WO2017195269A1 - ホットスタンプ成形体 - Google Patents
ホットスタンプ成形体 Download PDFInfo
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- WO2017195269A1 WO2017195269A1 PCT/JP2016/063856 JP2016063856W WO2017195269A1 WO 2017195269 A1 WO2017195269 A1 WO 2017195269A1 JP 2016063856 W JP2016063856 W JP 2016063856W WO 2017195269 A1 WO2017195269 A1 WO 2017195269A1
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- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 56
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 49
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
Definitions
- the present invention relates to a hot stamping molded body.
- Structural members used in automobiles and the like are sometimes manufactured by hot stamping (hot pressing) in order to increase both strength and dimensional accuracy.
- hot stamping hot pressing
- the steel material for hot stamping is heated to Ac 3 or more, and the steel material for hot stamping is rapidly cooled while being pressed with a mold. That is, in the manufacturing, pressing and quenching are performed simultaneously. According to the hot stamp, it is possible to produce a molded article with high dimensional accuracy and high strength.
- Patent Document 1 discloses a hot-pressed plated steel sheet on which a Zn plating layer is formed
- Patent Document 2 discloses an automotive member plated steel sheet on which an Al plating layer is formed
- Patent Literature 3 discloses a Zn-plated steel sheet for hot pressing in which various elements such as Mn are added to the plated layer of the Zn-plated steel sheet.
- these plated steel sheets have the following problems.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a hot stamping molded article excellent in fatigue characteristics, phosphate treatment properties, coating film adhesion and weldability.
- the gist of the present invention is as follows.
- a hot stamping molded body includes a base material; a plating layer, and the plating layer includes an interface layer and an intermediate layer in order from the base material side to the surface side.
- the oxide layer, and the interface layer includes ⁇ Fe, Fe 3 Al, and FeAl having a total structure of 99% by area or more, and an average Al content is 8.0% by mass or more and 32.5% by mass.
- the average Zn content is limited to more than 5% by mass of Zn content of the base material, the remainder of the chemical component contains Fe and impurities, and the average film thickness is 1.0 ⁇ m or more
- the intermediate layer includes Fe (Al, Zn) 2 and Fe 2 (Al, Zn) 5 having a total structure of 99 area% or more, an average Al content of 30 to 50% by mass, and an average Zn content The amount is 10 to 40% by mass, and the balance of the chemical components contains Fe and impurities.
- the average film thickness is 5.0 ⁇ m or more, and the oxide layer has an average film thickness of 0.1 to 3.0 ⁇ m.
- the interface layer may have an average film thickness of 1.0 to 10.0 ⁇ m.
- the plating layer further includes an average of more than 0 mass% and 10.0 mass% or less of Si, and the intermediate layer In the above, 0 to 50 area% of the Fe (Al, Zn) 2 and the Fe 2 (Al, Zn) 5 may be substituted with Fe (Al, Si).
- the alloy form of the plating layer, the amount of Al and Zn in the specific layer in the plating layer, and the thickness of the oxide formed as the outermost layer of the plating layer are improved. Yes.
- the fatigue property improvement of the molded product based on the suppression of the occurrence of LME, the improvement of the phosphate treatment property of the molded product, and the improvement of the coating film adhesion thereby All of the improvement of the weldability of the molded body can be achieved.
- FIG. 2 is an example of a cross-sectional SEM image showing a processed part of a molded body obtained by subjecting an Al—Zn-based plated steel material to hot V bending immediately after heating under the conditions of Example 1.
- FIG. It is an example of the cross-sectional SEM image which shows the process part of a molded object which carried out the hot V bending process immediately after heating Zn type plated steel materials on the conditions of Example 1.
- FIG. It is an example of the cross-sectional SEM image which shows the process part of the molded object which carried out the hot V bending process immediately after heating Al type plated steel materials on the conditions of Example 1.
- FIG. 6 shows the surface of a molded body when an Al—Zn-based plated steel material is rapidly cooled while being processed with a flat plate mold equipped with a water-cooling jacket immediately after being heated under the conditions of Example 1 and then subjected to phosphate treatment. It is an example of a SEM image (secondary electron image).
- a hot stamping molded body means what is obtained by performing hot stamping (hot pressing) on a plated steel material for hot stamping.
- the hot stamped molded body may be simply referred to as “formed body”, and the hot stamped plated steel material may be simply referred to as “steel material” or “plated steel material”.
- the present inventors examined the fatigue properties (LME resistance) and phosphate treatment properties of hot stamped bodies (Al—Zn-based plated steel materials, Zn-based plated steel materials, and Al-based plated steel materials).
- the inventors of the present invention have, in order from the base material side to the surface side, the plating layer of the hot stamp molded body includes an interface layer, an intermediate layer, and an oxide layer. Includes a total of 99 area% or more of ⁇ Fe, Fe 3 Al, and FeAl, and the Al content is in the range of 8.0 mass% to 32.5 mass% and decreases as the base material is approached.
- the Zn content is limited to 5% by mass or less, the remainder of the chemical component contains Fe and impurities, the average film thickness is 1.0 ⁇ m or more, and the intermediate layer has Fe ( Al, Zn) 2 and Fe 2 (Al, Zn) containing 5, 30 to 50 mass% average Al content is 10 to 40 mass% average Zn content, the remainder of the chemical composition of Fe And an impurity, and the average film thickness is 5.0 ⁇ m or more Ri, the oxide layer, when the average film thickness is 0.1 ⁇ m or more 3.0 ⁇ m or less, to obtain a knowledge of the fatigue properties and phosphating of hot stamping member are both good, and.
- the average film thickness means an average value of the maximum film thickness and the minimum film thickness of a target layer (film).
- the hot stamp molded body 1 includes a base material 10 and a plating layer 20.
- base_material of the hot stamping molded object which concerns on this embodiment is demonstrated.
- the improvement of the LME resistance and the phosphate treatment property, which is a problem of the hot stamped article according to the present embodiment, is realized by the configuration of the plating layer. Therefore, the base material of the hot stamp molded body according to the present embodiment is not particularly limited. However, when the component of the base material is within the range described below, in addition to LME resistance and phosphate treatment property, a molded body having suitable mechanical properties can be obtained.
- the unit “%” of the content of alloy elements contained in the base material means “mass%”.
- C preferably 0.05 to 0.40%
- the strength of the hot stamped molded body is increased.
- the C content of the base material exceeds 0.40%, the toughness of the base material of the molded body may be insufficient. Therefore, the C content of the base material may be 0.05 to 0.40%.
- a more preferable lower limit of the C content of the base material is 0.10%, and a still more preferable lower limit is 0.13%.
- a more preferable upper limit of the C content of the base material is 0.35%.
- Si (Si: preferably 0.5% or less)
- Si has the effect of deoxidizing steel.
- the Si content of the base material may be 0.5% or less.
- the upper limit value of the Si content of the base material is preferably 0.3%, and the upper limit value of the Si content of the base material is more preferably 0.2%.
- a more preferable lower limit value of the Si content of the base material can be determined according to a required deoxidation level, for example, 0.05%.
- Mn manganese (Mn: preferably 0.5 to 2.5%)
- Mn content of the base material may be 0.5 to 2.5%.
- a more preferable lower limit value of the Mn content of the base material is 0.6%, and a more preferable lower limit value is 0.7%.
- a more preferable upper limit value of the Mn content of the base material is 2.4%, and an even more preferable lower limit value is 2.3%.
- Phosphorus (P) is an impurity contained in steel.
- the P contained in the base material may segregate at the crystal grain boundaries of the base material to reduce the toughness of the base material of the molded body, and may reduce the delayed fracture resistance of the base material. Therefore, the P content of the base material may be 0.03% or less. It is preferable to reduce the P content of the base material as much as possible.
- S is an impurity contained in steel.
- S contained in the base material may form sulfides, thereby reducing the toughness of the base material of the molded body and reducing the delayed fracture resistance of the base material. Therefore, the S content of the base material may be 0.01% or less. It is preferable to reduce the S content of the base material as much as possible.
- Al content when used with respect to the base material of the molded body according to the present embodiment, this term means sol. It means the content of Al (acid-soluble Al).
- Aluminum (Al) is generally used for the purpose of deoxidizing steel. However, when the Al content is high, the Ac 3 point of the steel material before hot stamping rises, and the heating temperature necessary for quenching of the steel rises during hot stamping, which is not desirable for hot stamping production. Therefore, the Al content of the base material may be 0.10% or less. A more preferable upper limit value of the Al content of the base material is 0.05%. A more preferable lower limit of the Al content of the base material is 0.01%.
- N Nitrogen (N: preferably 0.01% or less) is an impurity contained in the steel.
- N contained in the base material may form nitrides and reduce the toughness of the base material of the molded body. Further, N contained in the base material is combined with B to reduce the amount of solid solution B when B is contained in the base material in order to improve the hardenability of the steel material before hot stamping, and the hardenability of B. The improvement effect may be reduced. Therefore, the N content of the base material may be 0.01% or less. It is preferable to reduce the N content of the base material as much as possible.
- the base material of the hot stamping molded body of the present embodiment can further contain one or more selected from the group consisting of B and Ti.
- B preferably 0 to 0.0050% Since B has a function of improving the hardenability of steel, it increases the strength of the base material of the molded body after hot stamping. However, this effect is saturated if the B content of the base material is too high. Therefore, the B content of the base material may be 0 to 0.0050%. A more preferable lower limit of the B content of the base material is 0.0001%.
- Ti contained in the base material combines with N contained in the base material to form a nitride.
- Ti and N are bonded in this way, the bonding between B of the base material and N of the base material is suppressed, and a decrease in the hardenability of the base material due to BN formation can be suppressed.
- Ti contained in the base material has an effect of making the austenite grain size finer when heated in a hot stamp due to its pinning effect, thereby increasing the toughness of the molded body.
- the Ti content of the base material may be 0 to 0.10%.
- a preferable lower limit of the Ti content of the base material is 0.01%.
- the base material constituting the hot stamped molded body of the present embodiment can further contain one or more selected from the group consisting of Cr and Mo.
- Cr preferably 0 to 0.5%
- Cr contained in the base material improves the hardenability of the base material of the steel before hot stamping.
- the base material has too much Cr content, Cr carbide is formed. This Cr carbide is difficult to dissolve during the heating of the hot stamp, may hinder the progress of austenitization, and may reduce the hardenability. Therefore, the Cr content of the base material may be 0 to 0.5%. A more preferable lower limit of the Cr content of the base material is 0.1%.
- Mo contained in the base material enhances the hardenability of the base material of the steel material before hot stamping.
- Mo content of the base material may be 0 to 0.50%.
- a more preferable lower limit of the Mo content of the base material is 0.05%.
- the base material constituting the hot stamping molded body of this embodiment may further contain one or more selected from the group consisting of Nb and Ni.
- Nb preferably 0 to 0.10%
- Nb contained in the base material forms carbides, refines the crystal grains of the base material during hot stamping, and increases the toughness of the molded body.
- the base material has too much Nb content, the above effect is saturated.
- the Nb content of the base material is too large, the hardenability of the base material may deteriorate. Therefore, the Nb content may be 0 to 0.10%.
- a more preferable lower limit of the Nb content of the base material is 0.02%.
- Ni contained in the base material increases the toughness of the base material of the molded body.
- the base material Ni further suppresses embrittlement due to the presence of molten Zn during heating with a hot stamp.
- the Ni content of the base material may be 0 to 1.0%.
- a more preferable lower limit of the Ni content of the base material is 0.1%.
- the balance of the chemical composition of the base material constituting the hot stamping molded body of the present embodiment is composed of Fe and impurities.
- an impurity means what may be contained in the ore or scrap as a raw material when manufacturing a molded object industrially, or the thing which may be mixed due to a manufacturing environment etc.
- the plating layer 20 of the hot stamp molded body 1 includes an interface layer 21, an intermediate layer 22, and an oxide layer 23 from the base material 10 side of the molded body 1 toward the surface side of the molded body 1. And sequentially.
- the interface layer is formed adjacent to the base material. Most of the structure of the interface layer is composed of ⁇ Fe, Fe 3 Al, and FeAl. That is, the interface layer of the hot stamping molded body according to the present embodiment is mainly composed of an Fe—Al alloy phase having a low Al content. There may be a slight inclusion in the interface layer due to impurities mixed during plating formation. However, the inventors, when observing the interface layer in the cross section of the plated layer of the hot stamping molded body, if the structure contains ⁇ Fe, Fe 3 Al, and FeAl in a total of 99 area% or more, as described above It was confirmed that the influence of inclusions can be ignored.
- the average Al content of the interface layer needs to be 8.0 mass% or more and 32.5 mass% or less.
- the Al content in the interface layer is not uniform, and the Al content in the interface layer decreases as it approaches the base material.
- the interface layer Zn exists in a solid solution state in the above-described Fe—Al alloy phase.
- the inventors have found that Zn hardly dissolves in the interface layer of the molded body according to the present embodiment, and the average Zn content of the interface layer is 5% by mass or less. Due to the presence of the interface layer, liquid metal embrittlement cracking (LME) can be suppressed.
- LME liquid metal embrittlement cracking
- Zn content of an interface layer may not be uniform, since LME will be suppressed as long as the average Zn content of an interface layer is 5 mass% or less, an interface layer is more than 5 mass% Zn. It may include a region containing. The Zn content in the interface layer is minimized at the interface between the interface layer and the base material. Therefore, the minimum value of the Zn content in the interface layer exceeds the Zn content of the base material.
- the configuration of the interface layer is schematically shown in FIG.
- the Al content in the interface layer 21 is not uniform.
- the Al content at the interface between the base material 10 and the interface layer 21 is the same as the Al content of the base material 10.
- the Al content increases, and the structure is the ⁇ Fe phase with the smallest Al content, the Fe 3 Al phase with the second smallest Al content, and the Al content third. It changes in the order of few FeAl phases.
- the Zn content at the interface between the base material 10 and the interface layer 21 is the same as the Zn content of the base material 10.
- the Zn content also increases as the distance from the interface between the base material 10 and the interface layer 21 increases. However, the amount is kept low, and the average Zn content in the entire interface layer 21 does not exceed 5 mass%. .
- the average film thickness of the interface layer When the average film thickness of the interface layer is less than 1.0 ⁇ m, the LME suppressing effect cannot be sufficiently obtained. Therefore, the average film thickness of the interface layer needs to be 1.0 ⁇ m or more. When the average film thickness of the interface layer is set to 2.0 ⁇ m or more, the above effect is exhibited at a higher level.
- the lower limit value of the average film thickness of the interface layer is more preferably 5.0 ⁇ m, 6.0 ⁇ m, or 7.0 ⁇ m. Although it is not necessary to specify the upper limit of the average film thickness of the interface layer, an interface layer having an average film thickness exceeding 15.0 ⁇ m is not preferable because it may deteriorate the performance such as corrosion resistance. Therefore, the upper limit value of the average film thickness of the interface layer is preferably 15.0 ⁇ m, more preferably 10.0 ⁇ m, 9.0 ⁇ m, or 8.0 ⁇ m.
- the intermediate layer 22 is a layer containing Fe, Al, and Zn, and is formed on the interface layer 21. Most of the structure of the intermediate layer is composed of Fe (Al, Zn) 2 and Fe 2 (Al, Zn) 5 .
- Fe (Al, Zn) 2 is a phase in which part of Al in FeAl 2, which is a kind of Fe—Al intermetallic compound, is substituted with Zn
- Fe 2 (Al, Zn) 5 is A part of Al in Fe 2 Al 5, which is a kind of Fe—Al intermetallic compound, is a phase in which Zn is substituted. In some cases, inclusions caused by impurities mixed during the formation of the plating are slightly included in the intermediate layer.
- the inventors when observing the intermediate layer in the cross section of the plated layer of the hot stamped molded body, contains Fe (Al, Zn) 2 and Fe 2 (Al, Zn) 5 having a total structure of 99 area% or more. In other words, it was confirmed that the influence of the inclusions as described above can be ignored.
- the chemical component of the intermediate layer includes, by unit mass%, Al having an average of 30% to 50% and Zn having an average of 10% to 40%. Moreover, the average Al content of the intermediate layer exceeds the average Al content of the interface layer.
- the average Al content of the intermediate layer is 30% by mass or more.
- the average Al content of the intermediate layer is 50% by mass or less when imparting excellent phosphate processing properties to the molded body. That is, when the average Al content of the intermediate layer is outside the range of 30 to 50% by mass, there is a very high possibility that the configuration of the interface layer or the oxide layer will be inappropriate.
- the lower limit value of the average Al content of the interface layer is preferably 32% by mass or 35% by mass. In this case, the LME suppressing effect of the interface layer can be expressed more reliably.
- the preferable upper limit of the average Al content of the interface layer is 50% by mass or 45% by mass, and in this case, the phosphate treatment property of the oxide layer can be further improved.
- the average Zn content of the intermediate layer is 10% by mass or more.
- the average Zn content in the intermediate layer is 30% by mass or less. That is, when the average Zn content in the intermediate layer is outside the range of 10 to 40% by mass, there is a very high possibility that the configuration of the interface layer or the oxide layer will be inappropriate.
- a preferable lower limit of the average Zn content in the intermediate layer is 12% by mass or 13% by mass, and in this case, the phosphate treatment property of the oxide layer can be further improved.
- a preferable upper limit of the average Zn content of the intermediate layer is 28% by mass or 25% by mass, and in this case, the LME suppressing effect of the interface layer can be more reliably exhibited.
- the film thickness of the intermediate layer does not directly affect the phosphatability and LME resistance of the molded body. However, when the thickness of the intermediate layer is small, the corrosion resistance performance of the molded body is lowered. Therefore, the thickness of the intermediate layer is preferably 5.0 ⁇ m or more. Moreover, when the film thickness of an intermediate
- an oxide layer 23 mainly composed of Zn oxide is formed as the outermost surface layer of the molded body on the surface side of the molded body of the intermediate layer.
- the oxide layer 23 is formed by oxidizing the plating of the hot stamping plated steel material in the heating process when manufacturing the hot stamping molded body.
- This oxide layer improves the phosphatability of the hot stamping body.
- the average film thickness of the oxide layer needs to be 0.1 ⁇ m or more.
- the average thickness of the oxide layer is 3.0 ⁇ m or less.
- the average film thickness of an oxide layer shall be 2.0 micrometers or less, since performance, such as a corrosion resistance of a molded object and weldability, is exhibited at a high level, it is preferable.
- the states of the interface layer, the intermediate layer, and the oxide layer can be specified by the following means.
- the Al content of the interface layer is obtained by cutting the molded body perpendicularly to the surface, polishing the cross section, and analyzing the Al content distribution in the region including the interface layer in this cross section with an analyzer such as EPMA. .
- the average Zn content of the interface layer, the average Al content and average Zn content of the intermediate layer, and the average Si content of the plating layer are obtained based on the concentration distribution obtained by the above method.
- the metal structures of the interface layer and the intermediate layer can be obtained by crystal structure analysis using TEM or the like.
- the thicknesses of the interface layer, the intermediate layer, and the oxide layer can be obtained by taking an enlarged photograph of the above-mentioned cross section with an electron microscope and performing image analysis on the enlarged photograph.
- the structure of the plating layer of the molded object which concerns on this embodiment is not substantially uniform along the direction parallel to the surface of a molded object.
- the thicknesses of the interface layer, the intermediate layer, and the oxide layer often differ between the processed region and the unprocessed region. Therefore, the analysis described above must be performed in an unprocessed area of the green body.
- a molded body in which the state of the plating layer in the unprocessed region is within the above-described range is regarded as the molded body according to the present embodiment.
- the alloy form of the interface layer and the intermediate layer constituting the plating layer, the Al content and the Zn content in the interface layer and the intermediate layer, and the interface layer are improved.
- the plating layer is preferably formed so that the total amount of Al and Zn in the plating layer is 20 g / m 2 or more and 100 g / m 2 or less.
- the total amount of Al and Zn in the plating layer 20 g / m 2 or more, the effects (fatigue properties and phosphate treatment properties) of the interface layer, intermediate layer, and oxide layer described above can be further enhanced. it can.
- the total amount is 100 g / m 2 or less, the raw material cost of the molded body can be suppressed, the manufacturing cost can be reduced, and the weldability of the hot stamped molded body can be further improved.
- the more preferable lower limit of the total amount of Al and Zn in the plating layer is 30 g / m 2 .
- a more preferable upper limit of the total amount of Al and Zn in the plating layer is 90 g / m 2 .
- the total amount of Al and Zn contained in the plating layer can be measured by dissolving the hot stamped product with hydrochloric acid and subjecting the solution to inductively coupled plasma emission spectroscopy (ICP analysis). By using this method, the amounts of Al and Zn can be obtained individually.
- ICP analysis inductively coupled plasma emission spectroscopy
- the plating layer preferably contains an average of more than 0 mass% and 10.0 mass% of Si.
- the average Si content in the plating layer is set to more than 0% by mass, the adhesion between the base material and the plating layer can be improved.
- the average Si content is 10.0% by mass or less, it is possible to prevent deterioration in performance such as corrosion resistance and weldability of the hot stamped molded body.
- the more preferable lower limit of the average Si content of the plating layer is 0.1% by mass or 0.3% by mass.
- a more preferable upper limit of the average Si content of the plating layer is 8.0% by mass.
- the hot stamped article according to the present embodiment has excellent characteristics, and therefore the lower limit value of the average Si content of the plating layer is 0% by mass.
- the phase configuration of the intermediate layer changes.
- the intermediate layer contains a total of 99 area% or more of Fe (Al, Zn) 2 and Fe 2 (Al, Zn) 5 , but the plating layer has an average of 0 mass.
- part of Fe (Al, Zn) 2 and Fe 2 (Al, Zn) 5 is replaced with Fe (Al, Si).
- Fe (Al, Si) is a phase in which a part of Al in FeAl is replaced by Si.
- the hot stamping molded product according to this embodiment is manufactured so that the average Si content of the plating layer is 10.0% by mass, the amount of Fe (Al, Si) in the intermediate layer is about 50 area%. Therefore, when the plating layer contains an average of more than 0 mass% and 10.0 mass% of Si, the intermediate layer has a total of 99 area% or more of Fe (Al, Zn) 2 , Fe 2 (Al, Zn) 5 and Fe (Al , Si), and the content of Fe (Al, Si) is 0 to 50 area%.
- the manufacturing method of the hot stamping molded body of this embodiment includes a step of manufacturing a hot stamped plated steel material and a step of hot stamping the hot stamped plated steel material.
- the step of manufacturing the hot stamped plated steel material includes a step of manufacturing a hot stamped plated steel material and a step of forming an Al—Zn plated layer on the hot stamped plated steel material.
- the manufacturing method of the hot stamping molded object which concerns on this embodiment includes a rust prevention oil film formation process and a blanking process as needed. Hereinafter, each process is explained in full detail.
- a plated steel material that is a material of the hot stamping molded body includes a base material and a plating layer.
- a base material for hot stamped steel is manufactured.
- a molten steel having the same chemical composition as that of the base material of the hot stamping molded body according to this embodiment exemplified above is manufactured, and a slab is manufactured by a casting method using this molten steel. Or you may manufacture an ingot by the ingot-making method using the molten steel manufactured as mentioned above.
- the base material (hot rolled sheet) of the hot stamped plated steel material is obtained by hot rolling the slab or the ingot. If necessary, the hot-rolled sheet is subjected to pickling treatment, and the cold-rolled sheet obtained by performing cold rolling on the hot-rolled sheet after pickling treatment is used as a base for the hot stamped plated steel material. It may be a material.
- plating process In the plating treatment step, an Al—Zn plating layer is formed on the base material of the hot stamped plated steel material to produce a hot stamped plated steel material.
- the Al content in the plating bath is 40 to 70% by mass, and the Zn content is 30 to 60% by mass.
- the Al content (concentration) and Zn content (concentration) of the plating bath are substantially the same as the Al content (concentration) and Zn content (concentration) of the plating layer of the hot stamping plated steel material.
- the average Al content (concentration) and the average Zn content (concentration) of the plating layer of the hot stamping body are lower than the Al content (concentration) and Zn content (concentration) of the plating bath. This is because the Fe concentration in the plating layer increases due to alloying that occurs between Al and Zn of the plating layer and Fe of the base material during hot stamping.
- the plating layer of the hot stamping plated steel may be referred to as an unalloyed plating layer.
- the average Al content and the average Zn content in the unalloyed plating layer are analyzed by inductively coupled plasma emission spectroscopy after dissolving the unalloyed plating layer in hydrochloric acid containing an acid corrosion inhibitor (inhibitor). It is measurable by doing.
- 0.1 to 15.0 mass% Si is added to the unalloyed plated layer of the hot stamped plated steel material. Furthermore, it is preferable to contain.
- the Si content of the unalloyed plating layer decreases because Fe diffuses into the plating layer during alloying of the base material and plating. Therefore, when the Si content of the unalloyed plating layer is 0 to 15% by mass, the Si content of the alloyed plating layer is 0 to 10% by mass.
- the formation method of the unalloyed plating layer may be a hot dipping process, spray coating process, vapor deposition, as long as the average Al content and average Zn content in the unalloyed plating layer are controlled as follows: Any other treatment such as plating treatment may be used.
- the plating process includes immersing the base material of the hot stamped plated steel in a hot dipping bath containing Al, Zn, impurities, and optionally Si. And a step of pulling up the base material of the hot stamping plated steel material to which the plating metal has adhered from the plating bath.
- the plating treatment may be performed according to a conventional method so that the chemical composition of the obtained unalloyed plating layer is in the range described above.
- the plating layer is formed with a total weight per unit area of Al and Zn in the plating layer of 20 g / m 2 or more and 100 g / m 2 or less with respect to the base material. It is preferable that In order to secure the total weight per unit area, in this step, the total weight per unit area of Al and Zn in the plating layer when the base material of the hot stamped plated steel material is pulled up from the plating bath is 20 g. It is important to set it to / g 2 or more and 100 g / m 2 or less. Note that the total weight per unit area of Al and Zn contained in the plating layer is slightly reduced during alloying due to oxidation and evaporation. Moreover, in this process, ensuring of the said total amount is realizable by adjusting suitably the pulling-up speed of the steel materials from a plating bath, and the flow volume of the gas of wiping.
- the hot stamped plated steel material manufactured by the above-described method includes a base material and an unalloyed plated layer, and the unalloyed plated layer comprises 40.0 to 70.0 mass% Al, 30.0 to 60.0% by mass of Zn and 0-15.0% by mass of Si are contained.
- the hot stamping molded body according to the present embodiment is obtained.
- the hot stamp condition will be described in detail.
- Hot stamp process In the hot stamping process, hot stamping is performed on the hot stamping plated steel material.
- the normal hot stamping is performed by heating a steel material to a hot stamping temperature range (hot working temperature range), then hot working the steel material, and further cooling the steel material.
- a hot stamping temperature range hot working temperature range
- the alloying of the plating layer proceeds sufficiently if the steel material is heated to the hot stamp temperature range, the normal hot stamp technology does not place importance on the control of the heating condition of the steel material.
- the hot stamping plated steel is heated to the alloying temperature range, and (2) the temperature of the hot stamping plated steel is changed to the alloying temperature. (3) The hot stamping plated steel is heated to the hot stamping temperature range, and (4) the hot stamping plated steel is hot worked and cooled. It has been described above that the present inventors have substantially stopped the temperature rise of the steel material within the alloying temperature range and then resumed the temperature rise when raising the temperature of the hot stamped plated steel material to the hot stamp temperature range. It was found to be essential for obtaining a plating layer having a structure.
- the hot stamping plated steel material is charged into a heating furnace (gas furnace, electric furnace, infrared furnace, etc.).
- the hot stamped plated steel material is heated to a temperature range of 500 to 750 ° C. (alloying temperature range) and held within this temperature range for 10 to 450 seconds.
- the base material Fe diffuses into the plating layer, and alloying proceeds.
- the non-alloyed plating layer changes from the base material side to the surface side of the formed body, including an interface layer, an intermediate layer, and an oxide layer.
- the above-mentioned holding time is the time when the temperature of the hot stamped plated steel material is within the alloying temperature range. As long as the above holding time condition is satisfied, the temperature of the hot stamped plated steel material may vary within the alloying temperature range during the temperature holding.
- the rate at which the plated layer is alloyed is extremely small, and the heating time is extremely extended. Is not preferable.
- the temperature of the hot stamped plated steel is maintained above the alloying temperature range, that is, above 750 ° C., the oxide growth on the surface of the plated layer is excessively promoted during this holding process, and is obtained after HS. The weldability of the molded product is reduced.
- the heating conditions for heating the plated steel material for hot stamping to the above alloying temperature range are not particularly limited. However, from the viewpoint of productivity, it is desirable that the heating time is short.
- the temperature of the hot stamped plated steel material is maintained within the alloying temperature range as described above, and thereafter, from Ac 3 point to 950 ° C.
- the hot stamped plated steel is heated and then hot worked. At this time, it is necessary to limit the time during which the temperature of the hot stamped plated steel material is within the temperature range of Ac 3 to 950 ° C. (oxidation temperature range) to 60 seconds or less. If the hot stamping plated steel material temperature is within the oxidation temperature range, an oxide layer on the surface of the plating layer grows.
- the oxide film grows too much, and there is a concern that the weldability of the formed body may deteriorate.
- the lower limit of the time during which the hot stamped plated steel material temperature is within the oxidation temperature range is more than 0 seconds.
- the hot stamping plated steel material is heated in a non-oxidizing atmosphere such as a 100% nitrogen atmosphere, an oxidized layer is not formed, so the hot stamping plated steel material must be heated in an oxidizing atmosphere such as an air atmosphere. There is.
- the conditions such as the heating rate and the maximum heating temperature are not particularly specified, and various conditions that allow hot stamping are selected. Can do.
- the hot stamping plated steel material taken out from the heating furnace is press-molded using a mold.
- the steel material is quenched by a mold simultaneously with the press molding.
- a cooling medium for example, water
- a hot stamping body can be manufactured by the above process.
- the hot stamped plated steel was heated using a heating furnace.
- the plated steel material for hot stamping may be heated by energization heating. Even in this case, the steel material is heated for a predetermined time by energization heating, and the steel material is press-molded using a mold.
- the rust-preventing oil film forming process is to form a rust-preventing oil film by applying rust-preventing oil to the surface of the hot stamping plated steel after the plating process and before the hot stamping process. May be included.
- the surface of the hot stamped plated steel material may be oxidized.
- the rust-preventing oil film forming step can suppress the formation of the scale of the molded body. Note that any known technique can be used as a method of forming the rust-preventing oil film.
- This step is a step of forming the steel material into a specific shape by performing a shearing process and / or a punching process on the plated steel material for hot stamping after the antirust oil film forming step and before the hot stamping step. .
- the sheared surface of the steel material after blanking is easily oxidized. However, if a rust-preventing oil film is formed in advance on the steel material surface, the rust-preventing oil spreads to some extent on the shear surface. Thereby, the oxidation of the steel material after blanking can be suppressed.
- the inventors formed an Al—Zn-based plating layer, a Zn-based plating layer, and an Al-based plating layer on the base material 10, respectively.
- the Al—Zn-based plating layer includes 55.0% by mass of Al and 45.0% by mass of Zn.
- the Zn-based plating layer is substantially composed of only Zn. In particular, it was made only of Al.
- a steel material (plated steel material composed of a base material and a plating layer) on which each plating layer is formed is charged into a first heating furnace, heated to 700 ° C., and held for 120 seconds within this temperature range. did. Thereafter, the plated steel material is immediately charged into a second heating furnace and heated to 900 ° C., and then the plated steel material is treated so that the time during which the steel material temperature is in the range of Ac 3 to 950 ° C. is 30 seconds. 2 was removed from the furnace. Immediately after the plated steel material was taken out of the second heating furnace, a hot V bending test was performed on the plated steel material using a hand press machine.
- the time from the removal of the steel material from the furnace to the start of processing on the steel material was about 5 seconds, and the bending was performed at a steel material temperature of about 800 ° C.
- the V-bending was performed so that the outer diameter of the portion to be bent increased by about 15% from before the V-bending.
- the steel material was quenched to quench the steel material.
- the cooling was performed so that the cooling rate from about 800 ° C. to the martensitic transformation start point (about 410 ° C.) was 50 ° C./second or more.
- an SEM image of the bent outer side of the processed part of the molded body after cooling was taken, and the fatigue characteristics (LME resistance) of the molded body were evaluated based on whether or not LME was generated.
- 1 to 3 are cross-sectional photographs of a processed part of a molded body manufactured from an Al—Zn-based plated steel material, a Zn-based plated steel material, and an Al-based plated steel material.
- the alloyed Al—Zn-based plating layer 30 is formed on the base material 1
- the alloyed Zn-based plating layer 40 is formed on the base material 1.
- the alloyed Al-based plating layer 50 was formed on the base material 1.
- the observed processed part of the molded body is a part where the tensile process is performed, and is an outer part of the V-bend processed part where the occurrence of LME is concerned with respect to the bending center.
- the martensitic transformation start point (about 410 ° C.) Until the cooling rate was 50 ° C./second or more.
- the surface of the molded body was adjusted, and the molded body was subjected to phosphate treatment.
- an SEM image of the surface of the molded body was taken, and the phosphate processability was evaluated based on the degree of formation of the phosphate coating.
- FIGS. 4 to 6 show that the Al—Zn-based plated steel material, the Zn-based plated steel material, and the Al-based plated steel material taken out from the second heating furnace are rapidly cooled while being processed with a flat plate mold equipped with a water-cooling jacket. It is an example of the SEM image (secondary electron image) which shows the surface of these molded objects at the time of performing an acid salt process.
- slabs were manufactured by continuous casting using molten steel having the chemical composition shown in Table 1.
- the slab was hot-rolled to produce a hot-rolled steel material.
- the hot-rolled steel material was further pickled, and then cold-rolled to produce a cold-rolled steel material.
- this cold-rolled steel material was made into the base material (plate thickness 1.4mm) used for manufacture of a hot stamping molded object.
- the Ac 3 point of the base material was approximately 810 ° C.
- plating was formed on the base material thus manufactured using a plating bath having the composition shown in Table 2 to obtain a steel material for hot stamping.
- the adhesion amount of plating was controlled so that the total weight of Al and Zn was a value shown in Table 2.
- This steel was heated to the alloying temperature shown in Table 2, and the temperature was maintained for the alloying time shown in Table 2. Thereafter, the steel material is charged into a heating furnace and heated to a temperature range of Ac 3 to 950 ° C., and then the time during which the temperature of the steel material is within this temperature range becomes the holding time shown in Table 2, Was removed from the furnace.
- the steel material taken out from the heating furnace was immediately subjected to hot V bending using a hand press.
- the time from the start of taking out the steel material from the heating furnace to the start of the processing of the steel material was set to 5 seconds.
- the shape of the mold was such that the outer portion of the bending radius by the V bending process was extended by about 15% at the end of the bending process.
- the following steps were carried out in order to conduct a phosphate treatment evaluation test and a coating film adhesion evaluation test.
- the steel material taken out from the heating furnace was immediately hot stamped using a flat plate mold equipped with a water cooling jacket, and then accelerated cooled.
- the cooling rate was set to a cooling rate of 50 ° C./second or more up to the martensite transformation start point (410 ° C.).
- the surface adjustment was performed for 20 seconds at room temperature using the surface adjustment processing agent (brand name: Preparen X) by Nippon Parkerizing Co., Ltd. for each hot stamping molded object.
- each hot stamping molded body was subjected to phosphate treatment using a zinc phosphate treatment solution (trade name: Palbond 3020) manufactured by Nippon Parkerizing Co., Ltd.
- a zinc phosphate treatment solution (trade name: Palbond 3020) manufactured by Nippon Parkerizing Co., Ltd.
- the temperature of the treatment liquid was 43 ° C.
- the hot stamping molded body was immersed in the treatment liquid for 120 seconds.
- each hot stamping body was electrodeposited with a cationic electrodeposition paint manufactured by Nippon Paint Co., Ltd. by applying a slope of 160V, and further 20 at a baking temperature of 170 ° C. Baked for a minute.
- the average film thickness of the paint after electrodeposition coating was 10 ⁇ m in all the inventive examples and comparative examples.
- the states of the interface layer, the intermediate layer, and the oxide layer of the inventive example and the comparative example were specified by the following means.
- the average Al content and average Zn content of the interface layer, the average Al content and average Zn content of the intermediate layer, and the average Si content of the plating layer are obtained by cutting the molded body perpendicularly to the surface of the molded body, It was obtained by polishing the cross section and analyzing the cross section with an analyzer such as EPMA.
- the metal structures of the interface layer and the intermediate layer were obtained by crystal structure analysis using TEM or the like. An example in which the metal structure satisfies the provisions of the present invention was described as “OK”, and an example in which the metal structure did not satisfy was described as “NG”.
- the thicknesses of the interface layer, the intermediate layer, and the oxide layer were obtained by taking an enlarged photograph of the above-mentioned cross section with an electron microscope and performing image analysis on the enlarged photograph. The analysis described above was performed in an unprocessed area of the molded body.
- the total weight of Al and Zn in the plating layers of the inventive example and the comparative example was measured by high frequency inductively coupled plasma optical emission spectrometry (ICP-OES). That is, a sample was taken from an unprocessed portion (a portion that was not bent) of each invention example and comparative example, and the plating layer was dissolved with a 10% HCl aqueous solution and analyzed. Each element was identified and surveyed by applying plasma energy to each solution, exciting the constituent elements, and measuring the position and intensity of the emitted light lines (spectral lines).
- ICP-OES high frequency inductively coupled plasma optical emission spectrometry
- Table 3 shows configurations of invention examples and comparative examples confirmed by the above-described means.
- the balance of the average composition of the interface layer and the intermediate layer shown in Table 3 was Fe and impurities.
- the fatigue characteristics of the examples and comparative examples were evaluated by the following means.
- SEM scanning electron microscope
- a backscattered electron detector in the cross section of the steel material in the thickness direction of the V-bending portion of the examples and comparative examples.
- liquid metal embrittlement cracking The presence or absence of occurrence of LME was observed.
- GOOD favorable
- the phosphate treatment properties of the examples and comparative examples were evaluated by the following means.
- the phosphate coating formed on each phosphate-treated sample was dissolved and removed using an ammonium dichromate solution, and the difference in weight of the steel before and after removal of the coating was measured. It was regarded as the amount of coating.
- the sample whose adhesion amount is 2.0 g / m ⁇ 2 > or more was evaluated as favorable (GOOD) about phosphate processability.
- the amount of adhesion of the sample of less than 2.0 g / m 2 was evaluated as bad for phosphating properties (BAD).
- a sample having a coating film peeling rate of less than 5.0% was evaluated as good (GOOD) for coating film adhesion.
- GOOD coating film peeling rate
- BAD defective
- the weldability of the examples and comparative examples was evaluated by the surface resistance value.
- the surface resistance value of the sample was calculated from the voltage value when a current 2A was passed through the sample at a pressure of 250 kgf using a pressurized DC inverter power supply.
- a sample having a surface resistance value of 20 m ⁇ or less was evaluated as good for weldability (GOOD).
- Table 4 shows the fatigue properties (LME resistance), phosphate treatment properties, coating film adhesion, and weldability of the invention examples and comparative examples confirmed by the above-mentioned means.
- Comparative Example 101 was produced using a plating bath with insufficient Al content, LME could not be prevented. For this reason, the fatigue characteristics of Comparative Example 101 were poor. Since the comparative example 102 was manufactured using the plating bath with insufficient Zn content, the structure of the intermediate layer became inappropriate due to insufficient Zn. For this reason, in the comparative example 102, the phosphate processability was impaired and the coating film adhesion was poor. In Comparative Example 103, since the alloying temperature at the time of hot stamping was too high, the thickness of the oxide layer was excessive, and the weldability was poor.
- Comparative Example 104 since the alloying temperature at the time of hot stamping was too low, alloying of the plating layer became insufficient, a Zn-rich phase was generated, and LME could not be prevented. For this reason, the fatigue characteristics of Comparative Example 104 were poor.
- Comparative Example 105 the alloying time at the time of hot stamping was too long, so the thickness of the oxide layer was excessive and the weldability was poor.
- Comparative Example 106 the alloying time at the time of hot stamping was too short, so heating for alloying was insufficient. For this reason, in the comparative example 106, LME generate
- Comparative Example 106 since the heating was insufficient, the amount of oxide was small, and phosphate treatment property and coating film adhesion were insufficient.
- Comparative Example 107 since the alloying temperature and the holding time at the time of hot stamping were excessive, the thickness of the oxide layer was excessive and the weldability was poor.
- both the fatigue characteristics and the phosphate treatment properties are sufficiently exhibited for the hot stamped molded body in which the plating layer is formed on the surface of the base material. Therefore, the present invention is particularly promising in the field of structural members used in automobiles and the like.
Abstract
Description
(2)上記(1)に記載のホットスタンプ成形体では、前記界面層は、平均膜厚が1.0~10.0μmであってもよい。
(3)上記(1)または(2)に記載のホットスタンプ成形体では、前記めっき層中のAl及びZnの単位面積当たりの合計重量が20g/m2以上100g/m2以下であってもよい。
(4)上記(1)~(3)のいずれか一項に記載のホットスタンプ成形体では、前記めっき層は、平均0質量%超10.0質量%以下のSiをさらに含み、前記中間層において、前記Fe(Al、Zn)2及び前記Fe2(Al、Zn)5のうち0~50面積%が、Fe(Al、Si)に置換されていてもよい。
以下に、本実施形態に係るホットスタンプ成形体について説明する。本実施形態に係るホットスタンプ成形体1は、図7に示されるように、母材10とめっき層20とを含む。
以下に、本実施形態に係るホットスタンプ成形体の母材の、好ましい成分を説明する。本実施形態に係るホットスタンプ成形体の課題である、耐LME性及びりん酸塩処理性の改善は、めっき層の構成によって実現される。従って、本実施形態に係るホットスタンプ成形体の母材は特に限定されない。しかし、母材の成分が以下に説明する範囲内である場合、耐LME性及びりん酸塩処理性に加えて、好適な機械特性を有する成形体が得られる。以下、母材に含まれる合金元素の含有量の単位「%」は、「質量%」を意味する。
0.05%以上の炭素(C)が母材に含まれる場合、ホットスタンプ成形体の強度が高められる。一方、母材のC含有量が0.40%超である場合、成形体の母材の靭性が不足する場合がある。従って、母材のC含有量を、0.05~0.40%としてもよい。母材のC含有量のさらに好ましい下限値は0.10%であり、より一層好ましい下限値は0.13%である。母材のC含有量のさらに好ましい上限値は0.35%である。
シリコン(Si)は鋼を脱酸する効果を有する。しかしながら、Si含有量が多くなるとめっきに対する鋼材の濡れ性が低下し、正常にめっき処理できない可能性がある。従って、母材のSi含有量を0.5%以下としてもよい。さらに好ましい母材のSi含有量の上限値は0.3%であり、より一層好ましい母材のSi含有量の上限値は0.2%である。母材のSi含有量のさらに好ましい下限値は、求められる脱酸レベルに応じて定めることができ、例えば0.05%である。
0.5%を超えるマンガン(Mn)が母材に含まれる場合、ホットスタンプ前の鋼材の母材の焼入れ性が高められ、ホットスタンプ後の成形体の母材の強度が高められる。一方、母材のMn含有量を2.5%超とした場合、この効果は飽和する。従って、母材のMn含有量を0.5~2.5%としてもよい。母材のMn含有量のさらに好ましい下限値は0.6%であり、より一層好ましい下限値は0.7%である。母材のMn含有量のさらに好ましい上限値は2.4%であり、より一層好ましい下限値は2.3%である。
りん(P)は鋼中に含まれる不純物である。母材に含まれるPは、母材の結晶粒界に偏析して成形体の母材の靭性を低下させ、母材の耐遅れ破壊性を低下させる場合がある。従って、母材のP含有量を0.03%以下にしてもよい。母材のP含有量はできる限り少なくすることが好ましい。
硫黄(S)は鋼中に含まれる不純物である。母材に含まれるSは硫化物を形成して成形体の母材の靭性を低下させ、母材の耐遅れ破壊性を低下させる場合がある。従って、母材のS含有量は0.01%以下にしてもよい。母材のS含有量はできる限り少なくすることが好ましい。
用語「Al含有量」が本実施形態に係る成形体の母材に関して用いられる場合、この用語は母材中のsol.Al(酸可溶Al)の含有量を意味する。アルミニウム(Al)は一般に鋼の脱酸目的で使用される。しかしながら、Al含有量が多い場合、ホットスタンプ前の鋼材のAc3点が上昇し、ホットスタンプの際に鋼の焼入れに必要な加熱温度が上昇するので、ホットスタンプ製造上は望ましくない。従って、母材のAl含有量は0.10%以下としてもよい。母材のAl含有量のさらに好ましい上限値は0.05%である。母材のAl含有量のさらに好ましい下限値は0.01%である。
窒素(N)は鋼中に含まれる不純物である。母材に含まれるNは、窒化物を形成して成形体の母材の靭性を低下させる場合がある。さらに、母材に含まれるNは、ホットスタンプ前の鋼材の焼入れ性を向上させるために母材中にBが含有される場合、Bと結合して固溶B量を減らし、Bの焼入れ性向上効果を低下させる場合がある。従って、母材のN含有量を0.01%以下としてもよい。母材のN含有量はできる限り少なくすることが好ましい。
Bは、鋼の焼入れ性を高める働きを有するので、ホットスタンプ後の成形体の母材の強度を高める。しかしながら、母材のB含有量が多過ぎれば、この効果は飽和する。従って、母材のB含有量を、0~0.0050%としてもよい。母材のB含有量のさらに好ましい下限値は0.0001%である。
母材に含まれるTiは、母材に含まれるNと結合して窒化物を形成する。このようにTiとNとが結合する場合には、母材のBと母材のNとの結合が抑制され、BN形成による母材の焼入れ性の低下を抑制することができる。さらに、母材に含まれるTiは、そのピン止め効果により、ホットスタンプにおける加熱の際にオーステナイト粒径を微細化し、それにより成形体の靱性等を高める効果も有する。しかしながら、母材のTi含有量が多過ぎれば上記効果が飽和し、さらに、Ti窒化物が過剰に析出して成形体の母材の靭性が低下するおそれがある。従って、母材のTi含有量を0~0.10%としてもよい。母材のTi含有量の好ましい下限値は0.01%である。
母材に含まれるCrは、ホットスタンプ前の鋼材の母材の焼入れ性を高める。しかしながら、母材のCr含有量が多過ぎれば、Cr炭化物が形成される。このCr炭化物は、ホットスタンプの加熱時に溶解し難く、オーステナイト化の進行を妨げ、焼き入れ性を低下させる場合がある。従って、母材のCr含有量を0~0.5%としてもよい。母材のCr含有量のさらに好ましい下限値は0.1%である。
母材に含まれるMoは、ホットスタンプ前の鋼材の母材の焼入れ性を高める。しかしながら、母材のMo含有量が多過ぎれば、上記効果は飽和する。従って、母材のMo含有量を0~0.50%としてもよい。母材のMo含有量のさらに好ましい下限値は0.05%である。
母材に含まれるNbは、炭化物を形成して、ホットスタンプ時に母材の結晶粒を微細化し、成形体の靭性を高める。しかしながら、母材のNb含有量が多過ぎれば、上記効果は飽和する。さらに、母材のNb含有量が多過ぎれば、母材の焼入れ性が低下する場合がある。従って、Nb含有量を0~0.10%としてもよい。母材のNb含有量のさらに好ましい下限値は0.02%である。
母材に含まれるNiは、成形体の母材の靭性を高める。母材のNiは、さらに、ホットスタンプでの加熱時に、溶融Znの存在に起因した脆化を抑制する。しかしながら、母材のNi含有量が多過ぎれば、これらの効果は飽和する。従って、母材のNi含有量を0~1.0%としてもよい。母材のNi含有量のさらに好ましい下限値は0.1%である。
次に、本実施形態に係るホットスタンプ成形体1のめっき層20について説明する。成形体1のめっき層20は、図7に示されるように、成形体1の母材10側から成形体1の表面側に向かって、界面層21と、中間層22と、酸化物層23と、を順次含む。
界面層は、母材に隣接して形成される。界面層の組織の大半は、αFe、Fe3Al、及びFeAlから構成される。すなわち、本実施形態に係るホットスタンプ成形体の界面層は、主にAl含有量が少ないFe-Al合金相から構成される。なお、めっき形成中に混入した不純物に起因する介在物などが、界面層にわずかに含まれる場合もある。しかし発明者らは、ホットスタンプ成形体のめっき層の断面で界面層を観察した場合に、組織が合計99面積%以上のαFe、Fe3Al、及びFeAlを含んでいれば、上述のような介在物の影響は無視できる旨を確認した。界面層の組織を上述の如く制御するためには、界面層の平均Al含有量を8.0質量%以上32.5質量%以下とする必要がある。なお、後述するように界面層中のAl含有量は一様ではなく、母材に近づくに連れて界面層のAl含有量は低下する。
中間層22は、Fe、Al、及びZnを含む層であり、界面層21の上に形成される。中間層の組織の大半は、Fe(Al、Zn)2及びFe2(Al、Zn)5から構成される。Fe(Al、Zn)2とは、Fe-Al金属間化合物の1種であるFeAl2におけるAlの一部が、Znと置換されている相であり、Fe2(Al、Zn)5とは、Fe-Al金属間化合物の1種であるFe2Al5におけるAlの一部が、Znと置換されている相である。なお、めっき形成中に混入した不純物に起因する介在物などが、中間層にわずかに含まれる場合もある。しかし発明者らは、ホットスタンプ成形体のめっき層の断面で中間層を観察した場合に、組織が合計99面積%以上のFe(Al、Zn)2及びFe2(Al、Zn)5を含んでいれば、上述のような介在物の影響は無視できる旨を確認した。
さらに、中間層の成形体表面側には、成形体の最表層として、Zn酸化物を主成分とする酸化物層23が形成されている。酸化物層23は、ホットスタンプ成形体を製造する際の加熱過程で、ホットスタンプ用めっき鋼材のめっきが酸化されて生成したものである。この酸化物層が、ホットスタンプ成形体のりん酸塩処理性を向上させる。りん酸塩処理性および塗膜密着性の向上効果を得るためには、酸化物層の平均膜厚を0.1μm以上とする必要がある。但し、酸化物層が厚過ぎると、成形体の耐食性及び溶接性等に悪影響を及ぼすので、酸化物層の平均膜厚は3.0μm以下とする。なお、酸化物層の平均膜厚を2.0μm以下とした場合には、成形体の耐食性や溶接性等の性能が高いレベルで発揮されるため、好ましい。
界面層のAl含有量は、成形体を表面に垂直に切断し、断面を研磨し、この断面において界面層を包含する領域におけるAl含有量分布をEPMA等の解析装置で分析することにより得られる。界面層の平均Zn含有量、中間層の平均Al含有量及び平均Zn含有量、並びにめっき層の平均Si含有量は、上述の方法で得られる濃度分布に基づいて得られる。
界面層及び中間層の金属組織は、TEM等による結晶構造解析により得られる。
界面層、中間層、及び酸化物層の厚さは、上述の断面の拡大写真を電子顕微鏡で撮影し、この拡大写真を画像解析することにより得られる。
なお、本実施形態に係る成形体のめっき層の構成は、成形体の表面に平行な方向に沿って実質的に一様ではない。特に、界面層、中間層、及び酸化物層の厚さは、加工された領域と加工されていない領域とで異なることが多い。従って、上述された分析は、成形体の加工されていない領域において実施されなければならない。加工されていない領域におけるめっき層の状態が上述の範囲内である成形体は、本実施形態に係る成形体であるとみなされる。
次に、本実施形態に係るホットスタンプ成形体の製造方法について説明する。本実施形態のホットスタンプ成形体の製造方法は、ホットスタンプ用めっき鋼材を製造する工程と、ホットスタンプ用めっき鋼材にホットスタンプする工程とを含む。ホットスタンプ用めっき鋼材を製造する工程は、ホットスタンプ用めっき鋼材の母材を製造する工程と、ホットスタンプ用めっき鋼材の母材にAl-Znめっき層を形成する工程とを含む。本実施形態に係るホットスタンプ成形体の製造方法は、必要に応じて、防錆油膜形成工程及びブランキング加工工程を含む。以下、各工程を詳述する。
ホットスタンプ成形体の材料であるめっき鋼材は、母材と、めっき層とを備える。母材製造工程では、ホットスタンプ用めっき鋼材の母材を製造する。例えば、上に例示された本実施形態に係るホットスタンプ成形体の母材の化学組成と同じ化学組成を有する溶鋼を製造し、この溶鋼を用いて、鋳造法によりスラブを製造する。または、上述の通り製造された溶鋼を用いて、造塊法によりインゴットを製造してもよい。次いで、スラブ又はインゴットを熱間圧延することにより、ホットスタンプ用めっき鋼材の母材(熱延板)が得られる。なお、必要に応じて、上記熱延板に対して酸洗処理を行い、酸洗処理後の熱延板に対して冷間圧延を行って得られる冷延板をホットスタンプ用めっき鋼材の母材としてもよい。
めっき処理工程では、上記ホットスタンプ用めっき鋼材の母材にAl-Znめっき層を形成して、ホットスタンプ用めっき鋼材を製造する。
ホットスタンプ工程では、上述のホットスタンプ用めっき鋼材にホットスタンプを行う。通常のホットスタンプは、鋼材をホットスタンプ温度範囲(熱間加工温度範囲)まで加熱し、次いで鋼材を熱間加工し、さらに鋼材を冷却することにより行われる。通常のホットスタンプ技術によれば、製造時間を短縮するために、鋼材の加熱速度をなるべく大きくすることが良いとされる。また、鋼材をホットスタンプ温度範囲まで加熱すればめっき層の合金化が十分に進むので、通常のホットスタンプ技術は、鋼材の加熱条件の制御を重要視していない。しかしながら、本実施形態に係るホットスタンプ部材を製造するためのホットスタンプ工程では(1)ホットスタンプ用めっき鋼材を合金化温度範囲まで加熱し、(2)ホットスタンプ用めっき鋼材の温度を合金化温度範囲で保持し、(3)ホットスタンプ用めっき鋼材をホットスタンプ温度範囲まで加熱し、(4)ホットスタンプ用めっき鋼材を熱間加工及び冷却する。本発明者らは、ホットスタンプ用めっき鋼材をホットスタンプ温度範囲まで昇温させる際に、合金化温度範囲内で鋼材の昇温を略停止させ、その後昇温を再開することが、上述された構成を有するめっき層を得るために必須であることを見いだした。
防錆油膜形成工程は、めっき処理工程後、かつ、ホットスタンプ工程前に、ホットスタンプ用めっき鋼材の表面に防錆油を塗布して防錆油膜を形成するものであり、製造方法に任意に含まれても良い。ホットスタンプ用めっき鋼材が製造されてからホットスタンプが行われるまでの時間が長い場合には、ホットスタンプ用めっき鋼材の表面が酸化するおそれがある。しかしながら、防錆油膜形成工程により防錆油膜が形成されたホットスタンプ用めっき鋼材の表面は酸化し難いので、防錆油膜形成工程は、成形体のスケールの形成を抑制することができる。なお、防錆油膜の形成方法は、公知のいかなる技術を用いることもできる。
本工程は、防錆油膜形成工程後、かつ、ホットスタンプ工程前に、ホットスタンプ用めっき鋼材に対して剪断加工及び/又は打ち抜き加工を行って、当該鋼材を特定の形状に成形する工程である。ブランキング加工後の鋼材の剪断面は酸化し易い。しかしながら、鋼材表面に事前に防錆油膜が形成されていれば、上記剪断面にも防錆油がある程度広がる。これにより、ブランキング加工後の鋼材の酸化を抑制することができる。
塗膜剥離率=(A2/A1)×100
A1は試験領域の面積(60mm×120mm=7200mm2)であり、A2は塗膜が剥離した領域の面積(mm2)である。塗膜剥離率が5.0%未満の試料を、塗膜密着性について良好(GOOD)と評価した。一方、塗膜剥離率が5.0%以上の試料を、塗膜密着性について不良(BAD)と評価した。
表3に示すように、めっき層の合金形態及び組成についての改良、並びに、めっき層の最表層として形成される酸化物の膜厚についての改良を行っている、発明例のホットスタンプ成形体については、いずれも、LME発生の抑制に基づく成形体の疲労特性改善と、成形体のりん酸塩処理性の改善との両方が達成されていることが判る。
比較例102は、Zn含有量が不足しためっき浴を用いて製造されたので、中間層の組織がZn不足に起因して不適切となった。このため、比較例102ではリン酸塩処理性が損なわれ、塗膜密着性が不良であった。
比較例103は、ホットスタンプの際の合金化温度が高すぎたので、酸化物層の膜厚が過剰となり、溶接性が不良であった。
比較例104は、ホットスタンプの際の合金化温度が低すぎたので、めっき層の合金化が不十分となり、Znリッチ相が生じ、LMEを防止することができなかった。このため、比較例104の疲労特性は不良であった。
比較例105は、ホットスタンプの際の合金化時間が長すぎたので、酸化物層の膜厚が過剰となり、溶接性が不良であった。
比較例106は、ホットスタンプの際の合金化時間が短すぎたので、合金化のための加熱が不十分となった。このため、比較例106ではLMEが発生し、疲労特性が低下した。さらに、比較例106では、加熱が不十分であるので酸化物量が少なく、リン酸塩処理性及び塗膜密着性が不足した。
比較例107は、合金化温度およびホットスタンプの際の保持時間が過剰であったので、酸化物層の膜厚が過剰となり、溶接性が不良であった。
10 母材
20 めっき層
21 界面層
22 中間層
23 酸化物層
30 Al-Zn系めっき層
40 Zn系めっき層
50 Al系めっき層
60 化成結晶
70 透け領域
Claims (4)
- 母材と;
めっき層と;
を備えるホットスタンプ成形体であって、
前記めっき層は、前記母材側から表面側に向かって順に、界面層と、中間層と、酸化物層と、を含み、
前記界面層は、組織が合計99面積%以上のαFe、Fe3Al、及びFeAlを含み、平均Al含有量が、前記8.0質量%以上32.5質量%以下の範囲内であり、平均Zn含有量が前記母材のZn含有量超5質量%以下に制限され、化学成分の残部はFe及び不純物を含み、並びに平均膜厚が1.0μm以上であり、
前記中間層は、組織が合計99面積%以上のFe(Al、Zn)2及びFe2(Al、Zn)5を含み、平均Al含有量が30~50質量%であり、平均Zn含有量が10~40質量%であり、化学成分の残部はFe及び不純物を含み、並びに平均膜厚が5.0μm以上であり、
前記酸化物層は、平均膜厚が0.1~3.0μmである
ことを特徴とするホットスタンプ成形体。 - 前記界面層は、平均膜厚が1.0~10.0μmである
ことを特徴する請求項1に記載のホットスタンプ成形体。 - 前記めっき層中のAl及びZnの単位面積当たりの合計重量が20g/m2以上100g/m2以下である
ことを特徴とする請求項1又は2に記載のホットスタンプ成形体。 - 前記めっき層は、平均0質量%超10.0質量%以下のSiをさらに含み、
前記中間層において、前記Fe(Al、Zn)2及び前記Fe2(Al、Zn)5のうち0~50面積%が、Fe(Al、Si)に置換されている
ことを特徴とする請求項1から3のいずれか1項に記載のホットスタンプ成形体。
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WO2023074114A1 (ja) * | 2021-10-29 | 2023-05-04 | Jfeスチール株式会社 | 熱間プレス部材 |
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RU2710813C1 (ru) | 2020-01-14 |
CN109072396A (zh) | 2018-12-21 |
EP3456854A4 (en) | 2019-10-02 |
CA3020663C (en) | 2020-06-02 |
CA3020663A1 (en) | 2017-11-16 |
US20190160507A1 (en) | 2019-05-30 |
EP3456854A1 (en) | 2019-03-20 |
KR20180131589A (ko) | 2018-12-10 |
BR112018071451A2 (pt) | 2019-02-05 |
JP6566128B2 (ja) | 2019-08-28 |
JPWO2017195269A1 (ja) | 2019-01-24 |
MX2018013464A (es) | 2019-02-28 |
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