CN109252121B - Processing method of needle-shaped crystal patterns on surface of thin-wall pure titanium product - Google Patents
Processing method of needle-shaped crystal patterns on surface of thin-wall pure titanium product Download PDFInfo
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- CN109252121B CN109252121B CN201811274123.9A CN201811274123A CN109252121B CN 109252121 B CN109252121 B CN 109252121B CN 201811274123 A CN201811274123 A CN 201811274123A CN 109252121 B CN109252121 B CN 109252121B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
Abstract
The invention provides a processing method of needle-shaped crystal flowers on the surface of a thin-wall titanium product, which comprises the following steps: (1) degreasing: providing a finished thin-wall titanium product and removing oil stains on the surface of the product; (2) stress relief: placing the thin-wall titanium product in a vacuum furnace, vacuumizing to 1.0 multiplied by 10‑2Heating to 480-550 ℃ below Pa, and keeping the temperature for 0.25-2 h; (3) purification and homogenization treatment: heating to 680-750 ℃ for the second time, and preserving heat for 0.5-4 h; (4) crystal growth: heating to TβPreserving the heat for 3-10 h at the temperature of-1000 ℃; (5) quenching: cooling to T with the furnaceβ～(Tβ+40) deg.c, introducing argon gas and quick air cooling to TβObtaining needle-shaped patterns at the temperature below DEG C; (6) cooling, discharging, and continuously air cooling/furnace cooling to below 80 deg.C. The processing method of the invention does not need high pollution procedures such as polishing, acid washing and the like in the processing process, can obtain the needle-shaped crystal patterns with high finish degree and metallic luster, and has good uniformity and consistency of the patterns and excellent anti-fouling performance.
Description
Technical Field
The invention relates to the technical field of surface treatment of titanium products, in particular to a method for processing needle-shaped crystal patterns on the surface of a thin-wall pure titanium product.
Background
Along with the improvement of living standard, the sanitation and health of daily hardware products are increasingly concerned. Titanium products meet this health need of people with their excellent corrosion resistance and safety. At present, the main surface treatment modes of the thin-wall titanium product comprise modes of paint baking, sand blasting, wire drawing, conventional anodic oxidation and the like. Wherein, the baking varnish does not accord with the concept of health and environmental protection of titanium products, and can not effectively exert the characteristic of corrosion resistance. The surface effect obtained by the processes of sand blasting, wire drawing, conventional anodic oxidation and the like is single, the pollution resistance is poor, the titanium product is difficult to clean, the use experience of the titanium product is poor, and the advantages of bacteriostasis and sanitation are not exerted.
The published patent CN 107215139A discloses a processing method of titanium product crystal patterns, which directly raises the temperature to over 1000 ℃, resulting in that the crystal growth speed is too fast, and the grain size distribution and the shape uniformity of crystal grains can not be effectively controlled; particularly, the release of local cold working stress and the recrystallization of broken grains of a thin-wall product formed by cold working consume more energy, so that the size and the shape of patterns are obviously different from those of other parts. The diffusion speed of oxygen element is larger than the generation speed of oxide film under high temperature (above 1000 ℃), and the material surface can keep metallic luster and can not be oxidized. But in the cooling process, particularly at temperatures below 800 ℃, oxygen hardly diffuses and the degree of vacuum is low (10)-20.1Pa) and backfilling argon gas at this vacuum level resulted in the formation of a gray oxide film. At the same time, at 10-2At the temperature of more than 1000 ℃ and Pa grade, elements such as molybdenum, chromium and the like in the heating body and the heat insulation material of the hearth can volatilize to pollute the surface of the titanium material, and bright metal can not be obtainedAnd (4) gloss. Therefore, after the heat treatment, a process of polishing, etching with acid, and the like is required to be added to obtain metallic luster. For thin-wall parts with the thickness of less than 0.8mm, particularly workpieces with complex shapes, the polishing process can hardly be finished, and uneven phenomenon also exists in acid washing and etching. On the other hand, argon is directly introduced from high temperature (above 1000 ℃), the cooling capacity of the medium is very limited, the temperature reduction time in the phase change interval is too long, only coarse tissue can be obtained, and the fine needle-shaped tissue structure formed in the rapid quenching phase change process cannot be obtained; and under the high temperature condition, the strength of the thin-wall product is too low, and the workpiece is easy to deform in the argon air cooling process.
And published patent application No. CN 108220849A discloses a surface treatment method for titanium molecule fission of a bulk product, which also has the problems of uneven grain size distribution and large variation in grain pattern shape. The essence of the patent is to improve the strength of the product, and combine high temperature (above 1000 ℃), low pressure or low activity (minus 8-10 Pa) oxygen permeation and thermal oxidation (100-500 ℃) to improve the strength of the titanium product. However, oxygen, which is a harmful element of titanium materials, has a great influence on the toughness of titanium products, and particularly for thin-walled titanium products, the material becomes brittle, the impact resistance is poor and embrittlement easily occurs due to oxygen permeation at high temperature for a long time. Also, the patent directly adopts high-temperature air cooling of gas, has limited cooling capacity, can only obtain a coarse structure, and cannot obtain a fine needle-shaped phase change structure. Meanwhile, the nitrogen cooling adopted by the patent not only pollutes the surface of the material (nitrogen can react with a high-temperature titanium material), but also is easier to deform the thin-walled part (the nitrogen cooling capacity is strong, and the thermal stress is large). On the other hand, in the cooling process of high-temperature low-activity oxygen permeation and low-temperature air thermal oxidation treatment, a thicker oxide film is formed, and a crystal pattern with metallic texture and gloss cannot be obtained.
Disclosure of Invention
The invention provides a processing method of needle-shaped crystal patterns on the surface of a thin-wall (wall thickness of 0.15-0.8 mm) titanium product, which aims to solve the problems that the prior art is not uniform in grain size distribution, large in crystal pattern shape difference, not suitable for thin-wall titanium products and incapable of directly obtaining the surface with metal patterns.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the invention provides a processing method of needle-shaped crystal patterns on the surface of a thin-wall titanium product, which comprises the following steps:
(1) degreasing: providing a finished thin-wall titanium product and removing oil stains on the surface of the product;
(2) stress relief: placing the thin-wall titanium product in a vacuum furnace, vacuumizing to 1.0 multiplied by 10-2Heating to 480-550 ℃ below Pa, and keeping the temperature for 0.25-2 h;
(3) purification and homogenization treatment: heating to 680-750 ℃ for the second time, and preserving heat for 0.5-4 h;
(4) crystal growth: heating to TβPreserving the heat for 3-10 h at the temperature of-1000 ℃;
(5) quenching: cooling to T with the furnaceβ～(Tβ+40) deg.c, introducing argon gas and quick air cooling to TβObtaining needle-shaped patterns at the temperature below DEG C;
(6) and cooling and discharging, namely continuously cooling by air/furnace to below 80 ℃, and discharging to obtain the thin-wall titanium product with the surface provided with the needle-shaped crystal patterns.
Further, in the step (1), the wall thickness of the thin-wall titanium product is 0.15-0.80 mm, and the material is industrial pure titanium with the brand TA 1.
Further, in the step (1), ultrasonic or hot alkali solution is adopted to remove oil stains on the surface of the steel plate.
Further, the homogenization in the step (3) means that low-temperature recrystallization is performed to obtain a uniform grain size, and simultaneously, residual dirt on the surface is volatilized completely, and the oxide scale is decomposed and absorbed by the matrix. Under the conditions of high vacuum and high temperature, dirt on the surface of titanium metal is decomposed and vaporized to be removed; the porous oxide film reacts with the titanium metal, and diffuses and dissolves into the matrix, and disappears. The effects of uniform tissue and granularity and clean surface are obtained.
Further, said T in step (4)βThe alpha → beta phase transition temperature is 882-889 ℃ according to the difference of different smelting batches, mutual phagocytosis and surface microscopic atom rearrangement occur among crystal grains in the secondary growth process of the titanium metal crystal, and the crystal grains growWhen the size is large enough, the defects such as micro burrs, indentations and the like are phagocytosed.
Further, during the temperature rise in step (3) and/or step (4), a vacuum of 1.0 × 10 was maintained-2Pa below; preferably, the vacuum degree is kept between 6 and 9 multiplied by 10-3Pa。
Further, the secondary temperature rise process in the step (4) comprises the following steps: in the first stage, heating to 900-930 ℃, introducing high-purity argon, maintaining the pressure of the argon in the hearth at 10-80 Pa, and preserving the temperature for 10-30 min; then heating to 980-1260 ℃, and keeping the temperature for 1-5 h.
Further, in the step (5), the pressure of the introduced argon is 0.08-0.15 MPa, the metal is subjected to quick air cooling, and the metal is subjected to martensite phase transformation through a phase transformation interval to form needle-shaped relief patterns, and the needle-shaped relief patterns are stored; wherein too low argon pressure has limited cooling capacity and needle-like crystallized grains cannot be obtained, and too high argon pressure causes serious deformation of the titanium product.
Further, the heat treatment steps in steps (2) to (5) are sequentially subjected to batch furnace separation treatment, and the same effect can be obtained.
In a second aspect of the invention, there is provided a thin-walled titanium article having a surface with an acicular crystal pattern as processed by the above method.
Furthermore, the needle-shaped crystal patterns on the surface of the thin-wall titanium product have metallic luster, and the needle-shaped whiskers are 1-5 mm long; preferably 2-3 mm.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
(1) the thin-wall titanium product processed by the method has surface needle-shaped crystal patterns, does not need high-pollution steps such as grinding, polishing, acid washing and the like, and is more environment-friendly;
(2) through stress relief and homogenization treatment, the uniformity of grain size and the consistency of crystal patterns can be ensured;
(3) at Tβ～(TβThe quenching at 40) DEG C can exert the cooling effect of argon gas to the maximum extent, keep the uniformity of the cooling process and obtain fine needle-shaped patterns, and is more elegant and beautiful;
(4) under the condition of high vacuum/argon, the surface formed in the recrystallization and cooling processes is pollution-free, high in smoothness and good in dirt resistance.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
(1) Processing a titanium product: adopting a 0.6mm TA1 belt material (phase transition temperature Tbeta, 889 ℃), preparing a cup body with the diameter of 60mm and the depth of 80mm by blanking, stretching, trimming, curling and welding a handle; and ultrasonically cleaning and decontaminating the finished thin-wall titanium product.
(2) Stress relief: putting the cup body into a vacuum furnace, and vacuumizing to 8 multiplied by 10-3Pa, heating to 550 ℃, and keeping the temperature for 0.5h, wherein the vacuum degree is kept at 6-9 multiplied by 10 in the heating process-3Pa;
(3) purification and homogenization treatment: heating to 680 deg.C for 4h, and maintaining the vacuum degree at 6-9 × 10-3Pa；
(4) Crystal growth: raising the temperature to 990 ℃ again, and preserving the heat for 3 hours;
(5) quenching: cooling to 910 deg.C with the furnace, introducing 0.15MPa argon gas for rapid air cooling;
(6) and continuously cooling the material in an air cooling/furnace to below 80 ℃, discharging the material out of the furnace, and obtaining the needle-shaped patterns with metallic luster, wherein the length of the needle-shaped crystal whisker is 3-5 mm.
Example 2
(1) Processing a titanium product: the method is characterized in that a phi 48 multiplied by 0.5mmTA1 pipe (phase change starting temperature and phase change finishing temperature) is adopted, the pipe is expanded and thinned to phi 60 multiplied by 0.15mm by water, the mouth part is reduced to phi 38mm, a round bottom with the diameter of phi 60mm is welded, and then the thin-wall outdoor kettle is manufactured by rolling threads and curling edges. And removing dirt on the inner and outer surfaces by ultrasonic cleaning.
(2) Stress relief: putting the cup body into a vacuum furnace, and vacuumizing to 8 multiplied by 10-3Pa, heating to 480 ℃, and keeping the temperature for 0.24h, wherein the vacuum degree is kept at 6-9 multiplied by 10 in the heating process-3Pa;
(3) purification and homogenization treatment: heating to 750 deg.C for the second time, and keeping the temperature for 1hThe vacuum degree is kept at 6-9 x 10-3Pa；
(4) Crystal growth: heating to 950 ℃ again, and keeping the temperature for 8 hours;
(5) quenching: cooling to 920 ℃ along with the furnace, and introducing argon of 0.08MPa for quick air cooling;
(6) and continuously cooling the material in an air cooling/furnace to below 80 ℃, discharging the material out of the furnace, and obtaining the needle-shaped patterns with metallic luster, wherein the length of the needle-shaped crystal whisker is 1-3 mm.
Example 3
(1) Processing a titanium product: the strip material with the transformation temperature T of 0.6mmTA1 is adoptedβ889 ℃), a cup body with the diameter of 60mm and the depth of 80mm is manufactured by blanking, stretching, trimming, curling and welding a handle; and ultrasonically cleaning and decontaminating the finished thin-wall titanium product.
(2) Stress relief: putting the cup body into a vacuum furnace, and vacuumizing to 8 multiplied by 10-3Pa, heating to 550 ℃, and keeping the temperature for 0.5h, wherein the vacuum degree is kept at 6-8 multiplied by 10 in the heating process-3Pa;
(3) purification and homogenization treatment: heating to 750 deg.C for the second time, maintaining the vacuum degree at 6-9 × 10-3Pa；
(4) Crystal growth: heating to 910 ℃, introducing argon, maintaining the pressure between 10 and 30Pa, preserving the heat for 30min, heating to 1000 ℃, and preserving the heat for 4 h;
(5) quenching: cooling to 910 deg.C with the furnace, introducing 0.15MPa argon gas for rapid air cooling;
(6) and continuously cooling the mixture in an air cooling/furnace to 60 ℃ and discharging the mixture to obtain the acicular patterns with metallic luster, wherein the length of the acicular crystal whisker is 4-5 mm.
Example 4
(1) Processing a titanium product: the method is characterized in that a phi 48 multiplied by 0.5mmTA1 pipe (phase change starting temperature and phase change finishing temperature) is adopted, the pipe is expanded and thinned to phi 60 multiplied by 0.15mm by water, the mouth part is reduced to phi 38mm, a round bottom with the diameter of phi 60mm is welded, and then the thin-wall outdoor kettle is manufactured by rolling threads and curling edges. And removing dirt on the inner and outer surfaces by ultrasonic cleaning.
(2) Stress relief: putting the cup body into a vacuum furnace, and vacuumizing to 8 multiplied by 10-3Pa, heating to 550 ℃, and keeping the temperature for 0.1h, wherein the vacuum degree is kept at 5-8 multiplied by 10 in the heating process-3Pa between；
(3) Purification and homogenization treatment: heating to 750 deg.C for the second time, maintaining the vacuum degree at 6-8 × 10-3Pa；
(4) Crystal growth: heating to 900 ℃, introducing argon, maintaining 70-80 Pa, preserving heat for 10min, heating to 1200 ℃ again, and preserving heat for 1 h;
(5) quenching: cooling to 920 ℃ along with the furnace, and introducing 0.15MPa argon for quick air cooling;
(6) and continuously cooling the material in an air cooling/furnace to below 80 ℃, discharging the material out of the furnace, and obtaining the needle-shaped patterns with metallic luster, wherein the length of the needle-shaped crystal whisker is 2-4 mm.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (8)
1. A processing method of needle-shaped crystal patterns on the surface of a thin-wall titanium product is characterized by comprising the following steps:
(1) degreasing: providing a finished thin-wall titanium product with the wall thickness of 0.15-0.80 mm, and removing oil stains on the surface of the product;
(2) stress relief: placing the thin-wall titanium product in a vacuum furnace, vacuumizing to 1.0 multiplied by 10-2Heating to 480-550 ℃ below Pa, and keeping the temperature for 0.25-2 h;
(3) purification and homogenization treatment: heating to 680-750 ℃ for the second time, and preserving heat for 0.5-4 h;
(4) crystal growth: heating to TβPreserving the heat for 3-10 h at the temperature of-1000 ℃;
(5) quenching: cooling to T with the furnaceβ～(Tβ+40) deg.c, introducing argon gas and quick air cooling to TβObtaining needle-shaped patterns at the temperature below DEG C;
(6) cooling and discharging, namely continuously performing air cooling/furnace cooling until the temperature is lower than 80 ℃, and discharging to obtain a thin-wall titanium product with needle-shaped crystal patterns on the surface;
wherein, T is described in step (4)βThe alpha → beta phase transition temperature is 882-889 ℃; and in the step (4), the temperature rise adopts a secondary temperature rise process: in the first stage, heating to 900-930 ℃, introducing high-purity argon, maintaining the pressure of the argon in the hearth at 10-80 Pa, and preserving the temperature for 10-30 min; then heating to 980-1000 ℃ and preserving the heat for 1-5 h.
2. The method for processing the needle-like crystal patterns on the surface of the thin-wall titanium product as claimed in claim 1, wherein the thin-wall titanium product in step (1) has a wall thickness of 0.15-0.80 mm and is made of industrial pure titanium with a designation TA 1.
3. The method for processing the needle-like crystal patterns on the surface of the thin-walled titanium product as claimed in claim 1, wherein in the step (1), the surface of the thin-walled titanium product is degreased by using ultrasonic waves or hot alkaline solution.
4. The method for processing the needle-like crystal patterns on the surface of the thin-walled titanium product as claimed in claim 1, wherein the homogenization in the step (3) is to recrystallize at low temperature to obtain uniform grain size, and simultaneously, the residual dirt on the surface is volatilized completely, and the oxide scale is decomposed and absorbed by the matrix.
5. The method for processing the needle-like crystal patterns on the surface of the thin-walled titanium product as claimed in claim 1, wherein a vacuum of 1.0 x 10 is maintained during the temperature raising in step (3) and/or step (4)-2Pa or less.
6. The method for processing the needle-like crystal patterns on the surface of the thin-walled titanium product as claimed in claim 1, wherein the pressure of the argon gas introduced in step (5) is 0.08 to 0.15 MPa.
7. A thin-walled titanium article having an acicular crystal pattern on its surface, produced by the method of any one of claims 1 to 6.
8. The thin-walled titanium product having an acicular crystal pattern on the surface thereof according to claim 7, wherein the acicular crystal pattern on the surface of the thin-walled titanium product has a metallic luster, and the length of the acicular whiskers is 1 to 5 mm.
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| CN114752875A (en) * | 2022-04-08 | 2022-07-15 | 攀钢集团研究院有限公司 | Pure titanium sheet with surface crystal patterns and processing method thereof |
| CN114561533B (en) * | 2022-04-08 | 2024-03-12 | 攀钢集团研究院有限公司 | Processing method of crystal flowers on surface of pure titanium sheet |
| CN114657491A (en) * | 2022-04-08 | 2022-06-24 | 攀钢集团研究院有限公司 | Pure titanium sheet with surface crystal patterns and processing method thereof |
| CN114752876A (en) * | 2022-04-08 | 2022-07-15 | 攀钢集团研究院有限公司 | Processing method of pure titanium sheet surface crystal flower |
| CN114657365B (en) * | 2022-04-08 | 2024-03-12 | 攀钢集团研究院有限公司 | Pure titanium sheet with surface crystal patterns and processing method thereof |
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