WO2014017590A1 - 方向性電磁鋼板の製造方法 - Google Patents
方向性電磁鋼板の製造方法 Download PDFInfo
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Definitions
- the present invention relates to a method for producing a grain-oriented electrical steel sheet having excellent iron loss characteristics.
- a grain-oriented electrical steel sheet is a soft magnetic material whose crystal orientation is highly integrated in the Goss orientation ( ⁇ 110 ⁇ ⁇ 001>), and is mainly used for transformer iron cores, motor iron cores, and the like.
- grain oriented electrical steel sheets used for transformers are strongly required to have low iron loss in order to reduce no-load loss (energy loss).
- As means for reducing iron loss, reduction of plate thickness, increase of Si addition amount, improvement of orientation of crystal orientation, application of tension to steel plate, smoothing of steel plate surface, refinement of secondary recrystallization structure, etc. Is known to be effective.
- Patent Document 1 discloses a heating rate of 100 ° C./s or more in a non-oxidizing atmosphere in which P H2O / PH2 is 0.2 or less immediately before decarburization annealing of a cold-rolled steel sheet rolled to a final thickness.
- Patent Document 1 discloses a heating rate of 100 ° C./s or more in a non-oxidizing atmosphere in which P H2O / PH2 is 0.2 or less immediately before decarburization annealing of a cold-rolled steel sheet rolled to a final thickness.
- a technique for obtaining a grain-oriented electrical steel sheet with low iron loss by heating to a temperature of 700 ° C. or higher is disclosed.
- Patent Document 3 film characteristics and magnetic characteristics are obtained by heating a temperature range of 600 ° C. or higher to 800 ° C. or higher at a rate of temperature increase of 95 ° C./s and appropriately controlling the atmosphere in this temperature range.
- a technique for obtaining an electrical steel sheet that is superior to the above is disclosed.
- the present invention has been made in view of the above problems in the prior art, and its purpose is to increase the temperature rise rate when primary recrystallization annealing is as high as 80 ° C./s or more as in the prior art.
- the object is to propose a manufacturing method capable of stably obtaining a grain-oriented electrical steel sheet with low iron loss.
- the inventors have studied the ideal heat cycle in the primary recrystallization annealing, particularly the heating rate (heating pattern) from various viewpoints.
- the purpose of rapid heating to a temperature of about 700 ° C. in the temperature raising process in the primary recrystallization annealing is a temperature range in which recrystallization of ⁇ 222 ⁇ : ⁇ fiber ⁇ 111 ⁇ fiber structure easily proceeds preferentially.
- a temperature range such as 550 ° C. and 580 ° C. in a short time, it is considered that recrystallization of ⁇ 110 ⁇ : Goth structure ⁇ 110 ⁇ ⁇ 001> is relatively promoted.
- the present invention contains C: 0.001 to 0.10 mass%, Si: 1.0 to 5.0 mass%, Mn: 0.01 to 0.5 mass%, and Al: 0.0100 mass%. Less than, S, Se, O, and N: each reduced to 0.0050 mass% or less, the steel slab having a composition composed of Fe and unavoidable impurities in the remainder is hot-rolled and subjected to or after hot-rolled sheet annealing Without making the final sheet thickness by one or two or more cold rolling sandwiching the intermediate annealing, after the primary recrystallization annealing, and then applying the annealing separator and finish annealing In the production method, rapid heating is performed at an average temperature increase rate of 40 to 200 ° C./s between 550 and 700 ° C.
- the steel slab in the method for producing a grain-oriented electrical steel sheet according to the present invention further includes Cu: 0.01 to 0.2 mass%, Ni: 0.01 to 0.5 mass%, Cr: 0.00% in addition to the above component composition. 01 to 0.5 mass%, Sb: 0.01 to 0.1 mass%, Sn: 0.01 to 0.5 mass%, Mo: 0.01 to 0.5 mass%, Bi: 0.001 to 0.1 mass% Ti, 0.005 to 0.02 mass%, P: 0.001 to 0.05 mass%, and Nb: 0.0005 to 0.0100 mass%, or one or more selected from And
- the method for producing a grain-oriented electrical steel sheet according to the present invention is characterized in that sulfide and / or sulfate is added to the annealing separator, or nitriding is performed after the primary recrystallization.
- the present invention even when the temperature rising rate in the temperature raising process of the primary recrystallization annealing is relatively low, the effect of refining secondary recrystallized grains equal to or higher than that of the prior art that rapidly heats at a high temperature rising rate is achieved. Therefore, it is possible to easily and stably obtain a grain-oriented electrical steel sheet with low iron loss.
- 3 is a graph showing the influence of a heating pattern on the relationship between a heating rate between 550 and 700 ° C. and iron loss. It is a graph which shows the influence which a heating pattern has on ⁇ 110 ⁇ inverse strength.
- the test piece was heated to 700 ° C. at various heating rates using an electric heating device, then heated to 800 ° C. at 30 ° C./s, and held for 60 seconds in a wet hydrogen atmosphere.
- a primary recrystallization annealing was performed which also served as a carbon annealing.
- the heating in the primary recrystallization annealing is performed by heating pattern 1 in which the temperature is continuously increased from room temperature to 700 ° C. at a constant temperature increase rate and heated between 700 ° C. and 800 ° C. at a constant temperature increase rate;
- the heating pattern 2 was held for 3 seconds at 450 ° C. during heating up to 700 ° C., and the heating pattern 3 was held for 15 seconds at a temperature of 450 ° C. during heating up to 700 ° C.
- the heating rate in the heating patterns 2 and 3 is the heating rate before and after the holding, and the atmosphere conditions and the like in the heating patterns 2 and 3 are all the same as those in the heating pattern 1.
- Test specimens of the same dimensions are collected from the same position of the cold rolled coil obtained in Experiment 1, and continuously heated from room temperature to 700 ° C. at an annealing rate of 40 ° C./100° C./s using an electric heating device.
- an electric heating device When heating from room temperature to 700 ° C. at an annealing rate of 100 ° C./s, after heating at 400 ° C., 500 ° C., or 600 ° C. during heating for 3 seconds, 700 ° C. To 800 ° C. at a temperature rising rate of 30 ° C./s, and subjected to primary recrystallization annealing also serving as decarburization annealing for 60 seconds in a wet hydrogen atmosphere.
- the inverse strength was measured by the X-ray diffraction method. When held at 400 ° C. and 500 ° C., it was held at 600 ° C. or at 40 ° C./s. Compared to the case of continuous heating, the ⁇ 110 ⁇ inverse strength is high and equal to or higher than that when rapidly heated at 100 ° C./s, that is, the Goss orientation ( ⁇ 110 ⁇ ) that becomes the nucleus during secondary recrystallization ⁇ 001>) It was confirmed that the recrystallization of grains was promoted.
- the mechanism by which this phenomenon occurs is considered as follows.
- the driving force that causes recrystallization is strain energy, that is, it is considered that the release of strain energy is likely to occur in a portion with high strain energy
- technical literature Shiraiwa, Terasaki, Kodama, “Al killed steel The phenomenon of ⁇ 222 ⁇ preferentially recrystallized in the Japan Institute of Metals, Vol. 35, No. 1, p. 20) is preferentially recrystallized in the ⁇ 222 ⁇ structure. It shows that high strain energy is accumulated.
- the strain energy decreases, and the driving force for causing recrystallization of the ⁇ 222 ⁇ structure significantly decreases. Since the ⁇ 222 ⁇ structure needs to exist in a certain amount as the structure phagocytosed by the Goss grains, the recrystallization of the ⁇ 222 ⁇ structure is suppressed excessively, and thus the primary recrystallization sufficient for the secondary recrystallization. It is likely that the organization was not obtained. Therefore, when the heating rate is relatively slow, it is considered that the same effect as when the heating rate is high is obtained only when the tissue recovery temperature range is maintained for a very short time, and the heating rate is high. In this case, it is considered that the same effect as that obtained under the condition where the heating rate is higher is obtained.
- C 0.001 to 0.10 mass%
- C is a component useful for the generation of goth-oriented crystal grains, and needs to be contained in an amount of 0.001 mass% or more in order to effectively exhibit such action.
- C is set in the range of 0.001 to 0.10 mass%. Preferably, it is in the range of 0.01 to 0.08 mass%.
- Si 1.0 to 5.0 mass%
- Si has the effect of increasing the electrical resistance of steel and lowering the iron loss, and needs to contain at least 1.0 mass%. On the other hand, addition exceeding 5.0 mass% makes it difficult to cold-roll. Therefore, Si is set in the range of 1.0 to 5.0 mass%. Preferably, it is in the range of 2.0 to 4.5 mass%.
- Mn 0.01 to 0.5 mass%
- Mn is an element effective for improving the hot workability of steel, and needs to be contained in an amount of 0.01 mass% or more. On the other hand, addition exceeding 0.5 mass% is not preferable because the austenite fraction increases during hot rolling and the texture deteriorates. Therefore, Mn is in the range of 0.01 to 0.5 mass%. Preferably, it is in the range of 0.01 to 0.10 mass%.
- Al Less than 0.0100 mass%, N, S, Se: each 0.0050 mass% or less
- Al, N, S, and Se are components that form inhibitors, and when added excessively, the temperature that causes secondary recrystallization increases. In addition, it becomes difficult to control secondary recrystallization.
- an inhibitor forming element when such an inhibitor forming element is present in a large amount, not only a high slab heating temperature is required for solid solution dispersion, but also when the slab heating temperature is insufficient, coarse AlN, MnS , MnSe, etc. cause the primary recrystallization structure to be non-uniform and cause secondary recrystallization failure. Therefore, it is necessary to reduce Al to less than 0.0100 mass% and N, S, and Se to 0.0050 mass% or less.
- Al is 0.0050 mass% or less
- N, S, and Se are each 0.0030 mass% or less.
- the balance other than the above components is Fe and inevitable impurities.
- O since O has an inhibitory effect of inhibiting the secondary recrystallization by forming an oxide, it is desirable to reduce it to 0.0050 mass% or less in the steelmaking stage for manufacturing the steel slab.
- the grain-oriented electrical steel sheet targeted by the present invention includes Cu: 0.01 to 0.2 mass%, Ni: 0.01 to 0.5 mass%, Cr: 0.01 in addition to the essential components described above.
- Ti: 0.005 to 0.02 mass%, P: 0.001 to 0.05 mass%, and Nb: 0.0005 to 0.0100 mass% can be contained.
- the addition of these elements can suppress fluctuations in the size of primary recrystallized grains due to temperature variations during the manufacturing process.
- the addition amount is less than the lower limit value of the above range, the above effect cannot be obtained sufficiently.
- the addition amount exceeds the upper limit value of the above range, poor appearance of the coating and secondary recrystallization are likely to occur.
- the crystal grains gradually become coarse even in the initial stage of the secondary recrystallization annealing.
- the particle size at the time of primary recrystallization may be large.
- the primary recrystallization grain size before secondary recrystallization needs to be suppressed to a certain extent, specifically 35 ⁇ m or less. The driving force is lost, and secondary recrystallization failure may occur.
- conventional techniques for nitriding before secondary recrystallization are applied, or sulfides and sulfates are added to the annealing separator to cause sulfurization in the steel sheet. It is also possible to moderately suppress grain growth during secondary recrystallization annealing and suppress secondary recrystallization failure.
- the method for producing a grain-oriented electrical steel sheet according to the present invention is a method of hot rolling a steel slab having the above-described component composition, and after or without hot-rolled sheet annealing, at least once with or without intermediate annealing.
- This is a manufacturing method comprising a series of steps in which cold rolling is performed to obtain a final plate thickness, followed by primary recrystallization annealing, followed by application of an annealing separator and secondary recrystallization annealing.
- the method for producing the steel slab is not particularly limited, and the steel slab can be produced by melting the steel having the above-described component composition by a conventionally known refining process and using a continuous casting method, an ingot-bundling rolling method, or the like.
- the steel slab is then subjected to hot rolling, but the reheating temperature of the steel slab prior to hot rolling is not particularly limited as long as it is capable of rolling in the component system of the present invention in which an inhibitor is not actively added.
- the reheating temperature of the steel slab prior to hot rolling is not particularly limited as long as it is capable of rolling in the component system of the present invention in which an inhibitor is not actively added.
- the hot-rolled hot-rolled sheet is subjected to cold-rolling of the final thickness after hot-rolled sheet annealing or by hot-rolled sheet annealing, or by cold rolling at least twice with intermediate annealing interposed therebetween.
- a board there is no restriction
- the cold-rolled sheet having the above final thickness is subjected to primary recrystallization annealing.
- primary recrystallization annealing rapid heating is performed at an average temperature increase rate of 40 to 200 ° C./s between 550 and 700 ° C., and as a preceding step, 10 ° C. / It is necessary to keep the temperature rising rate below s for 1 to 10 seconds.
- the reason why the temperature range for rapid heating is in the range of 550 to 700 ° C.
- the temperature range is a temperature range where ⁇ 222 ⁇ is preferentially recrystallized, as disclosed in the technical literature described above, By rapidly heating this temperature range, it is possible to promote the generation of the ⁇ 110 ⁇ ⁇ 001> orientation that becomes the nucleus of secondary recrystallization. As a result, the secondary recrystallized structure is refined and iron loss is reduced. It is because it is improved.
- the reason for setting the average temperature increase rate in the above temperature range to 40 to 200 ° C./s is that the effect of improving the iron loss is not sufficient if it is less than 40 ° C./s. This is because the iron loss improvement effect is saturated.
- the reason for maintaining a temperature rising rate of 10 ° C./s or less in any temperature range between 250 ° C. and 550 ° C. for 1 to 10 seconds is that the temperature rising rate is lower than that in the conventional technique in which the temperature is continuously increased. This is because the effect of improving the iron loss can be obtained even by heating between 550 and 700 ° C.
- the heating rate of 10 ° C./s or less may be a negative heating rate as long as the steel plate temperature does not deviate from the range of 250 to 550 ° C.
- the technical idea of the present invention is to reduce the recrystallization superiority of ⁇ 222 ⁇ by holding for a short time in a temperature range in which dislocation density is reduced and recrystallization does not occur. Therefore, the above effect cannot be obtained at less than 250 ° C. at which dislocation transfer is hardly expected.
- ⁇ 222 ⁇ recrystallization begins to occur, and even when maintained at a temperature of more than 550 ° C., ⁇ 110 ⁇ Generation of ⁇ 001> orientation cannot be promoted.
- the holding time if the holding time is less than 1 second, the holding effect is not sufficient.
- the holding time exceeds 10 seconds, the recovery may proceed excessively and secondary recrystallization failure may occur.
- the steel sheet that has been subjected to the primary recrystallization annealing satisfying the above conditions is then subjected to finish annealing for secondary recrystallization after applying and drying an annealing separator on the steel sheet surface.
- an annealing separator for example, MgO as a main component and optionally added TiO 2 or the like as needed, or SiO 2 or Al 2 O 3 as a main component can be used.
- the conditions for finish annealing are not particularly limited, and may be performed according to a conventional method.
- the steel sheet is then coated with an insulating coating on the surface of the steel sheet, or coated with an insulating coating on the surface of the steel sheet, and then subjected to flattening annealing that combines baking and shape correction.
- the type of the insulating coating is not particularly limited, but in the case of forming an insulating coating that applies a tensile tension to the steel sheet surface, Japanese Patent Laid-Open Nos. 50-79442 and 48-39338 are disclosed. It is preferable to bake at about 800 ° C. using a coating solution containing phosphate-chromic acid-colloidal silica disclosed in the above.
- the secondary recrystallized structure can be stably refined over almost the entire length of the product coil, and good iron loss characteristics can be imparted.
- a steel slab containing 0.01 mass% was heated at 1100 ° C. for 30 minutes, and then hot-rolled to a hot-rolled sheet having a thickness of 2.2 mm, and subjected to hot-rolled sheet annealing at 1000 ° C. for 1 minute. Cold rolling was performed to obtain a cold rolled coil having a final thickness of 0.23 mm.
- a sample of L: 300 mm ⁇ C: 100 mm was taken from the longitudinal direction and the center in the width direction of the cold-rolled coil thus obtained, and in the laboratory, the primary recycle that also served as decarburization annealing using an induction heating device. Crystal annealing was performed.
- this primary recrystallization annealing as shown in Table 1, a pattern (No. 1, No. 1) which is continuously heated from room temperature (RT) to 700 ° C. at a constant heating rate of 20 to 300 ° C./s. 2,9,11,13) and two types of patterns (No. 3 to 8, 10, 12) of heating between T1 and T2 during heating between the above temperatures for a predetermined time at a predetermined heating rate. After heating, 700 ° C.
- a steel slab having the composition shown in Table 2 is heated at 1200 ° C. for 20 minutes, and then hot rolled to form a hot-rolled sheet having a thickness of 2.0 mm and subjected to hot-rolled sheet annealing at 1000 ° C. for 1 minute.
- channel on the steel plate surface was given.
- the mixture was heated from room temperature to 750 ° C. at various heating rates similarly shown in Table 2, heated from 750 to 840 ° C.
- an annealing separator containing MgO as the main component and 10 mass% of TiO 2 is applied as a water slurry and applied and dried. Then, after winding on the coil and subjecting it to final finish annealing, a phosphate-based insulating tension coating was applied, and flattening annealing was performed for both baking and shape correction to obtain a product coil of grain-oriented electrical steel sheet.
- a test piece having a size of L: 320 mm ⁇ C: 30 mm was taken from the longitudinal direction and the width direction central portion of the product coil thus obtained, and the iron loss W 17/50 was measured by the Epstein test. It was written together in 2. From Table 2, No. 1 which performed the heating of primary recrystallization annealing on the conditions suitable for this invention. It can be seen that all the steel sheets 4 to 12 have excellent iron loss characteristics.
- Example 2 No. of Table 2 used in Example 2 was used. Samples with a width of 150 mm were collected from 1 hot-rolled sheet and heated at 1150 ° C. for 2 minutes at 1150 ° C. at one edge of the plate width (30 mm from the width end) and 1050 ° C. for 2 minutes. Thus, the crystal grains at one edge of the steel plate were coarsened.
- This treatment assumes that the steel sheet is overheated due to deceleration, etc. due to some trouble during annealing line passing, and the material whose crystal grains are coarsened at this stage is the same as the normal material.
- the post-process is a process, it is considered that secondary recrystallization failure is likely to occur due to changes in texture and primary recrystallization grain size.
- the hot-rolled sheet is cold-rolled to obtain a cold-rolled sheet having a final sheet thickness of 0.23 mm, and then heated from room temperature to 750 ° C. at a heating rate of 100 ° C./s, provided that the heating is performed at 450 ° C. For 3 seconds, heated from 750 to 800 ° C. at a heating rate of 25 ° C./s, and then subjected to primary recrystallization annealing also serving as decarburization annealing for decarburization in a wet hydrogen atmosphere.
- an annealing separator containing MgO as a main component and added with 5 mass% of TiO 2 in the form of a water slurry was applied and dried, and subjected to final finish annealing.
- 1-4 grain-oriented electrical steel sheets were obtained.
- no. No. 1 steel sheet was not held during the heating of the primary recrystallization annealing.
- No. 3 steel sheet was decarburized and then subjected to nitriding treatment.
- an annealing separator in which 10 mass% of MgSO 4 was added in addition to TiO 2 was used.
- the technology of the present invention can also be used for texture control of thin steel sheets.
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Abstract
Description
<実験1>
C:0.03mass%、Si:3.1mass%、Mn:0.03mass%を含有し、かつ、Al:0.0100mass%未満、S,Se,OおよびN:各0.0050mass%以下に低減し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを熱間圧延して熱延板とし、熱延板焼鈍を施し、1回の冷間圧延により板厚が0.30mmの冷延板(コイル)とした後、この冷延コイルの長手方向、幅方向の中央部から、L:300mm×C:100mmの試験片を30枚切り出した。
このようにして得た仕上焼鈍後の試験片について、SST(単板試験器)を用いて鉄損W17/50(商用周波数50Hzで磁束密度1.7Tまで励磁した際の鉄損)を測定し、その結果を図1に示した。この図から、加熱途中の450℃で3秒間保持する加熱パターン2の場合には、連続昇温する加熱パターン1の場合よりも良好な鉄損が得られており、例えば、加熱パターン2の場合には昇温速度40℃/sでも加熱パターン1の昇温速度80℃/sと同等の鉄損が得られている。これに対して、加熱途中の450℃で15秒間保持する加熱パターン3の場合には、全ての試験片で鉄損W17/50が1.10W/kg以上となり(図示せず)、さらに昇温速度が100℃/s以上では、二次再結晶自体が起きていなかった。
実験1で得た冷延コイルの同一位置から同一寸法の試験片を採取し、通電加熱装置を用いて、室温から700℃までを焼鈍速度40℃/sまたは100℃/sで連続して加熱する条件と、室温から700℃までを焼鈍速度100℃/sで加熱する際、加熱途中の400℃、500℃、600℃のいずれかの温度で3秒間保持する条件で加熱した後、700℃から800℃まで昇温速度30℃/sで加熱し、湿水素雰囲気中で60秒間保持する脱炭焼鈍を兼ねた一次再結晶焼鈍を施した。斯くして得られた一次再結晶焼鈍板について、X線回折法でインバース強度を測定したところ、400℃および500℃で保持した場合には、600℃で保持した場合や、40℃/sで連続加熱した場合と比較して{110}インバース強度が高く、100℃/sで急速加熱したときと同等以上となっていること、すなわち、二次再結晶時に核となるGoss方位({110}<001>)粒の再結晶が促進されていることが確認された。
一般に、再結晶を起こす駆動力は歪エネルギーである、すなわち、歪エネルギーの解放は、歪みエネルギーの高い部分において生じ易いと考えられており、技術文献(白岩、寺崎、小玉、「Alキルド鋼での等温焼鈍中の再結晶挙動」、日本金属学会誌、第35巻、第1号、p.20)において認められた{222}が優先的に再結晶するという現象は、{222}組織に高い歪エネルギーが蓄積されていることを示している。
C:0.001~0.10mass%
Cは、ゴス方位結晶粒の発生に有用な成分であり、かかる作用を有効に発現させるためには0.001mass%以上の含有を必要とする。一方、Cを0.10mass%を超えて含有すると、脱炭焼鈍において脱炭不良を起こすおそれがある。よって、Cは0.001~0.10mass%の範囲とする。好ましくは0.01~0.08mass%の範囲である。
Siは、鋼の電気抵抗を高めて鉄損を低下させる効果があり、少なくとも1.0mass%の含有を必要とする。一方、5.0mass%を超える添加は、冷間圧延することを困難とする。よって、Siは1.0~5.0mass%の範囲とする。好ましくは2.0~4.5mass%の範囲である。
Mnは、鋼の熱間加工性を向上させるのに有効な元素であり、0.01mass%以上含有させる必要がある。一方、0.5mass%を超える添加は、熱延時にオーステナイト分率が増加し、集合組織が劣化するため好ましくない。よって、Mnは0.01~0.5mass%の範囲とする。好ましくは0.01~0.10mass%の範囲である。
Al,N,SおよびSeは、インヒビターを形成する成分であり、過剰に添加すると二次再結晶を起こす温度が上昇し、二次再結晶を制御することが困難となる。また、このようなインヒビター形成元素が多く存在すると、その固溶分散のために、高いスラブ加熱温度が必要となるだけでなく、スラブ加熱温度が十分でなかった場合は、粗大化したAlN,MnS,MnSe等が一次再結晶組織を不均一にして二次再結晶不良を引き起こす原因となる。よって、Alは0.0100mass%未満、N,S,Seはそれぞれ0.0050mass%以下に低減する必要がある。好ましくは、Al:0.0050mass%以下、N,S,Se:それぞれ0.0030mass%以下である。
これらは、結晶粒径や表面に偏析したり、あるいは、炭窒化物を形成したりすることで、補助的なインヒビターとしての作用を有する元素である。インヒビターを積極的に添加しない本発明の成分系においては、これらの元素を添加することで、製造工程中の温度のバラつきによる一次再結晶粒の大きさの変動を抑制することができる。しかし、添加量が上記範囲の下限値未満では上記効果が十分に得られず、逆に、上記範囲の上限値を超えると被膜の外観不良や二次再結晶不良が発生しやすくなる。
本発明の方向性電磁鋼板の製造方法は、前述した成分組成を有する鋼スラブを熱間圧延し、熱延板焼鈍を施した後もしくは施すことなく、1回もしくは中間焼鈍を挟む2回以上の冷間圧延を施して最終板厚とした後、一次再結晶焼鈍を施し、その後、焼鈍分離剤を塗布して二次再結晶焼鈍を施す一連の工程からなる製造方法である。
上記鋼スラブは、その後、熱間圧延に供するが、熱間圧延に先立つ鋼スラブの再加熱温度は、インヒビターを積極的に添加しない本発明の成分系では、圧延可能な温度があればよく特に制限はないが、1100℃以上とするのが好ましい。
熱間圧延した熱延板は、熱延板焼鈍を施した後、あるいは熱延板焼鈍を施すことなく、1回または中間焼鈍を挟む2回以上の冷間圧延により、最終板厚の冷延板とする。なお、上記熱間圧延以降から冷間圧延までの製造条件については、特に制限はなく、常法に準じて行なえばよい。
ここで、急速加熱する温度域を550~700℃の範囲とする理由は、先述した技術文献に開示されているように、この温度域は、{222}が優先再結晶する温度範囲であり、この温度範囲を急速加熱することによって、二次再結晶の核となる{110}<001>方位の発生を促進することができ、その結果、二次再結晶組織を細粒化し、鉄損が改善されるからである。
また、上記温度範囲の平均昇温速度を40~200℃/sとする理由は、40℃/s未満では鉄損の改善効果が十分ではなく、一方、200℃/sより高くしても、鉄損改善効果が飽和するからである。
上記に説明した本発明の製造方法によれば、製品コイルのほぼ全長に亘って安定的に二次再結晶組織を細粒化し、良好な鉄損特性を付与することができる。
このようにして得た冷延コイルの長手方向および幅方向中央部から、L:300mm×C:100mmの試料を採取し、ラボにて、誘導加熱装置を用いて脱炭焼鈍を兼ねた一次再結晶焼鈍を施した。なお、この一次再結晶焼鈍では、表1に示したように、室温(RT)から700℃の間を一定の昇温速度20~300℃/sで連続的に加熱するパターン(No.1,2,9,11,13)と、上記温度間の加熱途中のT1~T2間を所定の昇温速度で所定時間加熱するパターン(No.3~8,10,12)の2種類のパターンで加熱した後、700℃から820℃までを昇温速度40℃/sで加熱し、湿水素雰囲気中で820℃×2分間の脱炭を施した。
次いで、上記一次再結晶焼鈍後の試料に、MgOを主成分とし、TiO2を5mass%添加した焼鈍分離剤を水スラリー状にして塗布・乾燥した後、最終仕上焼鈍を施し、リン酸塩系の絶縁張力コーティングを塗布・焼付けし、方向性電磁鋼板とした。
次いで、同じく表2に示した種々の昇温速度で室温から750℃まで加熱し、750から840℃までを昇温速度10℃/sで加熱してから、PH2O/PH2=0.3の湿水素雰囲気中で2分間保持する脱炭焼鈍を兼ねた一次再結晶焼鈍を施した後、MgOを主成分とし、TiO2を10mass%添加した焼鈍分離剤を水スラリー状にして塗布・乾燥し、コイルに巻き取り、最終仕上焼鈍を施した後、リン酸塩系の絶縁張力コーティングを塗布し、焼付と形状矯正を兼ねた平坦化焼鈍を施して方向性電磁鋼板の製品コイルとした。
次いで、上記熱延板を冷間圧延し、最終板厚0.23mmの冷延板とした後、室温から750℃まで昇温速度100℃/sで加熱し、ただし、上記加熱途中の450℃で3秒間保持し、750から800℃まで昇温速度25℃/sで加熱した後、湿水素雰囲気で脱炭する脱炭焼鈍を兼ねた一次再結晶焼鈍を施した。その後、MgOを主成分とし、TiO2を5mass%添加した焼鈍分離剤を水スラリー状にして塗布・乾燥し、最終仕上焼鈍を施して表3に示したNo.1~4の方向性電磁鋼板を得た。なお、上記方向性電磁鋼板の製造に際して、No.1の鋼板については、一次再結晶焼鈍の加熱途中での保持は行わず、No.3の鋼板については、脱炭後、窒化処理を施し、また、No.4の鋼板については、TiO2に加えてMgSO4を10mass%添加した焼鈍分離剤を用いた。
上記の結果を表3に併記した。なお、表3中に示した鉄損値は、高温加熱した片側エッジ部試験片の鉄損値も含む平均値である。この結果から、一次再結晶焼鈍の加熱途中の450℃で3秒間保持した鋼板は、いずれも鉄損特性が良好であり、中でも窒化処理を施したNo.3や、焼鈍分離剤中にMgSO4を添加したNo.4の鋼板では、高温加熱した片側エッジ部にも二次再結晶不良(二次再結晶が生じていない不良箇所)は認められず、鉄損特性も大きく改善されていることがわかる。
Claims (4)
- C:0.001~0.10mass%、Si:1.0~5.0mass%、Mn:0.01~0.5mass%を含有し、かつ、Al:0.0100mass%未満、S,Se,OおよびN:それぞれ0.0050mass%以下に低減し、残部がFeおよび不可避的不純物からなる成分組成の鋼スラブを熱間圧延し、熱延板焼鈍を施した後もしくは施すことなく、1回もしくは中間焼鈍を挟む2回以上の冷間圧延により最終板厚とした後、一次再結晶焼鈍を施し、その後、焼鈍分離剤を塗布して仕上焼鈍を施す方向性電磁鋼板の製造方法において、
前記一次再結晶焼鈍の加熱過程における550~700℃間を平均昇温速度40~200℃/sで急速加熱するとともに、250℃~550℃間のいずれかの温度域において昇温速度10℃/s以下で1~10秒間保持することを特徴とする方向性電磁鋼板の製造方法。 - 前記鋼スラブは、前記成分組成に加えてさらに、Cu:0.01~0.2mass%、Ni:0.01~0.5mass%、Cr:0.01~0.5mass%、Sb:0.01~0.1mass%、Sn:0.01~0.5mass%、Mo:0.01~0.5mass%、Bi:0.001~0.1mass%、Ti:0.005~0.02mass%、P:0.001~0.05mass%およびNb:0.0005~0.0100mass%のうちから選ばれる1種または2種以上を含有することを特徴とする請求項1に記載の方向性電磁鋼板の製造方法。
- 前記焼鈍分離剤中に硫化物および/または硫酸塩を添加することを特徴とする請求項1または2に記載の方向性電磁鋼板の製造方法。
- 前記一次再結晶後に窒化処理を施すことを特徴とする請求項1または2に記載の方向性電磁鋼板の製造方法。
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JP6350398B2 (ja) * | 2015-06-09 | 2018-07-04 | Jfeスチール株式会社 | 方向性電磁鋼板およびその製造方法 |
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KR20180087378A (ko) * | 2015-12-04 | 2018-08-01 | 제이에프이 스틸 가부시키가이샤 | 방향성 전자 강판의 제조 방법 |
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US20220112573A1 (en) * | 2019-01-16 | 2022-04-14 | Nippon Steel Corporation | Method for producing grain oriented electrical steel sheet |
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JP2015172223A (ja) * | 2014-03-11 | 2015-10-01 | Jfeスチール株式会社 | 方向性電磁鋼板の製造方法 |
JP2015193921A (ja) * | 2014-03-17 | 2015-11-05 | Jfeスチール株式会社 | 鉄損特性に優れる方向性電磁鋼板の製造方法 |
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US10428403B2 (en) | 2014-11-27 | 2019-10-01 | Jfe Steel Corporation | Method for manufacturing grain-oriented electrical steel sheet |
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RU2015105718A (ru) | 2016-09-10 |
RU2599942C2 (ru) | 2016-10-20 |
CN104160044A (zh) | 2014-11-19 |
JP5716870B2 (ja) | 2015-05-13 |
EP2878688B1 (en) | 2019-07-03 |
EP2878688A4 (en) | 2016-03-02 |
US9748028B2 (en) | 2017-08-29 |
JPWO2014017590A1 (ja) | 2016-07-11 |
KR20150010787A (ko) | 2015-01-28 |
EP2878688A1 (en) | 2015-06-03 |
US20150194247A1 (en) | 2015-07-09 |
IN2015DN00610A (ja) | 2015-06-26 |
CN104160044B (zh) | 2016-01-13 |
KR101625540B1 (ko) | 2016-05-30 |
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