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    • 专利摘要:
    ELECTRIC STEEL SHEETS NOT ORIENTED AND A METHOD OF MANUFACTURING THE SAME. The present invention relates to a non-oriented electric steel plate that includes: a base iron (1); and a tension-insulating film (2) of not less than 1 g / m2 and not more than 6 g / m2 on a base iron surface (1). An oxide layer (3) containing at least one type of oxide selected from the group consisting of Si, AI, and Cr having a thickness of not less than 0.01 µm and not more than 0.5 µm formed on the surface of base iron (1).
    公开号:BR112012020219B1
    申请号:R112012020219-7
    申请日:2011-02-15
    公开日:2020-12-01
    发明作者:Takeshi Kubota；Yousuke Kurosaki；Masahiro Fujikura；Takahide Shimazu；Shuichi Yamazaki
    申请人:Nippon Steel Corporation；
    IPC主号:
    专利说明:

    TECHNOLOGICAL FIELD
    [001] The present invention relates to a steel plate not oriented for electrical purposes, suitable for use as an engine's iron core material and a method of manufacturing it. CONTEXT OF THE INVENTION
    [002] It has been very desirable to manufacture a more efficient electrical appliance and obtaining less loss in the core is necessary for an unoriented electric steel plate used as the iron core material of an engine contained in an appliance electric. Then, we studied a technique of using Si, Al, and others in an electric steel plate not oriented to increase the resistivity and increase the diameter of the grains, a technique of adjusting the annealing of the hot rolled plate and a cold rolling ratio and consequently improve the texture and so on.
    [003] In addition, a non-oriented electric steel sheet is an electric steel sheet with random crystals orientations in a direction parallel to its surface, but depending on the use of a non-oriented electric steel sheet, there is still sometimes a case of a magnetic property in a direction parallel to its surface, for example, a lamination direction better than that in the other direction is preferable. For example, in the case when a split core is used as a motor stator, the electric steel sheet as described above is preferably used for the split core. As an electric steel sheet with a better magnetic property in the direction of the rolling, a grain-oriented electric steel sheet is also considered, but a glass-coated film exists on the surfaces of the grain-oriented electric steel sheet, so that drilling is difficult to do. Thus, when compared to non-oriented electric steel sheet, more controls are needed for the manufacture of oriented grain electric steel sheets and the electric grain oriented steel sheet is of higher cost. By the way, if the split core is used as a motor stator, the magnetization direction of the electric steel plate is allowed to agree with the direction in which the magnetic flux flows, and therefore the motor efficiency can be enhanced. Thus, it is possible to improve the production of the electric steel sheet as a material and increase the winding filling factor.
    [004] Several proposals have been made regarding electric steel sheets not oriented towards a split core. However, in conventional techniques, it is difficult to obtain sufficient magnetic property in the lamination direction. LIST OF CITATIONS PATENT LITERATURE Patent Literature 1: Patent Publication Open to Japanese Public Inspection No. 2004-332042 Patent Literature 2: Patent Publication Open to Japanese Public Inspection No. 2006-265720 Patent Literature 3: Patent Publication Open to Japanese Public Inspection No. 2008-260996 Patent Literature 4: Patent Publication Open to Japanese Public Inspection No. 56-55574 Patent Literature 5: Patent Publication Open to Japanese Public Inspection No. 2001-140018 Patent Literature 6: Japanese Patent Publication No. 2001-279400 SUMMARY OF THE INVENTION TECHNICAL PROBLEM
    [005] The present invention aims to provide a non-oriented electric steel plate capable of obtaining a better magnetic property in the direction of the rolling and a method of manufacturing it. SOLUTION OF THE PROBLEM
    [006] The inventors focused on the technique disclosed in the Patent Application 4 and believed that when using an insulation film of the type of traction application as an insulating material formed on the surfaces of a base iron of an unoriented electric steel plate, it may be possible to improve the magnetic property in the lamination direction, and several experiments have been conducted. However, it has been found that insulation film of the type of tensile application is normally used, the insulation film cannot withstand sufficiently various procedures (drilling, interlocking, and so on) to form a split core. In other words, peeling of the insulation film and the like sometimes occurs. Further, the magnetic property in the lamination direction was improved, but the improvement was not sufficient. The inventors conducted a rigorous study in order to examine these causes, and then found that the adhesion between the insulating film of the type of application of traction and base iron is low, and that due to this, insufficient traction acts on the base iron. The traction that acts on the base iron is not enough. Thus, the inventors conducted a careful knowledge-based study, and then found that a case of a specific resistant oxide layer on the base iron surfaces, the oxide layer contributes to improving the adhesion between the base iron and the film. traction-type insulation, and the magnetic property of the rolling direction is significantly improved. Furthermore, it was also found that with improved adherence, the peeling of the insulating or similar film is suppressed.
    [007] The essence of the present invention is presented below. (1) A non-oriented electric steel plate including: a base iron, an oxide layer containing at least one type of oxide selected from the group consisting of Si, Al, and Cr and with a thickness of not less than 0, 01 pm and no more than 0.5 pm being formed on a base iron surface; and a traction-type insulating film of no less than 1 g / m2 and no more than 6 g / m2 on the base iron surface, where Base iron contains: 51, Al, and Cr: no less than 2% by weight and not more than 6% by weight of the total content; and Mn: not less than 0.1% by weight and not more than 1.5% by weight, A C content of the base iron is equal to or less than 0.005% by weight, and the remainder of the base iron is composed of Fe and unavoidable impurities. (2) The sheet of electric steel not oriented according to (1), in which the total content of Al and Cr of base iron is equal to or more than 0.8% by weight. (3) The electric steel sheet not oriented in accordance with (1) or (2), in which the insulating film is formed by cooking a coating solution containing phosphate and colloidal silica. (4) The electric steel plate not oriented in accordance with (1) or (2), on which the alumina sol. (5) A method of fabricating a non-oriented electric steel plate including:
    [008] Carry out the finishing annealing of a cold rolled steel strip; e Form a traction-type insulating film of not less than 1 g / m2 and more than 6 g / m2 on a surface of the cold-rolled steel strip, on which the cold-rolled steel strip contains: 51, Al, and Cr: not less than 2% by weight or more than 6% by weight in total content; and Mn: not less than 0.1% by mass and not more than 1.5% by mass, A C content of the cold rolled steel strip is equal to or less than 0.005% by mass,
    [009] A remainder of the cold-rolled steel strip is composed of Fe and unavoidable impurities, and the completion of annealing finish includes the formation of an oxide layer containing at least one type of oxide selected from the group consisting of Si and A1 and having a thickness of not less than 0.01 pm and not more than 0.5 pm on the surface of the cold rolled steel strip with the determination of a temperature of the cold rolled steel strip of not less than 800 ° C and not more than 1100 ° C in an atmosphere where the total Si and Al content of the cold rolled steel strip is represented as X (mass%), the ratio of the partial pressure of water vapor to hydrogen is equal a or less than 0.005 x X2. 6.) The method of fabricating an electric steel sheet not oriented in accordance with (5), in which the formation of the insulating film includes, after the completion of the annealing finish: the application of a coating solution to a surface of the cold rolled steel strip; and carrying out the cooking of the coating solution by determining the temperature of the cold rolled steel strip to less than 800 ° C and no more than 1100 ° C. 7.) The method of fabricating an electric steel sheet not oriented in accordance with (5), in which the formation of the insulating film includes: the application of a coating solution to the surface of the cold-rolled steel strip prior to making finishing annealing, and cooking the coating solution during finishing annealing. 8.) The method of manufacturing an electric steel plate not oriented in accordance with (6) or (7), in which the coating solution contains colloidal silica phosphate. 9.) The method of making an electric steel sheet not oriented in accordance with (6) or (7), in which the coating solution contains boric acid and an alumina sol. 10.) The method of manufacturing an electric steel sheet not oriented in accordance with any of items (5) to (9), in which the total content of Al and Cr of the cold rolled steel strip is equal to or greater than 0.8% by mass. ADVANTAGE EFFECTS OF THE INVENTION
    [0010] In accordance with the present invention, it is possible to obtain a high adhesion between a base iron and an insulating film applying traction, and significantly increase a magnetic property in a rolling direction. BRIEF DESCRIPTION OF THE DRAWINGS
    [0011] Figure 1A shows a sectional photograph taken by an electronic scanning microscope of a cross-section of an oxide on the surface of a steel strip in which the finishing annealing was carried out in an atmosphere where the pressure ratio partial (PH2O / PH2) is 0.1;
    [0012] figure 1B illustrates a sectional photograph taken by an oxide scanning electronic microscope on the surface of a steel strip in which the finishing annealing was carried out in an atmosphere where the partial pressure ratio (PH2O / PH2) is 0.01;
    [0013] figure 2 is an illustration of the infrared reflection-absorption spectrum of an external oxide film 102;
    [0014] figure 3 is an illustration of the relationship between the composition of a cold-rolled strip of acid and a finishing annealing atmosphere, and a state of a base iron surface;
    [0015] figure 4 is a sectional illustration of an electrical steel sheet structure not oriented in accordance with an embodiment of the present invention;
    [0016] figure 5 is a flowchart illustrating an example of a method for manufacturing a non-oriented electric steel sheet; and
    [0017] figure 6 is a flowchart illustrating another example of the method of manufacturing non-oriented electric steel sheet. DESCRIPTION OF THE MODALITIES
    [0018] Firstly, an experiment regarding the application of a traction insulating film to a non-oriented electric steel plate driven by the motors will be explained.
    [0019] In the experiment, two strips of cold-rolled steel for a non-oriented electric steel sheet each containing Si: 3% by mass, Mn: 0.15% by mass, and Al: 1.2% by mass, and a remainder of Fe and unavoidable impurities and each 0.35 mm thick were fabricated. Then, finish annealing was performed at a temperature of 1000 ° C in a different annealing atmosphere on each cold-rolled steel strip. In one of the annealing atmospheres, the partial pressure ratio of water vapor to hydrogen (PH2O / PH2) was determined to be 0.01, and in the other annealing atmosphere the partial pressure ratio (PH2O / PH2) was determined to be 0.1. Then, a magnetic loss value (W10 / 50) was measured under a 50 Hz frequency excitation condition and the maximum magnetic flux density of 1.0 T in a rolling direction (an L direction) and a perpendicular direction to the rolling direction on a surface of the cold rolled steel strip (a C direction). After that, 3 g / m2 per surface and a coating solution composed of aluminum phosphate, colloidal silica and chromic acid were applied to both surfaces of each of the steel strips to be baked at 800 ° C. That is, the insulating films applied to traction were formed. Then, the magnetic loss value (W10 / 50) was removed again in the L direction and in the C direction. These results are listed in Table 1.Table 1

    [0020] As listed in Table 1, in the case of annealing in the atmosphere of partial pressure ratio (PH2O / PH2) of 0.1, an 8% improvement was confirmed with respect to the magnetic loss in the L direction. However, as if it was desired to form a split core from the electric steel sheet not oriented with the insulation films formed in this way, the insulation films are not able to withstand work such as drilling and interlocking.
    [0021] On the other hand, in the case of annealing in an atmosphere of partial pressure ratio (PH2O / PH2) of 0.01, an improvement of up to 17% was confirmed in relation to the magnetic force in the L direction and still the insulation films were able to withstand work such as drilling and interlocking sufficiently.
    [0022] The inventors observed the cross section of an oxide on the acid strip surface after the annealing finish in order to examine the cause of the difference in the resistance to the work of the insulation films due to the annealing finish in the atmosphere described above. Figure 1A illustrates a sectional photograph by scanning an electron microscope of an oxide on the surface of the steel strip which has been subjected to finish annealing in the atmosphere of partial pressure ratio (PH2O / PH2) of 0.1, and the figure 1B illustrates a sectional photograph by scanning an electron microscope of an oxide on the surface of the steel strip which has been subjected to finish annealing in the atmosphere of partial pressure ratio (PH2O / PH2) of 0.01.
    [0023] As illustrated in figure 1A, on the surface of a base iron 101 of the steel strip subjected to the annealing finish in the atmosphere of partial pressure ratio (PH2O / PH2) of 0.1, there was a thick inner layer 103 of oxide. On the other hand, as illustrated in figure 1B, on the base iron surface 101 on the steel strip subjected to the annealing finish in the atmosphere of partial pressure ratio (PH2O / PH2) of 0.01, there was an external 102 film of oxide with a thickness of 50 nm or more. By the way, an Au 104 deposited layer was formed on the outer oxide film 102 and on the inner oxide layer 103 to protect the outer oxide film 102 and the inner oxide layer 103 when making the samples for observation of the cross section.
    [0024] Further, figure 2 illustrates the reflection-infrared absorption spectrum of the outer film 102 of oxide. From the spectrum illustrated in figure 2, it is possible to confirm that the outer film 102 of oxide is made mainly of Al2O3.
    [0025] Therefore, it was found that in the manufacture of non-oriented electric steel sheets, the external oxide film is formed in the finishing annealing step of the cold-rolled steel strip and thus the pressure-insulating insulating film is formed, and in this way the adhesion between the insulation film and the base iron is significantly increased and also the magnetic property in the L direction is significantly improved. By the way, as will be described later, even in spite of the application of raw material (coating solution) of the insulating film of traction was carried out and then the annealing of finishing was carried out, and thus the formation of the external oxide film and the formation of the insulating film by cooking in the coating solution is carried out in parallel, the improvement of adhesion and the significant improvement of the magnetic property in the L direction are achieved.
    [0026] Here, the annealing condition is important for the formation of the external oxide film during the finishing annealing. Then, the inventors examined the relationship between the composition of the cold rolled steel strip undergoing finish annealing and the atmosphere of the finish annealing, and the state of the surface of the base iron. In the research, several cold-rolled steel strips different in the total content (X (% of mass)) of Si, Al, and Cr were manufactured for those subjected to annealing finish under an atmosphere of various partial pressure ratios (PH2O / PH2). Then, the state of one of the surfaces of each base iron was observed after the finishing re-cooking. By the way, the temperature of the finish annealing was determined to be 900 ° C. The result is illustrated in figure 3. In figure 3 the open mark means that the inner oxide layer was formed, and the closed mark means that the outer oxide layer was formed.
    [0027] From figure 3, it is observed that, as long as the total content (X (% by mass)) of Si, Al, and Cr is under the condition that the partial pressure ratio (PH2O / PH2 ) was less than 0.005 x X2, the external oxide film can be formed.
    [0028] Hereinafter, one embodiment of the present invention will be explained by reference to the attached drawings. Figure 4 is a cross section showing a figure of an electric steel sheet not oriented in accordance with the embodiment of the present invention.
    [0029] As illustrated in figure 4, on the electric steel plate not oriented in accordance with the modality, an insulating film of tension 2 with no less than 1 g / m2 and no more than 6 g / m2 is formed on the base iron surfaces 1. Also, on the base iron surfaces 1, an external oxide film 3 is formed containing at least one type of oxide selected from the group consisting of Si, Al, and Cr and with a thickness of no less than 0.01 pm and not more than 0.5 pm. In a base 1 iron, a base 4 and external oxide films 3 are contained. The external oxide film 3 is an example of an oxide layer.
    [0030] Base iron 1 contains Si, Al, and Cr: not less than 2% by weight and not more than 6% by weight of the total content and Mn: not less than 0.1% by weight and not more than 1.5% by mass. The C content of base iron 1 is 0.005% or less by weight, and the remainder of base iron 1 may be composed of Fe and unavoidable impurities.
    [0031] Then, a method for manufacturing the non-oriented electric steel sheet described above will be explained. Figure 5 is a flowchart illustrating an example of a non-oriented electrical steel sheet manufacturing method.
    [0032] In the modality, first perform the hot rolling of a plate (steel material) with a predetermined composition heated to a predetermined temperature in order to manufacture a hot rolled steel strip (Step S1) . Then, the shells are returned by acid pickling and the hot-rolled steel strip is cold rolled to make a cold-rolled steel strip (Step S2). Like cold rolling, cold rolling can only be done once or cold rolling can also be done twice or more with intermediate annealing being carried out between procedures. Incidentally, annealing can also be carried out as needed before cold rolling.
    [0033] Here, the components contained in the plate (steel material) will be explained.
    [0034] C increases magnetic loss and causes magnetic aging. Thus, the C content is determined to be 0.005% of the dough content or less.
    [0035] Si, Al, and Cr exhibit an effect of increasing the resistance of the electric steel plate not oriented to reduce the loss of eddy current. Thus, Si, Al, and Cr are used to form the external oxide film 3, the details of which will be described later. If the total content of Si, Al, and Cr are less than 2% by mass, the effect cannot be achieved sufficiently. Therefore, the total content of Si, Al, and Cr is determined at 2 mass% or more. If the total Si, Al, and Cr content exceeds 6% by mass, cold work such as cold rolling is difficult to do. Thus, the total content of Si, Al, and Cr is determined to be 6 mass% or less.
    [0036] Mn exhibits the effect of reducing the solid solution S when the plate is heated. If the Mn content is less than 0.1% by mass, the effect cannot be achieved sufficiently. Thus, the Mn content is determined to be 0.1% by weight or more. On the other hand, if the Mn content exceeds 1.5% by mass, the magnetic property deteriorates. Therefore, the Mn content is determined to be 1.5% by weight or less.
    [0037] By the way, the content of unavoidable impurities such as S, N, and O, and Ti, V, Zr, and Nb with the potential to bond to S, N, and O to form non-magnetic inclusions can be reduced as much as possible. In addition, rare earth elements, Ca, and so on can also be present for the purpose of avoiding S, N, and O. The preferable content of rare earth elements, Ca, and so on is not less than 0.002% and not greater than 0.01% by mass.
    [0038] Sn and Sb have the effect of improving the property in the L direction by improving the texture. When adding Sn and Sb, the synergistic effect with the effect of the present invention can be expected.
    [0039] After cold rolling (Step S2), the annealing of the cold rolled steel strip is carried out in a pre-determined atmosphere to manufacture the base iron 1 with the external oxide film 3 on the surfaces (Step S3). In finishing annealing, the temperature of the cold rolled steel strip is determined to be no less than 800 ° C and no more than 1100 ° C. If the temperature is below 800 ° C, it is difficult to form the external oxide 3 films sufficiently. On the other hand, if the temperature exceeds 1100 ° C, the cost is significantly increased, it is difficult to carry out the operation in a stable manner. Further, since the atmosphere of the finish annealing, taking into account the knowledge described above, the partial pressure ratio (PH2O / PH2) of the water vapor to hydrogen is determined in less than 0.005 x X2 in relation to the content total (X (mass%)) of Si, Al, and Cr. As long as the condition is satisfied, the desired outer oxide film can be formed with an oxide layer 3 as described above. The outer layer of oxide 3 contributes to a significant improvement in the adhesion between the traction insulating film and the base iron 1. Then, with the improvement of the adhesion, the traction acts efficiently and the magnetic property in the L direction is further improved. more.
    [0040] By the way, if the thickness of the external oxide film 3 is less than 0.01 pm, it is difficult to obtain sufficient adhesion. Therefore, the thickness of the oxide 3 outer film is desirably equal to or greater than 0.01 pm. Furthermore, even if the thickness of the external oxide film 3 exceeds 0.5 pm, it is difficult to obtain sufficient adhesion. This is because supposedly the outer oxide films 3 are formed in a thick way, there is an unnecessary tension of them on the base surface 4 on the base iron 1. Thus, the thickness of the external oxide film 3 is desirably equal to or less than 0.5 pm. The thickness of the external oxide film 3 must be controlled by adjusting, for example, the temperature of the finish annealing and the soak time. That is, as the soaking temperature increases and the soaking time is longer, the outer oxide 3 films are formed in a thicker manner.
    [0041] The substances containing the external oxide film 3 are terminated according to the content of Si, Al, and Cr, and the main component of the external oxide film 3 can be, for example, SiO2, Al2O3, Cr2O3, and so on. onwards. In the case of the content of Al and Cr in the cold-rolled steel strip, for example, the main component of the external oxide film 3 is SiO2, and if the total content of Al and Cr is equal to or greater than 0.8 % by mass, the main component of the external oxide film 3 is Al2O3 and Cr2O3, or (Al, Cr) 2O3. The main component of the external oxide film 3 is particularly limited. In the case that the main component is Al2O3 and Cr2O3, or (Al, Cr) 2O3, a particularly high adhesion must be obtained. Thus, the total content of Al and Cr is desirably equal to or greater than 0.8% by weight. By the way, the external oxide film 3 is not composed of these main components, and even if Al and Cr are small, sometimes Al2O3, Cr2O3, and so on, and even in the case of the total content of Al or Cr exceeds 0.8% by mass, there may be SiO2.
    [0042] After finishing annealing and the formation of the oxide layer (Step S3), the traction 2 insulating film forms on the surfaces of the base iron 1 (Step S4). In the formation of insulating films 2, the application and cooking of a predetermined coating solution is carried out. Depending on the coating solution, a coating solution used for grain-oriented electric steel plate can be used as the coating solution. For example, a coating solution containing colloidal silica phosphate can be used in its main components. The ratio of phosphate and colloidal silica is not limited in any particular way. The colloidal silica ratio is preferably from 4 mass% to 24 mass%, and the phosphate ratio is preferably from 5 mass% to 30 mass%. Such a coating solution is described, for example, in Japanese Public Inspection Patent Publication No. 48-39338, Japanese Japanese Public Inspection Patent Publication No. 50-79442, and so on. Furthermore, a coating solution containing boric acid and alumina sol as its main components can also be used. The ratio of the aluminum and boron component is not particularly limited. An aluminum oxide and boron equivalent, an aluminum oxide is preferably 50% by weight to 95% by weight. Such a coating solution is described, for example, in Japanese Public Inspection Open Patent Publication No. 06-65754 and Japanese Public Inspection Open Patent Publication No. 06-65755.
    [0043] Furthermore, the amount of formation of the traction application insulating film is determined to be no less than 1 g / m2 and no more than 6 g / m2 on one surface. If the amount of formation of the insulating film 2 is less than 1 g / m2, the traction is not applied sufficiently, thus making it difficult to sufficiently improve the magnetic property in the direction of blade L (direction L). On the other hand, if the amount of insulating film formation 2 exceeds 6 g / m2, the special factor is reduced.
    [0044] Furthermore, the cooking temperature determined at not less than 800 ° C and not more than 1100 ° C. If the cooking temperature is below 800 ° C, the traction is not applied sufficiently, thus making it difficult to sufficiently improve the magnetic property in the lamination direction (L direction). On the other hand, if the cooking temperature exceeds 1100 ° C, the cost is significantly increased and it becomes difficult to carry out the operation in a stable manner.
    [0045] Through a series of processes as described above, it is possible to manufacture an electric steel plate not oriented according to the modality. Then, in the non-oriented electric steel plate, the external oxide film 3 causes the base iron 1 and the insulating traction film 2 to adhere strongly to each other. Therefore, greater traction is applied to further improve the magnetic property in the lamination direction (L direction), and even in the case of varied jobs (drilling, interlocking and so on) to form a divided core and to be performed, the peeling on insulating film 2 or similar can be suppressed.
    [0046] By the way, the manufacturing method, application and cooking of the coating solution to form the coating films 2 (Step S4) are carried out after the annealing finish (Step S3). Cooking can be carried out in parallel with finishing re-cooking. That is, as illustrated in figure 6, it is also possible that after cold rolling (Step S2), the coating solution is applied to the cold rolled steel strip (Step S11), and that the finishing annealing is combined with rewashing the coating solution (Step S12).
    [0047] Furthermore, after the formation of the traction 2 insulating films, a coating film made of only resin and / or a coating film composed of an inorganic substance and resin can also be formed on the insulating films applied - tensile strips 2 in order to improve drilling performance by forming a core such as a split core. That is, the application and cooking of a coating solution normally used for the formation of an insulating film for non-oriented electric steel sheets can be performed, and thus the drilling performance can be improved. As the above coating solution, a coating solution containing chromate and acrylic resin can be used as the above coating solution. For example, a coating solution in which an aqueous solution of chromic acid and metallic acid, a metallic hydroxide and a metallic carbonate are dissolved, and an emulsion-type resin can also be added. Such a coating solution is described in Examined Japanese Patent Application Publication No. 50-15013, for example. In addition, a coating solution containing phosphate and an acrylic resin can also be used. For example, a coating solution can be used in which 1 to 300 parts by mass of an organic resin solution and every 100 parts of phosphate are added. A coating solution like this is described in Japanese Public Inspection Patent Publication No. 06-330338, for example. EXAMPLE
    [0048] Next, the experiments conducted by the inventors will be explained. The conditions in these experiments are employed in an exemplary manner to confirm the possibility and effects of the present invention, and the present invention is not limited to these examples. (First Experiment)
    [0049] First, steel plates (steel No. 1 to steel No. 7) all containing various components listed in Table 2 and the rest being made up of Fe and unavoidable impurities were hot-rolled to make hot-rolled steel strips all with a thickness of 2.5 mm. Then, the hot-rolled steel strips were annealed (hot-rolled sheet annealing) at 900 ° C for 1 minute. Then, acid pickling was carried out and cold rolling was carried out to manufacture cold rolled steel strips and all 0.35 mm thick.

    [0050] Subsequently, the annealing finish was performed under the conditions listed in Table 3, and the main component and the thickness of each of the external oxide films formed (oxide layers) were examined. The identification of the main component of the external oxide film was carried out by an infrared reflection-absorption spectrum, and the thickness of the external oxide film was examined through observation by transmission electron microscope.
    [0051] Next, the application and cooking of a coating solution was carried out under the conditions listed in Table 3 in order to form the insulating films applying traction. In Table 3, in the "COATING SOLUTION" column, "S" means that the coating solution containing colloidal silica, aluminum phosphate and chromic acid was used, and "A" means that the coating solution containing boric acid and sol alumina was used.
    [0052] Then, the adherence of each of the insulating films was evaluated. The result is also listed in Table 3. In Table 3, the "x" in the "ADHESION" column means that if the electric steel sheet is not oriented around a circular bar 30 mm in diameter, the insulating film has peeled off. Further, the "o" means that in the case of wrapping an electric steel sheet not oriented around a circular bar with a diameter of 30 mm, the insulating film did not peel, but that in the case of this steel sheet for purposes electrical appliances have been wrapped around a circular bar 20 mm in diameter, the insulating film has peeled off. The "◎" means that even when the electric steel sheet is not oriented around a circular bar with a diameter of 20 mm, the insulating film has not peeled off.
    [0053] In addition, the evaluation of an improvement rate in the magnetic loss in the L direction was also carried out. In the evaluation, the W1 value of magnetic loss (W10 / 50) of each non-oriented electric steel sheet manufactured by the method described above was measured to be compared to a W0 value of magnetic loss (W10 / 50) of a reference sample. A plate was used as a reference sample, in which insulating films were formed by the application of a coating solution containing phosphate and acrylic resin described in Open Patent Publication for Japanese Public Inspection No. 06-330338 instead of being used. traction insulating films. The reason why such an evaluation was carried out is because the absolute value of magnetic loss depends on the component and the conditions of the process. The result is also listed in Table 3. The numerical value in the column "MAGNETIC LOSS IMPROVEMENT RATE IN DIRECTION L" is a value expressed by "(W0 - W1) / W0." Table 3


    [0054] As listed in Table 3, if the condition of the present invention is satisfied, the adhesion of the insulating film and the magnetic property in the L direction were extremely good. Furthermore, in the case that the outer oxide film did not form and the inner oxide layer formed, the adhesion was extremely low. (Second Experiment)
    [0055] The steel plates of No. 1, No. 3, and No. 4 steels listed in Table 2 were hot rolled to manufacture hot rolled steel strips all 2.5 mm thick. Then, the hot-rolled steel strips were re-heated (hot-rolled sheet annealing) at 900 ° C for 1 minute. Subsequently, acid pickling and cold rolling were carried out to manufacture cold rolled steel strips, each 0.35 mm thick.
    [0056] Subsequently, a coating solution was applied under the conditions listed in Table 3. Next, the annealing of finishing and cooking of the coating solution was carried out under the condition listed in the Table 4. That is, the processes in accordance with the flowchart illustrated in figure 6 were carried out in the following experiment, whereas the processes in accordance with the flowchart illustrated in figure 5 were carried out in the first experiment. Then, similarly to the first experiment, the adherence of each insulating film and the rate of improvement in the magnetic loss in the L direction were evaluated. The result is also listed in Table 4. Table 4

    [0057] As listed in Table 4, also in case the annealing finish and cooking of the coating solution are carried out in combination according to the flow chart illustrated in figure 6, the extremely good adhesion of the insulating film and the extremely magnetic property good direction L could be obtained. INDUSTRIAL APPLICABILITY
    [0058] The present invention can be used in, for example, an electric steel sheet manufacturing industry and an industry in which electric steel sheets are used.
    权利要求:
    Claims (20)
    [0001]
    1. Non-oriented electric steel plate, characterized by the fact that it comprises: a base iron, an external oxide film containing at least one type of oxide selected from the group consisting of Si, Al and Cr in which the oxides are SiO2 , Al2O3 and Cr2O3, or (Al, Cr2) O3, and with a thickness of not less than 0.01 pm and not more than 0.5 pm formed on a surface of the base iron; and a traction insulating film of not less than 1 g / m2 and not more than 6 g / m2 on the surface of the base iron, in which the base iron contains: Si, Al and Cr: not less than 2% by weight and not more than 6% by weight of the total content; and Mn: not more than 0.1% by weight and not more than 1.5% by weight, a C content of the base iron is equal to or less than 0.005% by weight, and the rest of the base iron is composed of Fe and unavoidable impurities.
    [0002]
    2.Steel sheet according to claim 1, characterized by the fact that the total content of Al and Cr of the base iron is equal to or greater than 0.8% by weight.
    [0003]
    3.Steel sheet according to claim 1, characterized by the fact that the insulating film is formed by cooking a coating solution containing phosphate and colloidal silica.
    [0004]
    4.Steel sheet according to claim 1, characterized by the fact that the insulating film is formed by cooking a coating solution containing boric acid and alumina sol.
    [0005]
    5.Steel sheet according to claim 2, characterized by the fact that the insulating film is formed by cooking a coating solution containing phosphate and colloidal silica.
    [0006]
    Steel sheet according to claim 2, characterized by the fact that the insulating film is formed by cooking a boric acid coating solution and an alumina sol.
    [0007]
    7. Method of manufacturing a non-oriented electric steel sheet, characterized by the fact that it comprises: the completion of the annealing of finishing of a strip of cold-rolled steel; and the formation of a traction insulating film of no less than 1 g / m2 and no more than 6 g / m2 on the cold-rolled steel strip, where the cold-rolled steel strip contains: Si, Al, and Cr: not less than 2% by weight and not more than 6% by weight of the total content; and Mn: not less than 0.1% by weight and not more than 1.5% by weight, a C content of the cold-rolled steel strip is equal to or less than 0.005% by weight, the The remainder of the cold-rolled steel strip is composed of unavoidable im-purities, and the completion of annealing finish includes the formation of an external oxide film containing at least one type of oxide selected from the group consisting of Si, Al and Cr, where the oxides are SiO2, Al2O3 and Cr2O3, or (Al, Cr2) O3, and with a thickness of not less than 0.01 pm and not more than 0.5 pm on the surface of the steel strip cold rolled steel with a predetermined temperature for cold rolled steel strip not less than 800 ° C and not higher than 1100 ° C in an atmosphere, where the total Si and Al content of the cold rolled steel strip is represented by X (mass%), a partial pressure ratio of water vapor to hydrogen is equal to or less than 0.005 x X2.
    [0008]
    8. Method, according to claim 7, characterized by the fact that the formation of the insulating film comprises, after the completion of the annealing finish: the application of a coating solution to the surface of the cold-rolled steel strip; and carrying out the cooking of the coating solution with a predetermined temperature of the cold rolled steel strip of not less than 800 ° C and not more than 1100 ° C.
    [0009]
    9. Method according to claim 8, characterized by the fact that the coating solution contains phosphate and colloidal silica.
    [0010]
    Method according to claim 8, characterized in that the coating solution contains boric acid and an alumina sol.
    [0011]
    11. Method according to claim 7, characterized by the fact that the formation of the insulating film comprises: the application of a coating solution to the surface of the cold-rolled steel strip before the completion of the annealing; and carrying out the cooking of the coating solution during the finish annealing.
    [0012]
    12. Method according to claim 11, characterized by the fact that the coating solution contains phosphate and colloidal silica.
    [0013]
    13. Method according to claim 11, characterized by the fact that the coating solution contains boric acid and an alumina sol.
    [0014]
    14. Method according to claim 7, characterized by the fact that the total content of Al and Cr of the cold-rolled steel strip is equal to or greater than 0.8% by weight.
    [0015]
    15. Method according to claim 8, characterized by the fact that the total content of Al and Cr of the cold-rolled steel strip is equal to or greater than 0.8% by weight.
    [0016]
    16. Method according to claim 9, characterized by the fact that the total content of Al and Cr of the cold rolled steel strip is equal to or greater than 0.8% by weight.
    [0017]
    17. Method according to claim 10, characterized by the fact that the total content of Al and Cr of the cold rolled steel strip is equal to or greater than 0.8% by weight.
    [0018]
    18. Method according to claim 11, characterized by the fact that the total content of Al and Cr of the cold-rolled steel strip is equal to or greater than 0.8% by weight.
    [0019]
    19. Method according to claim 12, characterized by the fact that the total content of Al and Cr of the cold-rolled steel strip is equal to or greater than 0.8% by weight.
    [0020]
    20. Method according to claim 13, characterized by the fact that the total content of Al and Cr of the cold rolled steel strip is equal to or greater than 0.8% by weight.
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    法律状态:
    2017-08-01| B25D| Requested change of name of applicant approved|Owner name: NIPPON STEEL AND SUMITOMO METAL CORPORATION (JP) |
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2019-02-05| B06T| Formal requirements before examination|
    2019-09-10| B25D| Requested change of name of applicant approved|Owner name: NIPPON STEEL CORPORATION (JP) |
    2019-10-01| B15K| Others concerning applications: alteration of classification|Free format text: AS CLASSIFICACOES ANTERIORES ERAM: C23C 22/00 , C21D 8/12 , C21D 9/46 , C22C 38/00 , C22C 38/06 , C22C 38/16 , C23C 8/18 , H01F 1/16 Ipc: C22C 38/02 (1974.07), C22C 38/06 (1974.07), C22C 3 |
    2020-02-18| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|
    2020-07-21| B09A| Decision: intention to grant|
    2020-12-01| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 15/02/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    JP2010-033937|2010-02-18|
    JP2010033937|2010-02-18|
    PCT/JP2011/053096|WO2011102328A1|2010-02-18|2011-02-15|Non-oriented electromagnetic steel sheet and process for production thereof|
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