JP3252715B2 - Die for extruding aluminum and manufacturing method thereof - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aluminum extrusion die for extruding an aluminum extrusion having excellent surface properties and a method for producing the same.

[0002]

2. Description of the Related Art For architectural members such as wall materials, truck tilts, and the like, a method of forming a decorative part, which requires brilliancy, by extrusion has been adopted. Dies used for this type of extrusion are manufactured by subjecting hot tool steel to nitriding treatment such as salt bath nitriding.
The die surface such as the bearing surface hardened by the nitriding treatment has a large effect on the surface properties of the extruded profile obtained.However, the aluminum alloy during extrusion comes into contact with it and is worn by the metal flow of the aluminum alloy. It is an easy place. Therefore, how to keep the surface of the die in the same state as at the start of extrusion is important for stabilizing the quality of the extruded profile. For example, as the extrusion continues, the bearing surface wears out, the hard surface layer partially falls off, and the composition and hardness of the surface layer become uneven. The non-uniform surface layer causes dimensional variations in the extruded profile and adversely affects the surface properties of the profile. As a result, defects such as streaks that deteriorate the surface quality tend to appear on the surface of the extruded shape. Therefore, in an actual operation, after extruding a certain amount, the bearing surface is polished to correct the shape, renitrided, and repeatedly used for the next extrusion.

[0003]

Extrusion dies become thinner and thinner due to repeated reshaping of the die surface, and are eventually discarded. However, since the dies are expensive, the more times they can be used repeatedly by renitriding before they are discarded, the lower the production cost.
Also, the less the wear of the die bearing surface, the longer the life of the die, the higher the production efficiency and the more stable the shape quality. Especially for products requiring excellent surface properties such as building wall materials and truck tilts, it is important to control the die bearing surface, and always maintain a constant bearing shape for product quality control. It is necessary. However, in the dies processed by the current salt bath nitriding or gas nitriding, iron oxide is formed on the surface of the nitride layer in addition to iron nitride. The iron oxide peels and falls off from the bearing surface during extrusion, and deteriorates wear resistance. As a result, abrasion of the iron nitride is promoted, and surface defects such as streaks tend to occur. The present invention has been devised to solve such a problem. By controlling the nitriding conditions, the formation of iron oxide is suppressed, and a nitrided layer having excellent wear resistance is formed on a hot tool steel. It is an object of the present invention to obtain a long-life extrusion die suitable for producing an extruded profile having good surface quality.

[0004]

In order to attain the object, the manufacturing method of the present invention is characterized in that after hot tool steel is quenched and tempered, an oxide layer formed on the surface of the hot tool steel is mechanically removed. When performing a nitriding treatment that is removed by a treatment and / or a chemical treatment and is maintained at 480 to 550 ° C. for 5 to 10 hours in a nitriding gas atmosphere having a nitrogen source, Fe on the hot tool steel surface after the nitriding treatment is performed. The oxygen concentration in the atmosphere during the chemical treatment or the nitriding treatment is controlled to 20 to 100 ppm so that the X-ray intensity ratio of ₃ O ₄ / Fe ₃ N is 5% or less. The oxide layer generated by quenching / tempering is removed from the surface of the hot work tool steel by mechanical polishing using a file or the like, cleaning in a reactive gas, or the like. In cleaning using a reactive gas, for example, quenched and tempered hot tool steel is kept at 300 to 500 ° C. for 15 to 60 minutes together with a substance containing a fluorine source such as vinylidene fluoride resin. Further, a substance containing a chlorine source such as vinylidene chloride resin can also be used. When cleaning in a reactive gas, it is important to adjust the amount of oxygen in the atmosphere to 20 to 100 ppm. In an atmosphere in which the amount of oxygen exceeds 100 ppm, the cleaning effect of oxides by F or Cl decreases. Conversely, in an atmosphere where the oxygen content is less than 20 ppm, the cleaning action of F or Cl on the steel material surface is too strong, and a smooth surface state cannot be maintained.

As a nitriding gas atmosphere having a nitrogen source, ammonia gas alone or a mixed gas of ammonia gas and nitrogen gas is used. In order to compensate for the decrease in the amount of solute carbon on the surface caused by nitriding and to secure the C content of the base material, carbon dioxide gas is added at a rate of 5% by volume or less to a nitriding gas atmosphere having a nitrogen source. Is preferred. However, since the added carbon dioxide gas also acts as an oxygen source to oxidize the nitride layer, it is desirable to set the carbon dioxide gas addition amount to a value as low as possible as long as the amount of dissolved carbon is compensated. . In order to suppress the oxidation of the nitrided layer during the nitriding treatment, the oxygen amount of the nitriding atmosphere gas is set to 20.
It is important to adjust to １００100 ppm. In an atmosphere in which the amount of oxygen exceeds 100 ppm, crystal growth of nitrides is hindered by formation of oxides. Conversely, if the amount of oxygen is less than 20 ppm, the crystal orientation of the iron nitride is promoted, and it becomes difficult for the iron nitride to grow randomly. In the aluminum extrusion die according to the present invention, the nitrided layer is formed on the surface of the hot work tool steel after removing the oxide generated by the quenching / tempering treatment, and the surface layer after the nitriding treatment is formed of Fe ₃ O ₄ / Fe
_The 3N X-ray intensity ratio is regulated to 5% or less. At this time, Fe ₃ formed on the surface of the hot tool steel by nitriding treatment
N has a random crystal orientation without being oriented in a specific orientation.

[0006]

Embodiment

Substrate Selection and Hardness Tempering The extrusion die according to the present invention has a S
Hot tool steels such as KD61 and SKD62 are used and tempered to a predetermined hardness by quenching and tempering. The hardness of the substrate is preferably tempering in the range of H _RC 45 to 53.
If the hardness is more than H _RC 53, the toughness of the steel is deteriorated, easily cracked. Conversely too soft in hardness of less than H _RC 45, the die is easily deformed by the pressure during extrusion. Removal of oxides Iron oxide is generated on the surface of hot work tool steel after quenching and tempering. This oxide is composed of Fe ₃ O ₄ , Fe ₂
O _{3 and the} like are increased by the influence of the oxygen concentration in the atmosphere at the time of chemical treatment or nitriding treatment performed as a post-process.
In the process of preheating the nitrided die to about 500 ° C. at the time of extruding aluminum, the oxide on the surface tends to further increase.

[0007] Iron oxide has weak adhesion to a substrate,
Moreover, it is easily worn as compared with iron nitride Fe ₃ N. As a result, the aluminum is exfoliated or abraded during the extrusion of aluminum, causing defects on the surface of the extruded aluminum material. In order to suppress such defects, it is important to control iron oxide. In this connection, the present inventors have found that it is effective to control the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N on the surface of the die to 20% or less immediately before extrusion, and Japanese Patent Application No. 8-185618. No. (Japanese Unexamined Patent Application Publication No. 9-1
No. 92726). In order to reduce the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N to 20% or less, it is necessary to control the oxide from the beginning in the die manufacturing process. The present invention and the like further advance the research, and by controlling the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N on the die surface after the nitriding treatment to 5% or less, defects caused by iron oxide can be suppressed. I found Fe ₃ a peak value in the vicinity of the X-ray diffraction angle 35.5 degrees measured as O _4, X-ray diffraction angle as Fe ₃ N 43.
The peak value around 5 degrees is measured, and both peak values are compared.
The X-ray intensity ratio of e ₃ O ₄ / Fe ₃ N is determined. Although iron oxides generated on the surface of the substrate also includes Fe ₂ O _3, Fe ₂
Peak value of O ₃ from overlap with _{Fe 3 O 4, Fe 3 O} 4
The iron oxide can be quantified by measuring the peak value while paying attention to. In order to reduce the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N to 5% or less, first, a surface oxide generated on the surface of the hot tool steel by heat treatment such as quenching and tempering is mechanically removed.
For example, the surface oxide is removed by polishing the surface of the hot tool steel with a metal file, a paper file, or the like. This step can be omitted if the formation of surface oxides during quenching and tempering is controlled and oxides that do not need to be removed are generated.

Removal of Oxide by Chemical Treatment A die from which surface oxide has been removed with a paper file or the like or a dice having a small amount of surface oxide is further subjected to chemical cleaning to remove oxide before the nitriding treatment. As a chemical cleaning method, the dice is kept at 300 to 500 ° C. for 15 to 60 minutes together with a substance containing a fluorine source or a chlorine source. 3
By heating to 00 to 500 ° C., the fluorine source or chlorine source is decomposed, and activated F or Cl is generated. The activated F or Cl reacts with the oxide on the die surface, and the oxide is removed from the die surface. Heating temperature is 300 ℃
If the temperature is less than 500 ° C., the difference from the nitriding temperature in the subsequent process is too large, and if it exceeds 500 ° C., the cleaning effect by F or Cl is inferior. Further, if the holding time is less than 15 minutes, the cleaning is insufficient, and even if the holding time exceeds 60 minutes, the cleaning effect is not improved as long as the holding time.

As the fluorine source, gaseous, solid and the like are used. The gaseous fluorine source includes F ₂ , ClF ₃ , N
F ₃ , CF ₄ , SF ₆ , C ₂ F _{6 and the} like. Solid fluorine sources include PTFE, PCTFE, PVD containing fluorine.
There are resins such as F and PVF. For example, activated F can be generated by wrapping the dice with a resin sheet or heating with the pellets placed near the dice. As the chlorine source, gaseous, solid or the like is used. Examples of the gaseous chlorine source include HCl and ClF ₃ . Solid chlorine sources include chlorine-containing resins such as vinyl chloride and vinylidene chloride. Also in this case, activated Cl can be generated by wrapping the dice with a resin sheet or heating with the pellets placed near the dice. As an atmosphere for cleaning, it is important to adjust the oxygen concentration to 20 to 100 ppm. If the atmosphere contains a large amount of oxygen exceeding 100 ppm, the oxide on the die surface will not be decomposed by F or Cl, and the die surface will not be cleaned. In an atmosphere having an oxygen concentration of 100 ppm or less, cleaning of the die surface is performed smoothly. In an atmosphere having an oxygen content of 20 ppm or less, F or Cl excessively reacts with the steel surface, and surface uniformity is impaired. Also, as for the water vapor contained in the atmosphere, the oxygen potential is increased and F or Cl is consumed, so that the smaller the water vapor, the more preferable.

Nitriding treatment The dice from which oxides have been removed from the surface are subjected to nitriding treatment at 480 to 550 ° C. × 5 to 10 hours in a nitriding gas atmosphere containing a nitrogen source. If the treatment temperature does not reach 480 ° C., the reaction is slow, and if it exceeds 550 ° C., the steel of the base material is easily softened. If the heating time is less than 5 hours, a sufficient nitrided layer cannot be obtained, and if the heating time exceeds 10 hours, the effect corresponding to the prolonged heating time cannot be obtained. As the nitrogen source, ammonia alone or a mixed gas of ammonia and nitrogen is used. In addition, when carbon dioxide gas is added, a decrease in the amount of solute carbon on the surface of the steel material due to an increase in temperature is compensated. However, if an excessive amount of carbon dioxide is added, the oxygen potential of the atmosphere rises and the white layer may be oxidized.
% Or less. By this nitriding treatment, the surface of the die including the bearing surface has a thickness of 10 mm.
A white layer having a thickness of 4 to 8 μm is formed via a nitrogen diffusion layer of 0 to 150 μm. If the thickness of the white layer is less than 4 μm, the abrasion resistance is not sufficient, and if it exceeds 8 μm, the processing time becomes long and it is not economical. The white layer is composed of iron nitride Fe _x N (x
= 2 to 3) to impart sufficient hardness and wear resistance to the die. At this time, the oxygen concentration in the atmosphere is 20 to 1
It is necessary to adjust to 00 ppm. Oxygen concentration is 100p
pm, the production amount of iron oxide increases, and Fe ₃ O ₄
The X-ray intensity ratio of / Fe ₃ N may exceed 5%. On the other hand, when the oxygen concentration is less than 20 ppm, the crystal of Fe ₃ N takes a direction and is not formed in a random orientation effective for improving the wear resistance. Further, the oxygen content of less than 20 ppm
It also acts to weaken the force of dissolving C on the surface by CO ₂ or the like.

X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N Fe ₃ O ₄ and Fe ₂ O ₃ coexist in the iron oxide formed on the die surface. However, in X-ray diffraction, Fe
Since the peak value of the ₂ O ₃ overlaps the Fe ₃ O _4, can grasp the oxygen concentration of the nitride layer by the peak value of the Fe ₃ O ₄ in the vicinity ° diffraction angle 35.5. Iron nitride has Fe ₃ N, and can be identified by an X-ray diffraction peak value around 43.5 degrees. X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N 5
The condition of% or less is determined based on the results of many experiments by the present inventors and is an effective index for preventing the oxidation and disappearance of the nitride layer formed on the die surface. F
When the X-ray intensity ratio of e ₃ O ₄ / Fe ₃ N is 5%, the oxidation tendency of the nitride layer is separated. If it is 5% or more, the oxide tends to grow in the preheating step immediately before extrusion, and the Fe ₃ O ₄ / Fe ₃ N X
The line intensity ratio exceeds 20%. In this regard, in order to suppress the increase in oxides in the preheating step immediately before extrusion and maintain a sound nitrided layer, Fe ₃ O ₄ / F after nitriding is required.
An important factor is to make the X-ray intensity ratio of e ₃ N 5% or less.

Comparing the free energy of formation of iron oxide and iron nitride in the reaction during the nitriding treatment, the free energy of formation of iron oxide is smaller than the free energy of formation of iron nitride. In other words, if oxygen is present in the atmosphere, an oxide is likely to be formed first. Also in this respect, it is necessary to control the amount of oxygen in the atmosphere. Also,
As a result of investigation and research by the present inventors, it has been found that the (100) plane of Fe ₃ N depends on the amount of oxide. Note that the nitride peak is far from the oxide peak and can be easily distinguished, so that the influence of the oxide can be understood from the pole figure of the (100) plane. As described in the examples described later, the crystal orientation of the nitride becomes uniform as the amount of the oxide increases. This means that the amount of the oxide can be determined from the crystal orientation of the nitride. That is, Fe
Without crystal orientation of ₃ N are oriented, when a random amount of oxides is small, it can be seen that sound nitride layer is formed. In order to randomize the Fe ₃ N crystal, a passivated oxide film is formed from the die surface by mechanical means, chemical means or a combination of both prior to nitriding in order to form a nitride layer while suppressing the formation of oxide. It is important to remove and perform nitriding in an atmosphere in which the amount of oxygen is controlled. The above-mentioned conditions are also employed when renitriding for repeated use in the extrusion process. After the dies have been used for extrusion, a white layer, namely Fe
The nitride layer disappears due to abrasion, but is re-nitrided under the same conditions to be reused as an extrusion die having a sound nitride layer.

[0013]

【Example】

Example 1: The hot aluminum extrusion die made of a tool steel SKD61 by quenching and tempering, after tempering the hardness to H _RC 52, to remove the oxide polish the bearing surface with sandpaper. Thereafter, the die was wrapped with a vinylidene fluoride resin sheet, placed in a heating furnace, and heated and maintained at 350 ° C. for 30 minutes. The vinylidene fluoride resin was decomposed by heating and holding, and the die surface was cleaned with a highly reactive decomposed gas to remove oxides such as a passive film from the surface. At this time, the amount of oxygen in the atmosphere was about 50 ppm. Then, NH3 by volume ratio
A mixed gas of ₃ : N ₂ : CO ₂ = 1: 3: 0.2 was introduced into a heating furnace and subjected to a nitriding treatment at 520 ° C. × 7 hours. At the time of nitriding, the amount of oxygen in the atmosphere was about 80 ppm. When the nitride layer formed on the die surface was subjected to X-ray diffraction, FIG.
The analysis result shown in (a) was obtained. As is clear from FIG. 1 (a), almost no Fe ₃ O ₄ was detected in the nitrified die, indicating that a nitride layer mainly composed of Fe ₃ N was formed. In this case, the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N was 3%. In addition, F
As shown in FIG. 2A showing the pole figure of e ₃ N (100), the plane orientation distribution of the crystal grains forming the nitride layer was almost random and random.

For comparison, FIG. 1B shows the result of X-ray diffraction of a nitride layer formed by a conventional salt bath nitriding using a cyanic acid-based salt bath. In a salt bath nitrided die, Fe ₃ N
And Fe ₃ O ₄ are identified on the outermost surface. In this case, Fe
The X-ray intensity ratio of ₃ O ₄ / Fe ₃ N was 7%. This is presumably because the surface of the nitrided layer was oxidized during the salt bath nitriding treatment, and the generated oxide layer appeared as an X-ray diffraction peak. Also, in the pole figure of Fe ₃ N (100) shown in FIG. 2B, Fe ₃ N is contained in the sample plane, and [110]
It shows a tendency of preferential orientation with axes close to. When the hardness distribution of the formed nitrided layer was measured, the surface hardness of the nitrided layer formed according to the present invention was higher than that of the nitrided layer formed by the conventional method, as shown in FIG.
The high surface hardness is attributable to the fact that the nitrided layer formed according to the present invention has a small amount of iron oxide and the nitrided layer is mainly formed of iron nitride having high hardness. Generally, it is said that the higher the surface hardness, the higher the wear resistance. The results of this hardness measurement indicate that the nitrided layer according to the present invention has excellent wear resistance.

Example 2 A building material was extruded from a billet of aluminum alloy 6063 using a die made according to the present invention and a spandrel die made by conventional salt bath nitriding. Prior to extrusion, each die was heated and held at 450 ° C. for 5 hours in a nitrogen atmosphere having an oxygen concentration of 50 to 60 ppm. In addition, Fe ₃ O ₄ / Fe ₃ on the preheated die surface immediately before extrusion.
When N was estimated from another experiment, the X-ray intensity ratio was 20% or less for the die subjected to the nitriding treatment according to the present invention and 30% for the conventional salt bath-nitrided die. The surface roughness of the extruded profile was measured, and the transition of the surface roughness according to the number of extruded billets was investigated. As can be seen from the investigation results in FIG. 4, in the conventional die subjected to the salt bath nitriding treatment, the surface roughness of the profile increased as the number of extruded billets increased. On the other hand, in the die subjected to the nitriding treatment according to the present invention, the rate of increase in the surface roughness of the profile is suppressed, and it can be seen that the profile having stabilized surface properties is obtained. In addition, when the bearing surface of the die was observed after the extrusion, almost no damage such as cracking or scabs was detected.

Example 3 Two kinds of dies subjected to nitriding treatment in the same manner as in Example 2 were subjected to a preheat treatment of heating and holding at 450 ° C. for 5 hours in a nitrogen atmosphere having an oxygen concentration of 50 to 60 ppm. Extruded from billet. After the obtained shaped material was subjected to alumite treatment and sealing treatment, characteristics such as color tone and gloss were examined. As can be seen from the investigation results in FIG. 5, the extruded profiles obtained using the conventional dies have low gloss at the beginning of the second and third billet presses, exhibit a high L value, and exhibit a whitish color tone. I was On the other hand, in the extruded profile obtained by using the die nitrided in accordance with the present invention, the start of pushing did not tend to become extremely white.

Example 4 Two kinds of dies subjected to nitriding treatment in the same manner as in Example 2 were subjected to a preheat treatment of heating and holding at 450 ° C. for 5 hours in a nitrogen atmosphere having an oxygen concentration of 50 to 60 ppm. Extruded. After extruding the same number of billets, the wear state of the bearing surface was visually observed for each die, and the surface of the extruded profile was visually observed. As a result, when extruded with a die nitrided according to the present invention, less cracking occurred and the surface gloss of the profile was higher than in the conventional method.
Furthermore, as a result of comparing the number of extruded billets up to the occurrence of abrasion after each nitriding treatment, cracking occurred in the conventional method after extruding 57 billets, making extruding impossible. On the other hand, in the case of using the dies which were subjected to the nitriding treatment according to the present invention, no cracking occurred even after 70 billets were extruded, and the extrudable state was obtained. This also confirms that the nitrided layer formed according to the present invention has good wear resistance due to the small amount of oxide.

[0018]

As described above, the extrusion die of the present invention has a reduced oxide content and excellent wear resistance.
₃ nitride layer mainly composed of N is formed on the die surface. The X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N on the die surface immediately before extrusion is adjusted to 5 to 100 ppm by adjusting the oxygen amount in the atmosphere for cleaning the die surface and the atmosphere for nitriding treatment to 20 to 100 ppm. %, And the crystal orientation of Fe ₃ N is random without orientation. Therefore, even when preheating is performed prior to extrusion, the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N is maintained at 20% or less. The nitride layer adjusted in this way is excellent in surface hardness and abrasion resistance, and can be extruded with good aluminum productivity. In addition, the surface shape of the obtained extruded material is stabilized, and a high-quality product is manufactured.

[Brief description of the drawings]

FIG. 1 is an X-ray diffraction pattern of a nitride layer formed in the present invention example (a) and the comparative example (b).

FIG. 2 is an Fe ₃ N (100) pole figure of the nitrided layers formed in the present invention example (a) and the comparative example (b).

FIG. 3 shows a hardness distribution of a surface of a die subjected to nitriding treatment in the present invention example and the comparative example.

FIG. 4 shows the effect of the die on the surface roughness of the obtained extruded profile when extruded using dies which have been subjected to nitriding treatment in the inventive examples and comparative examples.

FIG. 5 shows the effect of the die on the gloss and color tone of the extruded material obtained when extrusion is performed using the nits that have been subjected to nitriding in the inventive examples and the comparative examples.

Claims (10)

(57) [Claims] After a hot tool steel is quenched and tempered, an oxide layer formed on the surface of the hot tool steel is removed by a mechanical treatment and / or a chemical treatment, and a nitriding gas having a nitrogen source is provided. When performing nitriding at 480 to 550 ° C. for 5 to 10 hours in an atmosphere, the X-ray intensity ratio of Fe ₃ O ₄ / Fe ₃ N on the hot tool steel surface after the nitriding becomes 5% or less. As described above, a method for manufacturing an aluminum extrusion die, wherein the oxygen concentration in the atmosphere during the chemical treatment or the nitriding treatment is controlled to 20 to 100 ppm. 2. The manufacturing method according to claim 1, wherein the quenched and tempered hot tool steel is mechanically polished to remove an oxide layer from the surface of the hot tool steel. Fluoride and wherein quenching and tempered hot work tool steel
With substances containing iodine source holding 15 to 60 minutes to 300 to 500 ° C., a manufacturing method of claim 1, wherein the removal of oxide layer from the surface of the hot work tool steel. 4. The method according to claim 3, wherein a vinylidene fluoride resin is used as the substance containing a fluorine source. 5. The quenched and tempered hot tool steel is kept at 300 to 500 ° C. for 15 to 60 minutes together with a material containing a chlorine source to remove an oxide layer from the surface of the hot tool steel. The method according to claim 1. 6. The method according to claim 5, wherein a vinylidene chloride resin is used as the substance containing a chlorine source. 7. The method according to claim 1, wherein the nitriding gas atmosphere having a nitrogen source is ammonia gas alone or a mixed gas of ammonia gas and nitrogen gas. 8. A nitriding gas atmosphere having a nitrogen source to which carbon dioxide gas is added at a ratio of 5% by volume or less is used.
Or the manufacturing method of 7. 9. A nitrided layer is formed on the surface of the hot work tool steel after removing the oxide generated by the quenching / tempering treatment, and the surface layer after the nitridation treatment is formed of X _{3 of} Fe ₃ O ₄ / Fe ₃ N. Die for extruding aluminum that is regulated to a linear strength ratio of 5% or less. 10. The aluminum extrusion die according to claim 9, wherein the crystal orientation of Fe ₃ N formed on the surface of the hot tool steel by the nitriding treatment is random.