WO2017057453A1 - 熱間鍛造用金型及びそれを用いた鍛造製品の製造方法並びに熱間鍛造用金型の製造方法 - Google Patents
熱間鍛造用金型及びそれを用いた鍛造製品の製造方法並びに熱間鍛造用金型の製造方法 Download PDFInfo
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- WO2017057453A1 WO2017057453A1 PCT/JP2016/078611 JP2016078611W WO2017057453A1 WO 2017057453 A1 WO2017057453 A1 WO 2017057453A1 JP 2016078611 W JP2016078611 W JP 2016078611W WO 2017057453 A1 WO2017057453 A1 WO 2017057453A1
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- forging die
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J13/00—Details of machines for forging, pressing, or hammering
- B21J13/02—Dies or mountings therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
Definitions
- the present invention relates to a hot forging die having excellent oxidation resistance, a method for producing a forged product using the same, and a method for producing a hot forging die.
- the forging material is heated to reduce deformation resistance.
- heat-resistant alloys have high strength even at high temperatures
- hot forging dies used for forging require high mechanical strength at high temperatures.
- the workability of the forging material is reduced due to heat removal.
- a product made of a difficult-to-work material such as Alloy 718 or Ti alloy Forging is performed by heating a hot forging die together with the material. Therefore, the hot forging die must have a high mechanical strength at a high temperature similar to or close to that of the forging material.
- the hot forging referred to in the present invention includes hot die forging in which the temperature of the hot forging die is brought close to the temperature of the forging material and isothermal forging in which the temperature is the same as that of the forging material.
- JP 62-50429 A Japanese Examined Patent Publication No. 63-21737 U.S. Pat. No. 4,740,354
- the Ni-based superalloy described above is advantageous in that it has a high high temperature compressive strength, but in terms of oxidation resistance, a fine scale of nickel oxide scatters from the mold surface during cooling after heating in the atmosphere. Therefore, there is a problem that there is a risk of deterioration of the working environment and shape.
- the problem of oxidation of the mold surface and the accompanying scattering of the scale is a big problem in maximizing the effect that it can be used in the atmosphere.
- the object of the present invention is to solve the problem of deterioration of working environment and shape deterioration by preventing the above-mentioned Ni-base super heat-resistant alloy mold surface from being oxidized, and further suppresses deterioration of oxidation resistance due to repeated use.
- To provide a hot forging die a method for producing a forged product using the same, and a method for producing a hot forging die.
- the present inventor has studied the problems of the oxidation of the mold surface and the accompanying scale scattering, and found that these problems can be greatly improved by adopting the coating of the inorganic material on the mold surface, and has reached the present invention. That is, the present invention is, in mass%, W: 10.3-11.0%, Mo: 9.0-11.0%, Al: 5.8-6.8%, and the balance is Ni and It has a base material composition made of a Ni-based superalloy that is an inevitable impurity, and has a coating layer of an inorganic material on at least one of a molding surface and a side surface. , A hot forging die containing a total of 30% by mass or more of one or more of Al.
- the hot forging die preferably has an inorganic material coating layer on the entire surface.
- a coating layer consists of any one or more of nitride, an oxide, and carbide.
- a coating layer contains a nitride at least and 50% or more of the elements other than nitrogen constituting the nitride is Cr.
- a coating layer contains an oxide at least and 50% or more of the elements other than oxygen of the oxide is 50% by mass or more.
- a coating layer contains a carbide
- a coating layer is a mixed phase of a carbide and an oxide, and 30% or more by mass is Si among elements other than carbon and oxygen constituting the mixed phase of the carbide and the oxide. Is preferred.
- the coating layer has a laminated structure of two or more layers having different compositions. More preferably, it is a hot forging die having an Al oxide layer between the surface of the hot forging substrate and the coating layer.
- the present invention also relates to a method for producing a forged product in which a heated forging material is hot forged with an upper die and a lower die, wherein the forged product uses the hot forging die as the upper die and the lower die. It is a manufacturing method.
- the present invention relates to a method for producing a hot forging die using a Ni-based superalloy as a base material, wherein the mass is W: 10.3 to 11.0%, Mo: 9.0 to 11.0. %, Al: 5.8 to 6.8%, with the balance being Ni and at least one of the side surface and the side surface of the base material made of a Ni-based superalloy containing inevitable impurities, nitride, oxide
- the hot forging mold according to the above, wherein an Al concentrated oxide layer is formed between the surface of the base material and the coating layer by heating the base material on which the inorganic material is disposed. It is a manufacturing method.
- the hot forging die of the present invention has an effect of preventing oxidation of the die surface and the accompanying scattering of the scale due to its excellent oxidation resistance, and also suppresses a decrease in the effect even in repeated use. It is possible to produce an effect of suppressing deterioration of working environment and shape deterioration in hot forging in the atmosphere using this.
- the Ni-base superalloy having the following alloy composition defined in the present invention has a high-temperature compressive strength superior to other mold materials for hot forging, and heat such as isothermal forging and hot die forging in the atmosphere. Inter-forging can be performed.
- the unit is mass%.
- W forms a solid solution in the austenite matrix and also forms a solid solution in the gamma prime phase based on Ni 3 Al as a precipitation strengthening phase, thereby increasing the high temperature strength of the alloy.
- W crystallizes a body-centered cubic ⁇ - (Mo, W) phase consisting of a solid solution of W and Mo at the grain boundary to increase the grain boundary strength of the alloy and at the same time enhance the machinability of the alloy.
- W also has an effect of lowering the oxidation resistance, and if it is added in excess of 11.0%, cracking is likely to occur.
- the content of W in the Ni-base superalloy in the present invention is 10.3 to 11.0%.
- the preferable lower limit for obtaining the effect of W more reliably is 10.4%
- the preferable upper limit of W is 10.7%.
- Mo dissolves in the austenite matrix and also dissolves in the gamma prime phase based on Ni 3 Al, which is a precipitation strengthening phase, to increase the high temperature strength of the alloy.
- Mo has the effect
- the Mo content in the Ni-base superalloy according to the present invention is set to 9.0 to 11.0%.
- a preferable lower limit for obtaining the effect of Mo more reliably is 9.5%, and more preferably 9.8%.
- the upper limit of preferable Mo is 10.5%, More preferably, it is 10.2%.
- Al binds to Ni and precipitates a gamma prime phase composed of Ni 3 Al, thereby increasing the high temperature strength of the alloy, generating an alumina coating on the surface of the alloy, and imparting oxidation resistance to the alloy.
- the Al content in the Ni-base superalloy according to the present invention is set to 5.8 to 6.8% by mass.
- a preferable lower limit for obtaining the effect of Al more surely is 6.0%, and more preferably 6.1%.
- the upper limit of preferable Al is 6.6%, More preferably, it is 6.4%.
- the alloy is basically composed of Al, W, and Mo, which are essential components, and Ni with the remainder excluding inevitable impurities.
- Ni is a main element constituting a gamma phase and constitutes a gamma prime phase together with Al, Mo and W.
- the Ni-base superalloy according to the present invention can contain components other than Ni, Mo, W, and Al as inevitable impurities.
- an inorganic material coating layer is formed on a base material of a hot forging die having the above alloy composition.
- the purpose of forming a coating layer of an inorganic material on a hot forging die having the above alloy composition is to prevent peeling of the scale. Covering the surface of the mold for hot forging with a dense protective coating (coating layer) prevents direct contact between atmospheric oxygen and the mold base material at high temperatures, preventing oxidation of the mold surface. To do. Therefore, in the present invention, the inorganic material is coated in layers to form a coating layer of the inorganic material, thereby preventing the hot forging die from being oxidized.
- the said coating layer shall contain 30 mass% or more in total of 1 or more types of Si, Cr, and Al among Si and a metal element. This is because a coating layer of an inorganic material containing at least 30% by mass of one or more of these elements is particularly effective in preventing oxidation of the mold surface.
- the coating layer of the inorganic material referred to in the present invention is an oxide film that is naturally formed on the outermost surface of a hot forging die during heating before hot forging or during hot forging, such as a self-oxidizing film. Rather, it is formed by coating, spraying, vapor deposition, or the like.
- the coating layer contains at least 30% by mass of Si, Cr, and Al among Si and metal elements in total” means other than the self-oxidation film that is naturally formed during the hot forging process. It stipulates that As a method for coating an inorganic material, for example, in vapor deposition, a physical vapor deposition method (PVD method) can form a dense and uniform inorganic material, and is particularly suitable for forming a coating layer having a multilayer structure. Further, application and spraying are advantageous in terms of cost, and may be used when a single coating layer is formed.
- PVD method physical vapor deposition method
- the “inorganic material coating layer” referred to in the present invention does not include an oxide film of the alloy component, and an oxide layer, nitride layer, or carbide having a composition different from that of the alloy component. It is a single layer composed of one kind such as an oxide layer containing bismuth, or a composite layer composed of two or more kinds. Note that the oxide layer serving as the inorganic material does not include so-called glass lubrication.
- the “inorganic material coating layer” of the present invention does not include a glass lubricant whose effect is substantially impaired by one hot forging.
- the reason why the coating layer of the inorganic material is formed on either or both of the molding surface and the side surface in the present invention is that these two surfaces are usually exposed to a high-temperature atmosphere.
- an inorganic material coating layer is formed on either or both of the molding surface and the side surface.
- an inorganic material coating layer is formed on both the molding surface and the side surface. Good to do.
- the “molding surface” in the present invention refers to a surface that presses the forged material in order to hot forge the material to be forged.
- the surface shape may be flat like a so-called anvil.
- a mold-sculpted surface may be formed.
- a coating layer of an inorganic material on all surfaces (molding surface, side surface, bottom surface) of the hot forging die.
- the inorganic material coating layer is made of at least one of nitride, oxide, and carbide. This is because a dense oxygen barrier film is formed by a nitride, oxide, or carbide coating layer to prevent oxidation of the mold base material. And in this invention, a coating layer is formed with these inorganic materials, and peeling of a scale is prevented.
- the covering layer may be a single layer of any one of nitride, oxide, and carbide, or may have a laminated structure in which any two or more of nitride, oxide, and carbide are combined. Similar effects can be obtained even with a mixed phase of carbide and oxide.
- a coating layer is formed by selecting a range from a plurality of surfaces or a certain surface, it is better to form a separate coating layer for each surface or each selected range in terms of film formation cost, characteristics, and workability. This can be advantageous, and can be selected in consideration of the effect of preventing scale peeling and the cost.
- a coating layer in which 50% or more by mass of Si is an element other than oxygen is preferable, and in the case of a carbide coating layer, 50% or more by mass% of elements other than carbon.
- a coating layer in which is Si is preferred.
- a coating layer in which 30% or more by mass of Si other than carbon and oxygen is Si is preferable.
- the coating layer may have a multilayer structure of two or more coating layers having different compositions.
- a nitride layer having two or more layers having a different composition is used, characteristics such as oxidation resistance, adhesion, and life can be improved by a combination of coating layers having different compositions.
- an Al oxide layer is provided between the surface of the substrate and the coating layer.
- This Al oxide layer is a self-oxidized coating of Al contained in a base material (base material) for a hot forging die.
- base material base material
- a phenomenon may occur in which the coating layer or the coating layer and the base material are corroded by the glass lubricant.
- the self-oxidation film functions as a barrier layer that prevents the progress of corrosion by the glass lubricant.
- the self-oxidized film can be formed by performing a preliminary oxidation treatment after forming a coating layer of an inorganic material on the surface of the base material.
- the Al self-oxidation film can be formed, for example, by performing preliminary oxidation at 900 to 1100 ° C. for 3 to 5 hours.
- the thickness of the coating layer is preferably 2 to 200 ⁇ m per layer.
- the thickness of the coating layer suitable for fully exhibiting the characteristics of the coating layer is preferably 2 to 200 ⁇ m per layer. If the thickness per layer is excessively thin, the effect of forming the coating layer may be poor. Moreover, it is because there exists a possibility that an effect may be saturated or cost may rise even if the thickness of a coating layer is increased too much.
- Example 1 The following examples further illustrate the present invention. Ingots of Ni-base superalloys shown in Table 1 were produced by vacuum melting. In addition, the alloy which has a composition shown in Table 1 has the characteristic of the outstanding high temperature compressive strength as shown in Table 2, and has a characteristic sufficient as a metal mold
- a disc-shaped test piece having a diameter of 50 mm and a height of 10 mm is cut out from the above ingot, and one of the circular surfaces of the test piece is polished to No. 500, and an inorganic material coating layer is formed on the polished surface.
- a test piece was prepared. Using this test piece, the effect of preventing the oxidation of the mold surface and the scattering of the scale due to the formation of the coating layer was evaluated. The test piece produced this time simulates the surface of a hot forging die that is not subjected to stress. The coating layer was formed only on one side of the circular surface. Table 3 summarizes the composition of the coating layer, the layer structure, and the thickness per layer. No. No.
- No. 1 is a test piece using CrN and AlCrSiN and having three coating layers of a CrN layer, an AlCrSiN layer, and a CrN layer
- No. 1 2 is No.2.
- No. 1 is a test piece having five coating layers in which an AlCrSiN layer and a CrN layer are further stacked.
- No. 3 is a test piece having a coating layer in which two layers made of AlCrSiN are laminated
- No. 3 4 is a test piece having two coating layers composed of TiAlN and AlCrSiN, and these formed a film by the PVD method.
- No. 5 is a test piece having a coating layer composed of 25 to 27% by mass of colloidal silica and 73 to 75% by mass of SiC
- No. 5 6 is a test piece having a coating layer made of ceramics having the composition shown in Table 4, and these formed a coating by coating.
- No. No. 5 is water, no.
- the paint of No. 6 contains organic substances such as ethanol, but these are in a temperature range of 900 to 1100 ° C. where deterioration of the working environment and shape defects caused by oxidation of the Ni-base superalloy shown in Table 1 are problematic. It is not present in the film due to evaporation or the like.
- the left side is the base material side (Ni-base superheat-resistant alloy side) and the right end is the outermost surface side.
- film thickness per layer is the same film thickness when a plurality of coating layers having the same composition are formed, and the film thickness per layer is described.
- EDX energy dispersive X-ray analyzer
- the coating layer of the test piece contained at least 30% by mass of one or more of Si, Cr, and Al among Si and metal elements. . No. In the test pieces 5 to 6, it was confirmed by quantitative analysis by EDX that Si alone or the total amount of Si and Al was 30% by mass or more.
- 3G shows a photograph after the 10th heating test of the comparative material.
- the surface oxidation and the accompanying scattering of the scale were similarly observed from the 1st to the 10th time. From these results, no. 1-No. 4 and no.
- FIG. 6 it can be seen that the antioxidant effect is not reduced by peeling of the coating layer from the 1st to the 10th time. No. In FIG. 5, although peeling of the coating layer was observed, oxidation was prevented for the remaining region of the coating layer in the first to third heating tests. This is the case with, for example, no.
- the coating layer 5 can be sufficiently oxidized-resistant by reapplying it about 2 to 3 times.
- the cost of coating the inorganic material is no. 1-No. No. 4 compared with the PVD method. 5 and no.
- Application of the inorganic material 6 is inexpensive.
- No. The coating layer of No. 5 was completely peeled off at the fourth time. Since the coating layer of No. 6 does not peel off even if it is repeated 10 times, no recoating is required. 6 is No.6. Compared to 5, it is advantageous in terms of workability. Therefore, no. Application of 6 coating layers is preferred.
- FE-EPMA reflected electron image observed from the cross-sectional direction after resin coating and mirror polishing of the coating layer and base material after the 10th heating test of No. 6, (b) Al element map, (c) O element map Indicates.
- the shading in the element map image corresponds to the concentration of the element to be measured, and the whiter the concentration is. From these figures, it can be seen that Al and O are concentrated on the surface of the base material on the coating layer side, and an Al oxide layer is formed here.
- This Al oxide layer is No. It is formed during holding for 3 hours at 1100 ° C. after applying the ceramic paint of No. 6. No. 1 in a heating test held at 1100 ° C. for 3 hours and 10 repeated heating tests.
- the excellent oxidation resistance exhibited by the test piece No. 6 is No. 6. 6 is derived from the Al oxide layer formed on the surface of the base material on the coating layer side by the formation and heating of the coating layer 6.
- Example 2 When forging a forged material coated with a glass lubricant using a hot forging die with a coating layer formed, a phenomenon may occur in which the coating layer or the coating layer and the base material are corroded by the glass lubricant. is there.
- three test pieces were prepared in which 400 to 500 mg of glass lubricant was applied in the vicinity of the center on the sample processed in the same manner as the comparative material.
- the prepared test piece was put into a heated furnace, held for 3 hours, and then taken out from the furnace and air-cooled, and a heating test was performed once for 900, 1000, and 1100 ° C., which are temperatures assumed in an actual machine. .
- the atmosphere in the heating test is air, and all the atmospheres in the tests after this test are also air.
- Table 5 shows the composition of the glass lubricant used. Moreover, it confirmed that the total amount of Si and Al was 30 mass% or more by the quantitative analysis by EDX.
- FIG. 5 (a) shows a photograph of the sample before the 900 ° C heating test and Fig. 5 (d) shows the sample after the 900 ° C heating test.
- FIG. 5 (b) shows a photograph of the sample before the 1000 ° C. heat test, (e) after the 1000 ° C. heat test, (c) before the 1100 ° C. heat test, and (f) after the 1100 ° C. heat test. It can be seen that the base metal is corroded by the glass lubricant at 900, 1000 and 1100 ° C., and the reaction becomes more intense as the temperature rises.
- test piece prepared in the same manner as the test piece No. 6 was pre-oxidized in order to improve the Al self-oxidation film, and then 400 to 500 mg of glass lubricant was applied near the center of the test piece on the coating layer.
- a test piece was prepared.
- This test piece is No. 6 is a simulation of a state in which the glass lubricant covered with the forged material remains on the mold after the coating layer 6 is formed and preheated.
- a heating test was performed once, which was put into a furnace heated to 1100 ° C. where corrosion due to glass lubrication was most intense, held at 1100 ° C. for 3 hours, and then taken out from the furnace and air-cooled. Table 6 shows the preliminary oxidation conditions of the test piece and the film thickness of the coating layer.
- FIG. No. 7 shows that corrosion of the coating layer and the base material by the glass lubricant is suppressed.
- FE-EPMA reflected electron image observed from the cross-sectional direction after embedding the pre-oxidized coating layer and base material in resin and mirror polishing, (b) Al element map, (c) O element map Indicates. From these figures, it can be seen that Al and O are concentrated on the surface of the base material on the coating layer side, and an Al oxide layer is formed between the base material and the coating layer by pre-oxidation. No. The suppression of corrosion of the coating layer and the base material by the glass lubricant indicated by the test piece 7 is derived from this Al oxide layer.
- the coating layer formed on the molding surface of the mold was sufficiently maintained even though a slight peeled portion was confirmed in the mold carved surface by the constant temperature forging. From this, No. It can be seen that the coating layer 6 prevents oxidation of the mold base material and the accompanying scattering of the scale on almost all of the molding surface and suppresses corrosion by the glass lubricant.
- the coating material of the inorganic material according to the present invention has a mass%, W: 10.3-11.0%, Mo: 9.0-11.0%, Al: 5.8-6
- the hot forging die made of Ni-based superalloy with the balance of 8% and Ni and inevitable impurities is higher in oxidation resistance than that without a coating layer, It is advantageous in that it can prevent oxidation and the scattering of the scale accompanying it, and the type of coating layer does not peel off the coating layer even if it is repeatedly heated and cooled, and the reduction in oxidation resistance is suppressed. I understand.
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Abstract
Description
また、熱間鍛造において熱間鍛造用金型の温度が鍛造素材に比べて低い場合、抜熱により鍛造素材の加工性が低下するため、例えばAlloy718やTi合金等の難加工性材からなる製品の鍛造は、素材とともに熱間鍛造用金型を加熱して行われる。従って、熱間鍛造用金型は、鍛造素材と同じかもしくはそれに近い高温で、高い機械的強度を有したものでなければならない。この要求を満たす熱間鍛造用金型として、大気中での金型温度1000℃以上の熱間鍛造に使用できるNi基超耐熱合金が提案されている(例えば、特許文献1~3参照)。
なお、本発明で言う熱間鍛造とは、熱間鍛造用金型の温度を鍛造素材の温度まで近づけるホットダイ鍛造と、鍛造素材と同じ温度にする恒温鍛造を含むものである。
本発明の目的は、上述したNi基超耐熱合金の金型表面の酸化を防止することで作業環境の劣化及び形状劣化の問題を解決し、更に繰り返しの使用による耐酸化性の低下を抑制した熱間鍛造用金型及びそれを用いた鍛造製品の製造方法並びに熱間鍛造用金型の製造方法を提供することである。
すなわち本発明は、質量%で、W:10.3~11.0%、Mo:9.0~11.0%、Al:5.8~6.8%であり、且つ、残部がNi及び不可避的不純物であるNi基超耐熱合金からなる基材組成を有し、成形面、側面の少なくとも一方に無機材料の被覆層を有し、前記被覆層がSi及び金属元素のうち、Si,Cr,Alの一種以上を合計で30質量%以上含む熱間鍛造用金型である。
また、熱間鍛造用金型は表面全面に無機材料の被覆層を有することが好ましい。
また、被覆層が窒化物、酸化物、炭化物の何れか1種類以上でなることが好ましい。
また、被覆層は少なくとも窒化物を含み、その窒化物を構成する窒素以外の元素のうち質量%で50%以上がCrであることが好ましい。
また、被覆層は少なくとも酸化物を含み、その酸化物の酸素以外の元素のうち質量%で50%以上がSiであることが好ましい。
また、被覆層は少なくとも炭化物を含み、その炭化物の炭素以外の元素のうち質量%で50%以上がSiであることが好ましい。
また、被覆層が炭化物と酸化物との混合相であることが好ましく、その炭化物と酸化物との混合相を構成する炭素と酸素以外の元素のうち質量%で30%以上がSiであることが好ましい。
また、被覆層が、それぞれ異なる組成を有する2層以上の積層構造であることが好ましい。
更に好ましくは、前記熱間鍛造の基材の表面と前記被覆層との間にAl酸化物層を有する熱間鍛造用金型である。
また本発明は、加熱された鍛造素材を上型および下型によって熱間鍛造する鍛造製品の製造方法であって、前記上型及び下型として、前記の熱間鍛造用金型を用いる鍛造製品の製造方法である。
また、基材としてNi基超耐熱合金を用いた熱間鍛造用金型の製造方法であって、質量%で、W:10.3~11.0%、Mo:9.0~11.0%、Al:5.8~6.8%であり、且つ、残部がNi及び不可避的不純物であるNi基超耐熱合金からなる基材の成形面、側面の少なくとも一方に、窒化物、酸化物、炭化物の何れか1種類以上でなる無機材料を配置して被覆層を形成する熱間鍛造用金型の製造方法である。
また、前記無機材料を配置した基材を加熱することによって前記基材の表面と前記被覆層の間にAl濃化酸化物層を形成することを特徴とする前記の熱間鍛造用金型の製造方法である。
Wは、オーステナイトマトリックスに固溶するとともに、析出強化相であるNi3Alを基本型とするガンマプライム相にも固溶して合金の高温強度を高める。また、Wは、粒界にWとMoの固溶体からなる体心立方晶のα-(Mo、W)相を晶出し、合金の粒界強度を高めると同時に、合金の被削性を高める作用がある。一方、Wは、耐酸化性を低下させる作用も有し、且つ、11.0%を超えて添加すると割れが発生し易くなる。高温強度を高め、耐酸化性の低下を抑制し、且つ、割れの発生をより抑制する観点から、本発明におけるNi基超耐熱合金中のWの含有量は10.3~11.0%とする。Wの効果をより確実に得るための好ましい下限は10.4%であり、好ましいWの上限は10.7%である。
Moは、オーステナイトマトリックスに固溶するとともに、析出強化相であるNi3Alを基本型とするガンマプライム相にも固溶して合金の高温強度を高める。一方、Moは、耐酸化性を低下させる作用を有する。高温強度を高め、且つ、耐酸化性の低下をより抑制する観点から、本発明におけるNi基超耐熱合金中のMoの含有量は9.0~11.0%とする。Moの効果をより確実に得るための好ましい下限は9.5%であり、更に好ましくは9.8%である。また、好ましいMoの上限は10.5%であり、更に好ましくは、10.2%である。
本発明におけるNi基超耐熱合金は、不可避的不純物として、Ni、Mo、W、Al以外の成分を含むことができる。
上記の合金組成を有する熱間鍛造用金型に無機材料の被覆層を形成する目的は、スケールの剥離を防止するものである。熱間鍛造用金型の表面を緻密な保護被膜(被覆層)で覆うことで高温での大気中の酸素と金型母材との直接的な接触を遮断させ、金型表面の酸化を防止するものである。そのため、本発明では、無機材料を層状に被覆して無機材料の被覆層とし、熱間鍛造用金型の酸化を防止する。
また、本発明においては、前記被覆層がSi及び金属元素のうち、Si,Cr,Alの一種以上を合計で30質量%以上含むものとする。これらの元素の1種以上を30質量%以上含む無機材料の被覆層は、特に金型表面の酸化を防止する効果が優れているからである。なお、本発明で言う無機材料の被覆層とは、自己酸化被膜のように、熱間鍛造前の加熱や熱間鍛造中に熱間鍛造用金型の最表面に自然に形成される酸化被膜ではなく、塗布、噴霧、蒸着等により形成されるものを言う。前記の「被覆層がSi及び金属元素のうち、Si,Cr,Alの一種以上を合計で30質量%以上含む」とは、熱間鍛造工程中に自然に形成される自己酸化被膜以外のものであることを規定するものである。
なお、無機材料の被覆方法として、例えば蒸着においては、物理蒸着法(PVD法)は緻密で均一な無機材料を形成させることができ、特に多層構造の被覆層の形成には好適である。また、塗布や噴霧は、コストの面で有利であり、単層の被覆層を形成する場合に用いれば良い。
また、前述のように、本発明で言う「無機材料の被覆層」には、前記の合金成分による酸化被膜は含まず、前記合金成分とは別組成の酸化物層、窒化物層、或いは炭化物を含む酸化物層、等の1種からなる単層、または2種以上からなる複合層である。なお、前記無機材料となる酸化物層には、所謂ガラス潤滑は含まない。ガラス潤滑剤のような、1回の熱間鍛造でその効果がほぼ損なわれるものは本発明の「無機材料の被覆層」には含まない。
本発明において、スケール剥離の効果を更に確実なものとするには、熱間鍛造用金型の全ての面(成形面、側面、底面)に無機材料の被覆層を形成することが好ましい。これにより、高温での大気中の酸素と金型の母材の接触による金型表面の酸化とそれに伴うスケール飛散をより確実に防止し、作業環境の劣化及び形状劣化を防止できる。
また、被覆層を複数面またはある一つの面の中で範囲を選択して形成させる場合、面または選択範囲毎に別の被覆層を形成させた方が、膜形成のコストや特性や作業性の点で有利な場合があり、スケール剥離防止の効果とコストとを勘案して選択することができる。
なお、上述した被覆層の中でも、窒化物は窒素以外の元素のうち質量%で50%以上がCrであるCr系の窒化物であるものを選択するのが好ましい。このCr系の窒化物は高温における耐酸化性が高いためである。酸化物の被覆層の場合は、酸素以外の元素のうち質量%で50%以上がSiである被覆層が好ましく、炭化物の被覆層の場合は、炭素以外の元素のうち質量%で50%以上がSiである被覆層が好ましい。炭化物と酸化物の混合相の場合は、炭素と酸素以外の元素のうち質量%で30%以上がSiである被覆層が好ましい。これらの被覆層もまた、高温における耐酸化性向上の効果を得ることができる。
更に好ましくは、前記基材の表面と前記被覆層との間にAl酸化物層を有することである。このAl酸化物層は、熱間鍛造用金型用の基材(母材)に含まれるAlの自己酸化被膜である。例えば、被鍛造材にガラス潤滑剤を被覆したときに、前記ガラス潤滑剤によって被覆層または被覆層と母材が腐食される現象を生じる場合がある。その時にAlの自己酸化被膜が母材との界面に存在すると、かかる自己酸化被膜がガラス潤滑剤による腐食の進行を妨げるバリア層として機能することが分かった。なお、自己酸化被膜の形成には、母材表面に無機材料の被覆層を形成した後に予備酸化処理を行うことで形成させることができる。
なお、前記のAlの自己酸化被膜は、例えば、900~1100℃で3~5時間の予備酸化を行うことで形成することができる。この予備酸化の条件が熱間鍛造前に行う熱間鍛造用金型の予備加熱の条件と異なる場合は、自己酸化被膜を形成するために特別に予備酸化を行う必要がある。
また、本発明では、前記被覆層の厚さは1層あたり2~200μmが好ましい。無機材料の種類により特性が異なるが、被覆層の特性を十分に発揮させるに好適な被覆層の厚さは1層あたり2~200μmとすることが良い。1層あたりの厚さが過度に薄いと、被覆層形成の効果が乏しくなる場合がある。また、被覆層の厚さを過度に厚くしても効果が飽和したり、コストが上昇するおそれがあるためである。
以下の実施例で本発明をさらに詳しく説明する。真空溶解にて表1に示すNi基超耐熱合金のインゴットを製造した。なお、表1に示す組成を有する合金は表2に示すような優れた高温圧縮強度の特性を有するものであり、熱間鍛造用金型として十分な特性を有するものである。なお、高温圧縮強度(圧縮耐力)は1100℃で行ったものである。
試験片上に形成した被覆層組成を確認する方法として、例えば、エネルギー分散型エックス線分析装置(以下、EDXと記す)による定量分析が考えられる。No.1~4の試験片の被覆層では、膜厚が薄く母材成分の影響を受けるためEDXによる正確な定量分析の値が得られなかった。そのため、これらの試験片では、被覆層の組成を考慮することにより、試験片の被覆層がSi及び金属元素のうち、Si,Cr,Alの一種以上を合計で30質量%以上含むと判断した。No.5~6の試験片では、EDXによる定量分析により、Si単独、またはSiとAlの総量で30質量%以上であることを確認した。
図3(a)にNo.1、(b)にNo.2、(c)にNo.3、(f)にNo.6の加熱試験10回目後の写真を示す。これらの実施例の被覆層は10回の繰り返し加熱試験では剥離しなかった。図3(d)にNo.4の加熱試験10回目後の写真を示す。No.4の被覆層の剥離は、7回目後から徐々に進行したものである。図3(e)にNo.5の加熱試験4回目後の写真を示す。No.5の被覆層の剥離は1回目後から徐々に進行し4回目後には完全に剥離したため、No.5の加熱試験は4回目で中止した。図3(g)に比較材の加熱試験10回目後の写真を示す。比較材では、1乃至10回目まで、表面の酸化とそれに伴うスケールの飛散が同様に見られた。
これらの結果から、No.1~No.4およびNo.6において、1乃至10回目まで、被覆層の剥離による酸化防止効果の低下が生じていないことがわかる。また、No.5においては被覆層の剥離の進行が見られるものの、1乃至3回目の加熱試験では被覆層の残存している領域に関しては酸化が防止されていた。このことは、例えば、No.5の被覆層は2~3回程度で塗布をし直すことで十分に耐酸化性が得られるものである。
図4(a)にNo.6の加熱試験10回目後の被覆層と母材を樹脂埋め込みし鏡面研磨した後断面方向から観察したFE-EPMA反射電子像、(b)にAlの元素マップ、(c)にOの元素マップを示す。元素マップ画像における濃淡は測定対象元素の濃度に対応しており、白い程濃度が高い。これらの図から、母材の被覆層側表面にAlとOが濃化しており、ここにAl酸化物層が形成されていることが分かる。このAl酸化物層はNo.6のセラミックスの塗料を塗布後1100℃にて3時間の保持中に形成されている。1100℃にて3時間保持の加熱試験とその10回の繰り返しの加熱試験においてNo.6の試験片が示した優れた耐酸化性は、No.6の被覆層の形成と加熱により母材の被覆層側表面に形成されたAl酸化物層に由来するものである。
被覆層が形成された熱間鍛造金型を用いてガラス潤滑剤を被覆した被鍛造材を鍛造するとき、前記ガラス潤滑剤によって被覆層または被覆層と母材が腐食される現象を生じる場合がある。
まず、ガラス潤滑剤により母材が腐食される現象を評価するため、前記比較材と同様に加工した試料上の中心付近に400~500mgのガラス潤滑剤を塗布した試験片を3個作製した。作製した試験片を加熱された炉に投入し、3時間保持した後炉から取り出して空冷させる加熱試験を、実機において想定される温度である900、1000、1100℃に対して各1回行った。なお、加熱試験における雰囲気は大気とし、本試験以降の試験の雰囲気も全て大気である。表5に使用したガラス潤滑剤の組成を示す。また、EDXによる定量分析により、SiとAlの総量が30質量%以上であることを確認した。
また、図7(a)にNo.7の予備酸化後の被覆層と母材を樹脂に埋め込んで鏡面研磨した後、断面方向から観察したFE-EPMA反射電子像、(b)にAlの元素マップ、(c)にOの元素マップを示す。これらの図から、母材の被覆層側表面にAlとOが濃化しており、予備酸化により母材と被覆層との間にAl酸化物層が形成されていることが分かる。No.7の試験片が示した前記ガラス潤滑剤による被覆層と母材の腐食の抑制は、このAl酸化物層に由来するものである。
Claims (13)
- 質量%で、W:10.3~11.0%、Mo:9.0~11.0%、Al:5.8~6.8%であり、且つ、残部がNi及び不可避的不純物であるNi基超耐熱合金からなる基材組成を有し、成形面、側面の少なくとも一方に無機材料の被覆層を有し、前記被覆層がSi及び金属元素のうち、Si,Cr,Alの一種以上を合計で30質量%以上含むことを特徴とする熱間鍛造用金型。
- 熱間鍛造用金型の表面全面に無機材料の被覆層を有することを特徴とする請求項1に記載の熱間鍛造用金型。
- 前記被覆層が窒化物、酸化物、炭化物の何れか1種類以上でなることを特徴とする請求項1または2に記載の熱間鍛造用金型。
- 前記被覆層は少なくとも窒化物を含み、前記窒化物を構成する窒素以外の元素のうち質量%で50%以上がCrである請求項1乃至3の何れかに記載の熱間鍛造用金型。
- 前記被覆層は少なくとも酸化物を含み、前記酸化物を構成する酸素以外の元素のうち質量%で50%以上がSiである請求項1乃至3の何れかに記載の熱間鍛造用金型。
- 前記被覆層は少なくとも炭化物を含み、前記炭化物を構成する炭素以外の元素のうち質量%で50%以上がSiである請求項1乃至3の何れかに記載の熱間鍛造用金型。
- 前記被覆層が炭化物と酸化物との混合相である、請求項1乃至3の何れかに記載の熱間鍛造用金型。
- 前記炭化物と酸化物との混合相を構成する炭素と酸素以外の元素のうち質量%で30%以上がSiである、請求項7に記載の熱間鍛造用金型。
- 前記被覆層が、それぞれ異なる組成を有する2層以上の積層構造である請求項1乃至8の何れかに記載の熱間鍛造用金型。
- 前記基材の表面と前記被覆層との間にAl酸化物層を有することを特徴とする請求項1乃至3の何れかに記載の熱間鍛造用金型。
- 加熱された鍛造素材を上型および下型によって熱間鍛造する鍛造製品の製造方法であって、前記上型及び下型として、請求項1乃至10のいずれか一項に記載の熱間鍛造用金型を用いる鍛造製品の製造方法。
- 基材としてNi基超耐熱合金を用いた熱間鍛造用金型の製造方法であって、
質量%で、W:10.3~11.0%、Mo:9.0~11.0%、Al:5.8~6.8%であり、且つ、残部がNi及び不可避的不純物であるNi基超耐熱合金からなる基材の成形面、側面の少なくとも一方に、窒化物、酸化物、炭化物の何れか1種類以上でなる無機材料を配置して被覆層を形成する熱間鍛造用金型の製造方法。 - 前記無機材料を配置した基材を加熱することによって前記基材の表面と前記被覆層の間にAl濃化酸化物層を形成することを特徴とする請求項12に記載の熱間鍛造用金型の製造方法。
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EP3719152A4 (en) * | 2017-11-29 | 2021-03-31 | Hitachi Metals, Ltd. | Ni BASED ALLOY FOR HOT FORGING DIE, AND USING HOT FORGING DIE |
EP3719153A4 (en) * | 2017-11-29 | 2021-04-07 | Hitachi Metals, Ltd. | NI-BASED ALLOY FOR HOT DIE, HOT FORGING DIE USER, AND FORGED PRODUCTS MANUFACTURING PROCESS |
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US11692246B2 (en) | 2017-11-29 | 2023-07-04 | Proterial, Ltd. | Ni-based alloy for hot-working die, and hot-forging die using same |
Also Published As
Publication number | Publication date |
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US11207725B2 (en) | 2021-12-28 |
US20180290202A1 (en) | 2018-10-11 |
CN108136482A (zh) | 2018-06-08 |
EP3357601A4 (en) | 2019-05-01 |
JP6108260B1 (ja) | 2017-04-05 |
EP3357601A1 (en) | 2018-08-08 |
EP3357601B1 (en) | 2020-12-23 |
CN108136482B (zh) | 2019-09-17 |
JPWO2017057453A1 (ja) | 2017-10-05 |
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