#, 3#, etc., and it is noted that when the N hot-rolled samples are processed, scratches, stabbing and the like on the iron scales of the N hot-rolled samples are avoided, so that the iron scales of one or a plurality of the hot-rolled samples are peeled off, and the accuracy of the final experimental result is affected; respectively horizontally placing the processed N hot-rolled samples on respective smooth weighing paper, and sealing exposed parts of the processed N hot-rolled samples by using 704 silica gel, namely performing edge sealing treatment on four side surfaces and upper surfaces of the processed N hot-rolled samples by using 704 silica gel, and taking protection measures to prevent the four side surfaces and the upper surfaces of the N hot-rolled samples from generating chemical reactions with a dilute hydrochloric acid solution; after the silica gel is completely solidified, lightly removing the weighing paper of each of the N hot rolled samples to expose the surfaces of the N iron scales, wherein the length and the width of the N iron scales are 20mm by 20mm, so that the N hot rolled samples are ensured to be carried out on the premise of having the same area of the iron scales, the comparability of an experimental result is ensured, and then the N hot rolled samples are fixed by perforating the silica gel by using a fish wire, so that the N hot rolled samples are conveniently lifted in the experimental process, and the operation is convenient.
Step 140: preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution;
further, after preparing concentrated hydrochloric acid and deionized water according to a certain ratio to obtain a dilute hydrochloric acid solution, the method further comprises: storing the dilute hydrochloric acid solution into a volumetric flask; and sealing the volumetric flask.
Further, the concentration range of the concentrated hydrochloric acid is 36% -38%; the preparation ratio of the concentrated hydrochloric acid to the deionized water is 1: 1.
Specifically, the concentrated hydrochloric acid with the concentration range of 36% -38% and the deionized water are prepared according to the volume ratio of 1:1, the concentrated hydrochloric acid is diluted to a certain degree, the concentrated hydrochloric acid is poured into a volumetric flask after being sufficiently and uniformly shaken to obtain a certain amount of dilute hydrochloric acid solution, and the volumetric flask containing the dilute hydrochloric acid solution is sealed, so that the technical effect of avoiding the volatilization of the dilute hydrochloric acid solution is achieved.
Step 150: taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples; and the complete stripping time of each iron scale of the N hot-rolled samples is used for representing the strength of the bonding force of each iron scale of the N hot-rolled samples and the matrix.
Further, the step of taking N equal amounts of the dilute hydrochloric acid solution, respectively performing acid washing on the N hot-rolled samples, and recording the complete peeling time of the iron scales of the N hot-rolled samples includes: pouring N parts of the diluted hydrochloric acid solution with the same amount into N beakers respectively; respectively putting the N sealed hot-rolled samples into the N beakers; stirring the N hot-rolled samples in the same direction at a preset stirring speed by using a glass rod, and carrying out acid pickling on the N sealed hot-rolled samples; and recording the complete stripping time of the iron scales of the N hot rolling samples until the iron scales of the N hot rolling samples are completely stripped.
Further, the preset stirring speed is 30-60 r/min.
Specifically, N equal amounts of the dilute hydrochloric acid solution are taken from the volumetric flask, in the embodiment of the present application, N80 ml portions of the dilute hydrochloric acid solution are respectively poured into N beakers, then the N sealed hot rolled samples are respectively placed into the N beakers, then a glass rod is used to stir in the same direction at a stirring speed of 30 to 60r/min, and the N sealed hot rolled samples are subjected to acid washing, that is, the surfaces of iron scales of the N sealed hot rolled samples are subjected to acid washing, where it is noted that each 80ml portion of the dilute hydrochloric acid solution can only be used for acid washing one hot rolled sample, and a new dilute hydrochloric acid solution needs to be replaced during a second experiment, so that the N hot rolled samples and the dilute hydrochloric acid solution with equal amounts and equal concentrations are ensured to perform chemical reaction. The iron scale comprises the following components: the outermost layer is Fe2O3The middle layer is Fe3O4The innermost layer is FeO, and the iron scale is exposed to the dilute hydrochloric acid solutionIn the solution, the phenomena of reddening of the dilute hydrochloric acid solution, bubbling, scale peeling and the like occur in sequence. Wherein the red color in the dilute hydrochloric acid solution is due to Fe in the outermost layer of the scale2O3Dissolving and diffusing into the dilute hydrochloric acid solution, wherein Fe simple substance generated by the scale eutectoid reaction is very rarely insufficient to react with hydrochloric acid to generate bubbles, the bubbles appear to indicate that the dilute hydrochloric acid solution has penetrated into the matrix of the hot-rolled sample, the scale stripping indicates that FeO in the innermost layer is being dissolved until the scales of the N hot-rolled samples are completely stripped, and the complete stripping time of the scales of the N hot-rolled samples is recorded. Since the time for complete flaking of the scales of the N hot-rolled samples mainly depends on the FeO content of the innermost scale layer of each of the N hot-rolled samples, which in turn is used to characterize the strength of the bonding force of each of the scales of the N hot-rolled samples to the substrate, the strength of the bonding force of the scales of the N hot-rolled samples to the substrate can be obtained from the time for complete flaking of the scales of the N hot-rolled samples. If the content of FeO in the innermost layer of the scale is higher, the scale is easier to be pickled, and the time for completely peeling the scale of the hot-rolled sample is shorter, the bonding force between the scale and the matrix of the hot-rolled sample is weaker. Comparing the complete stripping time of the oxide scales of the N hot-rolled samples, wherein if the complete stripping time of the oxide scales of which hot-rolled sample is the shortest, the FeO content of the oxide scales of the hot-rolled samples is the highest and is most easily dissolved, so that the bonding force between the oxide scales of the hot-rolled samples and a substrate is the weakest; if the time for completely stripping the iron scale of the hot rolled sample is the longest, the FeO content of the iron scale of the hot rolled sample is the lowest and is most difficult to dissolve, and the bonding force between the iron scale of the hot rolled sample and a substrate is the strongest, so that the qualitative analysis of the bonding force between the iron scale and the substrate is realized, the adjustment and the perfection of a rolling process are facilitated, and the occurrence rate of defects of a hot rolled product is reduced. Further achieves the purposes of simple operation, short measurement period, less external interference factors and experimental resultHigh accuracy.
One or more technical solutions in the embodiments of the present application have at least one or more of the following technical effects:
the embodiment of the application provides an experimental method for measuring the binding force of iron scale, and the method comprises the following steps: processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2; respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel; after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing; preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution; and taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples. Since the time for complete flaking of each of the scales of the N hot-rolled samples depends on the FeO content of the innermost layer of the scales of the N hot-rolled samples, whereas the FeO content of the innermost layer of the scales of the N hot-rolled samples is used to characterize the strength of the bonding force of each of the scales of the N hot-rolled samples to the substrate, the strength of the bonding force to the substrate can be obtained from the time for complete flaking of the scales of the hot-rolled samples. Therefore, the technical problems that the operation is complex and tedious, the interference of external factors is easy to occur and the reliability is poor due to the fact that the binding force of the iron scale is measured by a drawing method and a pixel identification method commonly adopted in the prior art are solved. The technical effects of simple operation, short measurement period, less external interference factors and high accuracy of experimental results are achieved.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made in the embodiments of the present invention without departing from the spirit or scope of the embodiments of the invention. Thus, if such modifications and variations of the embodiments of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to encompass such modifications and variations.

Claims (7)

1. An experimental method for measuring the binding force of iron scale is characterized by comprising the following steps:
processing N hot rolling samples according to a preset specification, wherein N is a positive integer greater than or equal to 2;
respectively placing the processed N hot-rolled samples on respective weighing paper, and sealing the exposed parts of the processed N hot-rolled samples by using silica gel;
after the silica gel is solidified, removing the weighing paper of each of the N hot-rolled samples, exposing the surfaces of the N iron scales, and perforating holes on the silica gel by using fish lines for fixing;
preparing concentrated hydrochloric acid and deionized water according to a certain proportion to obtain a dilute hydrochloric acid solution;
taking N parts of the diluted hydrochloric acid solution with the same amount, respectively carrying out acid washing on the N hot-rolled samples, and recording the complete stripping time of the iron scales of the N hot-rolled samples; wherein, the complete stripping time of each scale of the N hot-rolled samples is used for representing the strength of the bonding force of each scale of the N hot-rolled samples and a matrix;
the method comprises the following steps of taking N parts of dilute hydrochloric acid solution with the same quantity, respectively carrying out acid washing on N hot-rolled samples, and recording the complete stripping time of iron scales of the N hot-rolled samples, and specifically comprises the following steps:
pouring N parts of the diluted hydrochloric acid solution with the same amount into N beakers respectively;
respectively putting the N sealed hot-rolled samples into the N beakers;
stirring the N hot-rolled samples in the same direction at a preset stirring speed by using a glass rod, and carrying out acid pickling on the N sealed hot-rolled samples;
and recording the complete stripping time of the iron scales of the N hot rolling samples until the iron scales of the N hot rolling samples are completely stripped.
2. The method of claim 1, wherein the predetermined gauge length and width are 20mm by 20 mm.
3. The method of claim 1, wherein after the preparing the concentrated hydrochloric acid and the deionized water according to a certain ratio to obtain the dilute hydrochloric acid solution, the method further comprises:
storing the dilute hydrochloric acid solution into a volumetric flask;
and sealing the volumetric flask.
4. The method according to claim 3, wherein the concentration of the concentrated hydrochloric acid is in the range of 36% to 38%.
5. The method of claim 3, wherein the concentrated hydrochloric acid and the deionized water are formulated at a ratio of 1: 1.
6. The method according to claim 1, wherein the preset stirring rate is 30 to 60 r/min.
7. The method of claim 1, wherein the silica gel is 704 silica gel.
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CN111157448A (en) * 2020-01-06 2020-05-15 北京科技大学 Novel method for quantitatively characterizing binding force of iron scale and steel matrix

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CN203216830U (en) * 2013-02-28 2013-09-25 首钢总公司 Measuring device for adhesion force of oxide scale
CN104713759A (en) * 2015-02-13 2015-06-17 东北大学 Method for detecting surface oxidized scale sample of hot rolled steel plate
CN105628607A (en) * 2015-12-29 2016-06-01 首钢总公司 Oxide scale binding force representation method
CN107705285A (en) * 2017-07-21 2018-02-16 首钢集团有限公司 A kind of characterizing method of surface of steel plate iron scale adhesion

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CN101201309A (en) * 2006-12-14 2008-06-18 上海梅山钢铁股份有限公司 Method for measuring hot rolling iron scale and oxide phase surface density thereof as well as usage
JP2011158328A (en) * 2010-01-29 2011-08-18 Nippon Steel Corp Oxide coating film adhesion strength evaluation method and its evaluation device of directional electromagnetic steel plate
CN203216830U (en) * 2013-02-28 2013-09-25 首钢总公司 Measuring device for adhesion force of oxide scale
CN104713759A (en) * 2015-02-13 2015-06-17 东北大学 Method for detecting surface oxidized scale sample of hot rolled steel plate
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