JPH0355204B2 - - Google Patents

Description

[Detailed description of the invention]

[Industrial Application Field] The present invention is applicable to wire drawing, cold forging, rolling, pipe drawing, etc., such as steel, stainless steel, Hastelloy, Incoloy, titanium, aluminum, magnesium,
The present invention relates to a lubrication treatment method for cold working of metal materials such as zirconium and its alloys. [Conventional technology] Conventionally, when cold working steel materials, a phosphate film is usually applied to the surface of the base material, and then a lubrication treatment is applied. It is well known that it is essential for cold working. In recent years, the use of materials other than steel, such as stainless steel, Hastelloy, Incoloy, titanium, aluminum, magnesium, zirconium, and their alloys, has increased, and with the development of these applications, it is possible to perform cold working with a high degree of workability. There is a demand for the development of a new lubrication treatment, but these metal materials are difficult to form a phosphate film that improves cold workability.
At present, this coating is not applied. In the case of stainless steel materials, oxalate coatings are available as an alternative to phosphate coatings, but seizure often occurs when subjected to high degree of cold working. As a lubricating film to which a chemical conversion film such as a phosphate film is not applied, there is a resin film. However, it is not suitable for high degree of cold working due to its poor adhesion to metal materials, heat resistance, and lubricity. The problems with the chemical conversion coatings currently applied for lubrication comparison are that, as mentioned above, the coating is difficult to form depending on the material, and in terms of workability, it is difficult to form a chemical coating on some materials. The processing time is long, 10 to 30 minutes, and when it comes to oxalate treatment of stainless steel materials,
This is not appropriate in terms of efficiency and cost since it requires a high temperature of 90° C. or higher and a relatively long treatment time of 10 to 30 minutes. [Problems to be Solved by the Invention] The present invention physically removes the oxide film on the surface of the metal material, and at the same time forms a metal film of zinc or zinc alloy that is easily formed into a phosphate film, The aim was to solve problems in terms of work and cost. [Means for Solving the Problems] As a specific means for solving the above-mentioned problems, the inventors of the present invention applied fine particles of zinc, zinc alloy, zinc or zinc alloy coated metal to the surface of the metal material by shot blasting. By spraying on the surface of the metal material, the oxide film on the surface of the metal material is removed, and at the same time, a zinc or zinc alloy film is formed on the surface of the metal material due to the collision of the fine particles, so that a zinc phosphate film is easily formed on the surface. After that, they found a method to chemically form a phosphate film thereon and then perform a lubrication treatment, thereby completing the present invention. Note that the present invention is applicable even if there is no oxide film on the surface of the metal material. [Description of Materials and Compositions] Metal materials used in the present invention include stainless steel, Hastelloy, Incoloy, titanium, zirconium, nickel, Kobaret, molybdenum, bearing steel, spring steel, high speed steel, and the like. The fine particles of zinc or zinc alloy or the fine metal particles coated with zinc or zinc alloy used for shot blasting should have a particle size of, for example, 0.2 to 1.1 mm, and the one with higher hardness will remove the oxide film on the surface of the metal material. Because of its good properties, it is best to coat iron-based fine particles with zinc and then heat the fine particles to alloy the zinc coating with the iron in the iron-based fine particles.A commercially available product is Dowa Iron Powder Industries Co., Ltd. Company-made Z-IRON
There is. The amount of metal zinc or zinc alloy film to be formed on the surface of the metal material is 0.1.
~50g/ ^m2 is suitable. To increase the amount of zinc metal or zinc alloy coating, increase the shot time. Furthermore, if the metal film is to be applied in a short period of time, the discharge amount of the shot should be increased. The discharge amount of the shot is generally 10 to 150 mm in projection thickness. As the phosphate treatment solution, a conventional acid phosphate treatment solution for zinc materials can be used. For example, phosphate ion 5
~100g/, zinc ion 3-50g/, nitrate ion 1-100g/, nickel ion 0-20g/
An example is an aqueous acidic phosphate solution consisting of 1, but no accelerator such as sodium nitrite is required during the treatment. This phosphate treatment is usually carried out at room temperature to 80° C. by dipping or spraying for 5 seconds to 10 minutes. In order to accelerate the film formation reaction, the surface of the metal to be treated on which the zinc or zinc alloy film has been formed may be surface-conditioned in advance with a surface-conditioning aqueous solution containing colloidal titanium. Next, the metal to be treated is treated with phosphate to form a phosphate film on the metal surface, and then washed with water or dried without washing with water, and finally subjected to a lubrication treatment without drying. Lubrication treatments include treatment with an aqueous alkaline soap solution, treatment with a liquid containing metal soap, treatment with lubricating oil,
Examples include methods such as solid lubrication treatment. Examples of alkaline soap treatment include immersion treatment in 40 to 100 g/aqueous solution of fatty acid soap such as sodium stearate at 70 to 90°C for 1 to 10 minutes, and drying to form a lubricating film.Metal soap treatment Examples include those treated with powders or solvent dispersions of metal salts of fatty acids such as calcium stearate, barium stearate, and zinc stearate. Examples of lubricating oils include oils, synthetic oils, mineral oils, etc. as base oils and extreme pressure additives such as sulfur compounds, phosphorus compounds, chlorine compounds, etc. Examples of solid lubricants other than metal soap include powders or solvent dispersions of molybdenum disulfide, tungsten disulfide, fluorine resins, graphite, wax, and the like. Further, in order to improve the adhesion of the solid lubricant to the surface of the base material, a resin may be added. [Function] By shot-blasting fine particles of zinc, zinc alloy, zinc-coated metal, or zinc alloy-coated metal onto the surface of a metal material, the oxide film on the surface of the metal material is physically removed, and at the same time, the fine particles are firmly attached or Penetrates and forms a film of metallic zinc or zinc alloy. By subjecting the surface on which this film has been formed to a phosphate treatment, a composite film of metal zinc and phosphate is formed on the surface of the metal material, which serves as an excellent base film for lubrication treatment. Since the phosphate film is composed of a group of microcrystals, it retains the lubricant well, and by applying lubrication treatment to this film, the film of zinc or zinc alloy - phosphate film - can be formed.
It exhibits excellent lubricity due to the synergistic effect of the lubricating film. Example 1 Particle size 0.3 on the surface of a pure titanium plate of 50 x 100 x 0.55 mm
~0.7 mm fine zinc particles were shot blasted for 10 minutes to form a metallic zinc coating of 15 g/m ² . Next, acidic zinc phosphate treatment solution for zinc at 62-68℃ (trade name Bonderite L3664, 90g/, AD4801 20
g/m 2 (manufactured by Nippon Parkerizing Co., Ltd.) for 10 minutes to form a zinc phosphate film of 9.8 g/m ² . It was washed with water, then immersed for 5 minutes in an aqueous lubricant solution containing sodium stearate as the main component (trade name: Bontariyube 235, manufactured by Nippon Parkerizing Co., Ltd., 70 g/) at 72 to 88°C, dried, and stearic acid A film with a soap content of 7 g/m ² was formed. The lubricity of this treated material was evaluated using the Bauten friction method.
Table 1 shows the results obtained using the abrasion tester. Comparative Example 1 was carried out using the same testing machine and treatment method as in Example 1, except that the step of shot blasting using fine zinc particles was omitted. Table 1 shows the results of the same lubricity evaluation as in Example 1, although no phosphate film was formed. As can be seen from this table, the material treated by the method of Example 1 had a lower coefficient of friction of 0.08 than Comparative Example 1, and the number of times of sliding before seizure occurred was 1200, which was excellent.

【table】

[Table] Example 2 A SUS304 stainless steel wire rod having an oxide film with a diameter of 2.3 mm was subjected to fine particles of zinc-iron alloy coated metal (trade name: Z-IRON manufactured by Dowa Iron Powder Industries Co., Ltd.) by shot blasting for 5 minutes. Projected onto stainless steel wire
Coat with 10 g/m ² of zinc-iron alloy. Next, a known zinc phosphate treatment solution Bonderite 3663 (manufactured by Nippon Parkerizing Co., Ltd.) 60g/AD4801 20
g/, soaked at 75-80℃ for 5 minutes, 12g/
m ² of zinc phosphate-based film was formed. After that, it was washed with water and dried. The lubricity of this wire was evaluated using a wire drawing tester. As a lubricant, powdered calcium stearate was placed in a die box in the pre-wire drawing process. Wire drawing was carried out under the conditions shown in Table 2, and there was no seizure even after 3 passes.
It was good and warm.

[Table] Comparative Example 2 Testing was carried out using the same testing machine and treatment method as in Example 2, except that the shot blasting process using zinc-iron alloy coated fine metal particles was removed. As a result, no zinc phosphate film was formed. Nakatsuta. Next, the lubricity was evaluated using a wire drawing tester, and as a result, seizure occurred in one pass. Comparative Example 3 An oxalate film of 9 g/m ² was formed on the same stainless steel wire as in Example 2 by the process shown in Table 3.
Lubricity evaluation was performed using a wire drawing tester using the same method as in Example 2. As a result, burn-in occurred in the second pass.

[Table] Example 3 Fine particles of zinc-iron alloy coated metal (trade name: Z-IRON manufactured by Dowa Iron Powder Industry Co., Ltd.) were shot blasted for 10 minutes on SCM-3 bar material with a diameter of 12 mm using the shot blasting method. Then, 15g/ ^m2 of zinc was added to the bar material.
Coated with iron alloy. Next, a known zinc phosphate treatment solution Bonderite L-3664 (manufactured by Nippon Parkerizing) 90g/AD4801 20g/, 65°C,
A 5 minute treatment produced a zinc phosphate based coating of 10 g/m ² . Next, wash with water, and then use Bondaryube #235 (manufactured by Nippon Parkerizing) 70g/, 75
℃ for 5 minutes and dried. This produced a lubricating layer of stearic acid soap of 7 g/m ² . To evaluate the lubricity of this bar material, a drawing test was conducted using a draw bench. The results are shown in Table-5. The drawing was carried out under the conditions shown in Table 4. Even after 3 passes, there was no seizure and the drawing force was low and good.

[Table] Comparative Example 4 Testing was carried out using the same testing machine and treatment method as in Example 3, except that the step of shot blasting using zinc-iron alloy coated fine metal particles was used. As a result, the weight of the zinc phosphate coating was 7 g/ ^m2 , and microscopic observation showed that the film completion rate was insufficient. Therefore, the chemical conversion treatment time was 10 minutes, twice that of Example 3, and the film weight was reduced to 11.
g/m ² was obtained and completed. The lubricity of the treated bar material was evaluated in the same manner as in Example 3, and the results are shown in Table 5.

[Table] As can be seen from Table 5, the pull-out force of the material treated by the method of Example 3 was lower than that of Comparative Example 4.
Excellent lubricity. [Effects of the Invention] As explained above, by performing the lubrication treatment of the present invention, oxide films on the surfaces of various metal materials are physically removed, and at the same time, zinc or zinc alloy films are formed on the surfaces of the metal materials, and phosphoric acid The salt film becomes a surface that is easily chemically formed. Therefore, a phosphate film can be chemically formed at a relatively low temperature and in a short time. The synergistic effect of the metal zinc-based film, phosphate film, and lubricant on the surface of the metal material provides excellent cold workability.

Claims (1)

[Claims] 1. Spray fine particles of zinc, zinc alloy, zinc or zinc alloy coated metal onto the surface of the metal material by shot blasting to form a zinc or zinc alloy film, form a phosphate film on the film, and then A method for lubricating metal materials, the method comprising applying lubrication treatment.